EPA-600/2-77-080
April 1977
Environmental Protection Technology Series
                        PILOT PLANT DESIGN FOR
        CHEMICAL DESULFURIZATION OF  COAL
                              industrial Environmental Research Laboratory
                                    Office of Research and Development
                                   U.S. Environmental Protection Agency
                              Research Triangle Park, North Carolina 27711

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                       RESEARCH REPORTING SERIES
 Research reports of the Office of Research and Development, U.S. Environmental Protection
 Agency, have been grouped into five series. These five broad categories were established to
 facilitate further development and application of environmental technology. Elimination of
 traditional grouping was consciously planned to foster technology transfer and a maximum-
 interface in related fields. The five series are:

    1.  Environmental Health Effects Research
    2.  Environmental Protection Technology
    3.  Ecological Research
    4.  Environmental Monitoring
    5.  Socioeconomic Environmental Studies

 This  report has been  assigned to the ENVIRONMENTAL  PROTECTION TECHNOLOGY
 series. This series describes research performed to develop and demonstrate instrumenta-
 tion, equipment, and methodology to repair or prevent environmental degradation from point
 and non-point sources of pollution. This work  provides the new or improved technology
 required for the control and treatment of pollution sources to meet environmental quality
 standards.
                             EPA REVIEW NOTICE
This report has been reviewed by the U.S. Environmental Protection Agency  and approved
for publication. Approval does not signify that the contents necessarily reflect the views and
policy of the Agency, nor does mention of trade names or commercial products constitute
endorsement or recommendation for use.

This document is available to the public through the National Technical Information
Springfield, Virginia 22161.                                            ciuon

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                                                   EPA-600/2-77-080
                                                          April 1977
                 PILOT  PUNT DESIGN
FOR CHEMICAL DESULFURIZATION  OF  COAL
                                by

                         LJ. Van Nice and M.J. Santy

                           TRW Systems Group
                             One Space Park
                        Redondo Beach, California 90278
                          Contract No. 68-02-1335
                           ROAP No. 21ADD-097
                         Program Element No. 1 ABO 13
                         EPA Project Officer: I Lorenzi

                     Industrial Environmental Research Laboratory
                      Office of Energy, Minerals, and Industry
                       Research Triangle Park, N.C. 27711
                             Prepared for

                     U.S. ENVIRONMENTAL PROTECTION AGENCY
                       Office of Research and Development
                          Washington, D.C. 20460

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                                ABSTRACT

     This document presents the results of a program for design and
operational planning of facilities for testing the Meyers Process for
chemical removal of pyritic sulfur from coal.  Two options were evaluated:
(1) a complete pilot plant test of the process at a 1/2-ton per hr scale
and (2) scale-up and testing of only the most critical portion of the
process, the reactor and regenerator section (reactor testing unit).

     The design and test planning effort for scale-up of the Meyers Process
described herein includes:  (1) a summary of background process data,
(2) a discussion of the pilot plant design, (3) pilot plant start-up  and
operational test plans and (4) the preliminary design, start-up and test
approach for the reactor testing unit.  Eight appendices are included
which contain the following:  (1) process flow diagrams for the complete
pilot plant, (2) pilot plant mass balance computer program, (3) pilot
plant plot plans and a sketch of the facility, (4) complete pilot plant
equipment list, (5) critical path schedule for construction of the pilot
plant,  (6) preliminary process flow diagrams for the reactor testing  unit
approach, (7) preliminary reactor test unit plot plans and a sketch of the
facility, and (8) reactor test unit equipment list.

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                            TABLE OF CONTENTS
                                                                     Page
Abstract	      iii
List of Figures	      ix
List of Tables	       x
Acknowledgments 	      xi
Metric Conversion Factors 	      xii
1.  Introduction	       1
2.  Background	       5
     2.1  Process Data	       6
          2.1.1  Simultaneous Coal Leaching-Reagent
                 Regeneration 	       7
          2.1.2  Coarse Coal Data	      10
          2.1.3  Cleaned Coal Data	      11
     2.2  Commercial Scale Process Costs	      12
3.  Pilot Plant Design  	      15
     3.1  Process Design	      16
          3.1.1  Feeding and Grinding	      17
          3.1.2  Mixing	      17
          3.1.3  Reaction and Regeneration	      17
          3.1.4  Secondary Reactor	      18
          3.1.5  Slurry Concentration 	      19
          3.1.6  First Filtration and Washing 	      19
          3.1.7  Crysta 11 izer System	      20
          3.1.8  Final Washing	      20
          3.1.9  Elemental Sulfur Removal 	      21
          3.1.10 Coal Stripping	      22
          3.1.11 Sulfur Recovery	      22
          3.1.12 Disposal 	      23
     3.2  Design Basis	      23
          3.2.1  Process Parameters 	      23

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                     TABLE OF CONTENTS  (continued)
                                                                   Page

                 3.2.1.1   Mixer/Reactor Section. 	     23
                 3.2.1.2   Washing Section	     25
                 3.2.1.3   Toluene Section	     26
          3.2.2  Mass  Balance	     27
          3.2.3  Additional  Equipment Criteria 	     38
     3.3  Materials  of Construction	     40
4.  Pilot Plant Start-Up  and Operational Verification  	     43
     4.1  Personnel  Training 	     43
     4.2  Pilot Plant  Start-Up Operations	     46
     4.3  Pilot Plant  Operational Verification 	     54
5.  Pilot Plant Operation  	     57
     5.1  Equipment  Testing  and Analysis Requirements	     58
          5.1.1   Coal  Feed Section  Testing	     59
          5.1.2   Reactor  Section Testing 	     59
          5.1.3   Sulfate  Removal System Testing	     61
          5.1.4   Organic  Solvent Section Testing 	     63
     5.2  Plant Operational  Schedule and Test Matrix 	     66
          5.2.1   Primary  Reactor (R-l) and Process
                 Chemistry Evaluations 	     75
          5.2.2  Secondary Reactor (R-2) Evaluation	     77
          5.2.3  Slurry Mix Tank (T-2) Operation 	     77
          5.2.4  Thickener (R-3) and Hydroclone (SP-2)
                Operations	     78
         5.2.5  Evaporator-Crystal!izer (SP-3) Operation.  ...     78
         5.2.6  Filter (S-2, S-3, S-4)  Operation	     79
         5.2.7  Wash Water  Contactor (T-ll, T-13) Operation .  .     79
         5.2.8  Azeotrope Still (T-14)	     80
         5.2.9  Solvent Centrifuge (S-5, S-6) Operation  ....     80
         5.2.10 Solvent Contactor (T-16) Operation	     80
                                   vi

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                      TABLE  OF  CONTENTS  (continued)
                                                                    Page
                 5.2.11  Solvent Stripper (SP-4)  and  Coal
                        Cooler  (E-4)  Operation	      80
                 5.2.12  Solvent Cooler (E-9)  Operation.  .....      81
                 5.2.13  Sulfur  Filter (S-7, S-8)  Operation.  ...      81
                 5.2.14  Pulverizer System (A-3),  Knock-Out
                        Drum (V-l), Cooling Water Drum (T-5),
                        Barometric Condenser  (E-1,2,3),
                        Vacuum  Pumps  (K-2,3,4),  Solvent  Still
                        (C-l),  and Carbon Absorption Drum
                        (SP-5)  Operations ...  	      81
     5.3  Materials Testing	      81
6.  Reactor Test Unit	      83
     6.1  RTU Process Design	      83
          6.1.1  Fine Coal Feed System	      84
          6.1.2  Fine Coal Wetting	      84
          6.1.3  Fine Coal Primary Reactor	      85
          6.1.4  Fine Coal Secondary Reactor	      86
          6.1.5  Coal Filtration	      87
          6.1.6  Coarse  Coal Reactor	      87
          6.1.7  Primary Reactor as a Regenerator 	      89
          6.1.8  Sizing  the Reactor Testing System	      89
     6.2  RTU Start-Up	      90
     6.3  Reactor Test Unit Operation and Equipment
         .Supplier Testing	      93
          6.3.1  Task 3-A, Reactor System Test Operation	      93
                 6.3.1.1  Fine  Coal Reaction  System  	      93
                 6.3.1.2  Coarse Coal Reactor System	      98
          6.3.2  Equipment Supplier Testing  	     100
                 6.3.2.1  Filtration	     TOO
                 6.3.2.2  Centrifugation	,	     100
                 6.3.2.3  Solvent Extraction  and Vapor
                          Stripping	     102

                                   YlV'

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7.  References
Appendices
                     TABLE OF CONTENTS (continued)
                                                                    Page

                 6.3.2.4  Crystallization	     102
                 6.3.2.5  Drying  	     102
                                                 	     105
     Appendix A - Process  Flow  Diagram  	     107
     Appendix B - Process  Mass  Balance  Computer  Program	     121
     Appendix C - Pilot  Plant Plot Plan and Configuration.  .  .  .     133
     Appendix D - Complete  Pilot  Plant Equipment List	     137
     Appendix E - Critical  Path Diagram	     141
     Appendix F - Reactor Test Unit Flow Diagram	     147
     Appendix G - Reactor Test Unit Plot Plan and Configuration.     151
     Appendix H - Reactor Test Unit Equipment List 	     155

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                            LIST OF FIGURES
1.   Pilot Plant Operation Schedule .................    44
2<   Pilot Plant Start-up and Operational Verification .......    45
3.   Anticipated Nine-Month C39 Week)  Test Schedule.  ........    67

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                              LIST OF TABLES
No.                                                                  Page
1.  Pilot Plant Mass Balance	28-35
2.  Feed and Product Process Streams	    36
3.  Test Variables to be Evaluated During Operation 	    69
4-  Test Sequence Detail	70-74
5-  Generalized Start-Up Sequence 	  91&92
6-  Summary of Manufacturer Testing Capabilities	  101

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                             ACKNOWLEDGMENTS

     The authors wish to acknowledge the valuable assistance received in
this project from the following TRW personnel:  D. Hopp for assistance in
computer programming; J. Blumenthal and B. Dubrow for managerial  assistance
and manuscript review; and L. Broberg and M. Ramirez for technical  typing.

     The authors owe appreciation to Lloyd Lorenzi, Jr., the monitoring
Project Officer for the Environmental Protection Agency under this  contract
for his constant interest, cooperation and valuable comments on the project,
and to T. Kelly Janes, also of EPA, for guidance and encouragement.
                                    XI

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                METRIC CONVERSION FACTORS
  British
     Metric
1 Btu
1 Btu
1 kw
1 hp (electric)
1 psi
5/9 (°F-32)
1 inch
1 ft
1 ft3
1 gallon
1 pound
1 ton (short)
252 calories
2.93 x 10"4 kilowatt-hours
1,000 joules/sec
746 joules/sec
0.07 kilograms/cm2
°C
2.54 centimeters
0.3048 meter
0.0920 meters2
0,0283 meters3 or 28.3 liters
3.79 liters
0.4536 kilograms
0.9072 metric tons
                          xi i

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                              1.  INTRODUCTION

This document presents the results of an Environmental  Protection Agency
sponsored program aimed at designing and planning the operation of test-
facilities for evaluation of the Meyers Process for coal desulfurization.
A complete pilot plant test of the process is one option for the next step
in the development of the Meyers Coal Desulfurization Process following
the successful completion of essential bench-scale testing.  A second
option would involve scale-up and testing of only the most critical  portion
of the process, the reactor and regenerator section.  The previous investi-
gation' firmly  established the technical and preliminary economic potential
of the Meyers Coal Desulfurization Process and led to the definition of a
baseline pyritic sulfur removal process which served as the basis for design
and test planning of both a full pilot plant and a reactor testing unit.


A pilot plant  design engineered  under ground  rules established by the EPA,
outstanding  in  the breadth  of its overall  capability, was  prepared.  The
plant  is designed to remove 95%  of the pyritic sulfur from raw run-of-mine
high pyritic sulfur (>3 wt %)  coal and to  accomplish this  with:   (1) con-
tinuous automated operation much  like  a  demonstration plant,  (2) maximum
flexibility  of operation, and (3) detailed measurement  of  both the perfor-
mance  of all major equipment  and  the  fate  of  all  pollutant-forming con-
stituents  through extensive instrumentation.   The plant design is sized to
operate continuously for sustained periods of time at a coal  throughput
from 1/4 ton to 1/2 ton/hr.   In  addition,  a secondary pilot  plant reactor
has been designed to do double duty  as a tenfold  geometric scale-up  of  the
critical primary  reactor/regenerator  unit.  Note  that a further  tenfold
scale-up of  the reactor/regenerator  unit would be equivalent to  the  size
which  would  be  utilized in a  50  tph  demonstration plant, with sufficient
desulfurized coal output to feed  a 100 to  150 MW  power  unit.

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Alternate approaches to scale-up  of the  Meyers  Process  not  requiring the
complete and versatile pilot plant  were  also  examined.   This  effort
resulted in a preliminary design  for testing  the  critical reactor/regen-
reactor section of the Meyers Process in much the same  manner as in the
pilot plant design.   The less critical steps  would be .tested  at equipment
manufacturers to develop design and scale-up  information for  process steps
downstream of the reactor section.   The  Reactor Test Unit design also
includes the capability to evaluate the  process for coarse  coals
(1/4 to 3/8 in. top  size) which cannot readily  be processed as  coal  slurry.

In addition to this  summary report, the  program output   consists of:
(1) a detailed construction bid book, suitable  for obtaining  fixed  price
bids on the construction of the pilot plant at  the TRW  Capistrano Test
Site (San Clemente,  California),  (2) an  estimate  of the cost  of construct-
ing the facility at  the TRW Capistrano Test Site, and (3) a scale model
of the complete pilot plant.

The Construction Bid Book, which  was submitted  to EPA under separate cover,
contains the following information:

     •  Scope of work to be performed during  plant construction.
     §  Plot plans and general arrangement drawings of  the  facility.
     •  Piping and instrumental drawings,
     •  Selected mechanical equipment types,  specifications and
        vendors.
     •   Piping specifications and line list.
     •   Insulation specification.
     t  Specification  for  foundation, sewers  and  paving.
    •  Structural specifications.

    •  Electrical specifications and drawings.
    •  Instrumentation summary and specifications.

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     t  Insulation summary and specifications.
     •  Protective coatings specifications.

A construction cost estimate for the pilot plant, as specified in the Bid
Book, has been prepared and submitted to EPA as a separate item.   The cost
estimate was based on written quotations from suppliers for all  major
equipment.  Generally, quotations were received from three or more sup-
liers for each major item and the most advantageous or lowest cost source
was selected for the estimate.  Piping, valving and instrumentation costs
were developed from catalog prices or recent procurement experience.  Craft
labor and construction materials were estimated using experience factors
for similar projects.

A detailed scale model of the pilot plant (3/8 in. = 1 ft) was delivered
to EPA.  The model was constructed from the piping and instrumentation
diagrams, the plot plans and the general arrangement drawings.

The following sections describe the design and test planning effort for
scale-up of the Meyers Process for the chemical desulfurization of coal.
Section 2.0 presents a summary of background information primarily
obtained during bench scale testing.  Section 3.0 discusses the pilot
plant design.  Pilot plant start-up (Section 4.0) and operational
(Section 5.0) test plans are detailed.  The preliminary design, start-up
and testing of the reactor section rather than the complete pilot plant,  is
described in Section 6.0.  This document also includes eight appendices
which contain the following:  (1) process flow diagrams for the complete
pilot plant, (2) pilot plant mass balance computer program, (3) pilot
plant plot plans and a sketch of the facility, (4) complete pilot plant
equipment list, (5) the critical path schedule for construction of the
pilot plant,  (6) preliminary process flow diagrams for the reactor test-
ing approach, (7) reactor test unit plot plans and a sketch of the
facility, and (8) reactor test unit equipment list.

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                              2,   BACKGROUND

The Meyers Process is a developing method for the removal  of pyritic sulfur
from coal utilizing a regenerate aqueous ferric sulfate leaching system.
An overall representation  of  the  process chemistry for both leaching and
regeneration  is  outlined below:

                           Process Des cri p t i on
      (1)  Crushed  coal  is  treated with warm ferric sulfate solution
          FeS2 + 4.6Fe2(S04)3 + 4.8H20 -> 10.2FeS04 + 4.8H2$04 + 0.8S

      (2)  Generated sulfur is removed with  a warm solvent bath or by
          vaporization
      (3)  Ferric sulfate solution is regenerated with air and excess
          ferric and  ferrous  sulfates are removed
          9.6FeS04 +  4.8H2S04 + 2.402 -»• 4.8Fe2(S04)3 + 4.8H20

The  process operates  under mild temperatures and pressure, i.e., 90 to
130°C  and ambient  to  100 psi  or greater.

The  coal  feed for  chemical desulfurization  may  range from finely ground
coal  (e.g., -100 mesh)  to  coarse  coal suitable  for shipping (e.g., -3/8 or
-1/4 in.).  The  major emphasis in the development of the process to date
has  been  on the  processing of fine coal utilizing a simultaneous leaching
and  regeneration approach  in  which the ferric sulfate leaching agent is
regenerated in the presence of the coal which is being leached.

Previous  EPA-sponsored  programs have been undertaken to (1) define  the
applicability of the  process  for  reduction  of sulfur oxide pollution from
stationary sources through desulfurization  of uncleaned run-of-mine

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 coal, (2) prepare conceptual  engineering  designs  of full-scale  units,
 and (3) prepare cost estimates  for commerical  plants.   These studies
 indicate that the Meyers Process is capable of removing 90 to 95% of the
 pyritic sulfur from  most coals  and  that application of the process  to
 run-of-mine Appalachian coal  reserves would free  high sulfur reserves
 comprising about 30% of the present Appalachian coal production  for power
 production under EPA's New Source  Performance Standards, while most of the
 remaining Appalachian coal can  be  desulfurized by the process to meet  state
 SOX standards.  In addition,  the process  is applicable for meeting  Federal
 and State standards  for selected Eastern  Interior,  Western Interior and
 Western coal reserves.  Engineering cost  analyses indicate that  the process
 will be cost-competitive with flue gas scrubbing  and other coal  conversion
 processes.

 Very recently, emphasis has been placed on the processing of coarse coal.
 It has been found that more than 80% of the pyritic sulfur can be removed
 from coarse run-of-mine Appalachian coal  in 48 hours, at 100°C,  and
 that near complete removal of pyritic sulfur can  be obtained on  continued
 leaching.   Further,  the utilization of clean coal,  typical of the output
 of a coal  preparation plant,  significantly increases the rate of pyrite
 removal  by the Meyers Process.

 Summary  information  on process  data for desulfurization of both  fine and
 coarse coal  is presented in Section 2.1 and a summary of factors which can
 reduce commercial  scale process costs is  presented  in Section 2.2.

 2.1  PROCESS  DATA

 The  majority  of process design  data on the Meyers Process were  generated
 under  two EPA  sponsored bench-scale process evaluation and development
 programs (Contract EHSD 71-7 and Contract 68-02-1336),

Under Contract EHSD 71-7,  data were generated which demonstrated the tech-
nical feasibility of  all  process unit operations,   In addition,  empirical

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rate expressions were  derived  for coal pyrite leaching (100 mesh x 0
Lower  Kittanning coal)  and  reagent  regeneration on which a preliminary
process  design  and  cost analysis was based.  More recent data, presented
in the following sections,  cover results derived from simultaneous Teaching-
regeneration  processing of  suspendable coal  (100 mesh x 0  and  14  mesh  x  0
Lower  Kittanning coal) and  preliminary data on  coarse coal  (1/4 inch x 0),
The suspendable coal experimentation was performed  under EPA Contract
68-02-1336.

2.1.1  Simultaneous Coal  Leaching-Reagent Regeneration

The  primary objective  of the second bench-scale program on the Meyers
Process  (EPA  Contract  68-02-1336) was the investigation of potential pro-
cess improvements aimed at  process  simplification and cost reduction.  A
number of  the attempted process  improvements proved successful; the most
important  were  simultaneous Teaching-regeneration, intermediate size coal
processing (14 mesh x  0), and  concentrated  slurry processing (>30 wt %).


In the combined Teaching-regeneration mode of operation the coal  to be
processed was slurried  in hot recycled reagent solution (nominally 5 wt %
iron,  2 wt  %  H^SO*)  in  a mixing vessel, heated to boiling,  and  refluxed for
15 to  30 minutes prior  to transfer to the Teaching-regeneration pressure
reactor  (L-R  reactor);  this slurry-mixing, coal-wetting operation in the
"mixer" minimized slurry foaming in the L-R reactor.   The slurry was
sampled at  this point in order to determine the  quantity of pyrite leached
from coal during the slurry mixing-heating operation;  the pyrite content
of the coal at the end  of this operation was considered the starting coal
pyrite concentration for the L-R operation.   After slurry transfer to the
leaching/regeneration reactor, the system was pressurized by nitrogen
to a nominal  100 psig   and heated to the desired L-R processing temper-
ature  (nominally 120°C).  As soon as the slurry temperature reached the
desired value, slurry circulation (through a reactor loop)  and  oxygen
injection to  the slurry were initiated.   L-R processing was varied from

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1  to 8 hours  in these  experiments.  Reactor slurry  samples  were  also
taken at frequent reaction  time  intervals  [0.5 to 1.0  hours)  during each
experiment.   Upon expiration  of  the desired L-R processing  time, the  re-
actor was depressurized and the  slurry was either transferred to a  settler
for further coal leaching at  90  to 95°C  or the leaching  reaction was  term-
inated by immediate filtration and cake  washing.  In either case, the
leached coal  was subsequently (1) washed with water to remove residual
iron sulfate; (2) washed with toluene for  recovery  of  elemental  sulfur,
(3) vacuum dried and (4) analyzed.  The  available data to date on L-R
processing of suspendable Lower  Kittanning coal leads  to the  following
observations:

     a  Coal  pyrite leaching  rates under L-R processing  at  120°C
        are approximately three  times higher than those  deter-
        mined for 102°C coal  leaching under continuous reagent
        exchange (separate  reagent regeneration).

     •  Pyrite leaching rates derived from L-R processing at
        120°C and 100  psig  of 100 mesh  x 0 and  14 mesh x 0
        Lower Kittanning coal are virtually identical.

     •  Coal  pyrite leaching  rates at 120°C are not detectably
        affected when  slurry  concentration is increased  from
        20 wt % to  33  wt %  solids.

     •  During the  first 2  hours of L-R  operation at 120°C
        and 100  psig (approximately 80%  pyrite removal)  the
        pyrite leaching  rate  from 100 mesh x 0 and
        14 mesh  x 0  Lower Kittanning coal  can be  represented
        by the empirical  expression

                 2  2
        i"L = kL Wp  Y  = wt pyrite removed/hr-100 wt coal
                                   8

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        where    W   =  wt % pyrite in coal
                 Y   =  ferric ion to total  iron  wt ratio,  and
                 kL  =  0.45 ± 0.05 (hours)"1  (wt % pyrite)"1

        Pyrite leaching rates decrease substantially after
        approximately 2 hours of  L-R  operation;  this
        observation may be  characteristic of the particular
        coal under investigation  and  it could be due to the
        high ash  content of the coal  (30 wt %).  Additional
        pyrite removal is attainable  during settler processing
        (90  to 95°C,  ambient pressure).

     •  L-R  processing, at  least  up to 130°C and 100 psig,
        does not  appear to  affect  the composition and heat
        content of the coal beyond those changes expected
        due  to pyrite removal; however, changes in trace
        elements  are  still  under  investigation.  Coal
        analysis  of "as received"  and processed coal fur-
        nished no evidence  of either  oxidation or sulfo-
        nation of the coal  matrix.

     •  Reagent regeneration rates under L-R operation appear
        to be the same as those determined from separate regen-
        eration operation.    During  2 hours of L-R operation,
        the  slurry Y  value  increases  from approximately 0.5 to
        0.9.

     •  100  hours of  reagent recycling under L-R conditions
        furnished no  evidence of  reagent efficiency
        deterioration.

The data generated on simultaneous coal leaching-reagent regeneration
processing has not yet been completely reduced and evaluated; however the
above conclusions on  process performance appear valid.  The formulated

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rate expression and the quoted value  of its  constant are considered
adequate for scale-up designs for suspendable  Lower Kittanning coal.   The
data listed below indicate typical  pyritic sulfur (Sp)  removals obtained
during,the processing of such coal  (starting Sp  = 4 wt  %, starting ash
30 wt %):

                                                          % Sp
                                                         Removal
     During slurry heating and mixing                     15-20
     After 1-hour L-R operation                            ^65
     After 2-hour L-R operation                            ^80
     After settler processing (20 hours at 90°C)           -^90

2.1.2  Coarse Coal Data

Processing of coarse coal by the Meyers Process  has not been as exten-
sively investigated as the suspendable coal; however, the available data
indicates that processing of coarse,  readily shippable  size coal is
feasible and therefore merits further investigations.

Data on coarse coal were generated with 100  to 500 grams, 1/4 in.  x 0
Lower Kittanning coal slurried in iron sulfate solution (5 wt % Fe,
15 to 20 wt % solids).   The leaching  temperature was maintained at 102°C
(reflux under ambient pressure).  The reaction time was varied from 4 to
48 hours.   The reagent in the reacting slurry  was exchanged frequently in
order to maintain the Y value in the  0.8 to  0.9  range.   The extent of
pyrite  removal  as a function of reaction time  was determined from ferrous
ion production and from sulfur forms  analyses  of the processed and unpro-
cessed  coal.   Pyrite  removal at several representative times are as follows:

              Reaction  Time, hr         % Sp Removal
                      4                     37
                      6                     44
                     24                      73
                     48                      81

                               "   10

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A sample of 1/4 In. x 0 Lower Ktttanntng coal was sieved tnto several
narrow size fractions.  The coal from several size fractions was processed
for 48 hours as described above.  The following results were obtained:

                 Size Fraction               % Sp Removal
                 4x8 Mesh                       67
                 8 x 14 Mesh                      83
                14 x 28 Mesh                      88
               100 Mesh x 0                       98
               1/4 in. x 0 Starting Coal          81

It is evident  that a rate expression for coal leaching must include a
particle size  relationship.  Additional data will be necessary to obtain
an improvement to the overall integrated rate expression which is currently
in use.

2.1.3  Cleaned Coal Data

Recently,  a sample of 8 mesh x  14 mesh Lower Kittanning coal was cleaned
by float-sink  and the 1.75 specific gravity float portion (80% w/w of the
sample) was treated by the Meyers Process under the same 48 hour con-
ditions described previously.

                             %  Sp Removal    Final % Ash     Final Btu
     Uncleaned sample             83              15          13,260
     Float sample                 92               5          14,740

The results show that (1) clean coal reacts substantially faster than
run-of-mine coal  and (2) coarse coal (In this case, a cleaned narrow size
fraction)  can  be desulfurlzed to near zero pyrite (Sp =  .09 wt %).
                                    11

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2.2  COMMERCIAL  SCALE PROCESS COSTS

Conceptual  full-scale process designs with corresponding cost estimates
have been prepared by TRW  and independently by several engineering  firms
during several stages of the EPA sponsored laboratory and bench-scale
development effort.  Escalation of costs have occurred due to inflation
since these data were generated and while the magnitudes have changed, it
is probable that the ratio of cost items is relatively constant.  Thus,  in
excess of one-half of the  process cost  of pyritic sulfur removal  by the
Meyers Process  is related  to the capital costs of the process.  The areas
where capital cost improvements are most likely  are:

     Processing  larger  particle size  coal:  Generally the cost
     of separating the  coal from  leach  solution  will rapidly
     decrease as particle  size  increases.  A  decrease in separ-
     ation cost  during  washing  and solvent extraction will be
     partly offset by  an  increased contact time  for solutions  to
     penetrate and equilibrate with  the internal pores  of coarser
     coal particles.

     Processing  cleaned coal:  Three  areas of cost  reduction
     appear to be related  to coal cleaning:   (1) there  is  less
     pyrite to  remove so  that less residence  time and oxygen
     are required, (2)  reaction rates with cleaned  coal  appear
     to increase, further  reducing residence  time,  and  (3)
     filtration  rates increase as the ash component of  coal  is
     decreased.

     Increasing  slurry  concentration;   Increasing the coal  con-
     centration  in the  slurry will reduce the volume of the
     reactor, although  not  in direct  proportion  to  the  reduction
     in  slurry volume.  A major effect  is that slurries with 33%
     and  greater  solids will not require a thickener and filtra-
     tion cost decreases as solid content increases.
                                   12

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     Alternate  methods  of removing  elemental  sulfur:   Removal
     of elemental  sulfur by extraction with  an  organic solvent
     has been evaluated in detail at bench-scale  and  is  the
     basis  for current  process  designs.   Direct vaporization
     of sulfur using hot purge  steam, or an  inert gas such as
     nitrogen,  has been evaluated briefly and has been found
     to be  feasible and to be as  effective as solvent extraction.
     Cost reduction ts  possible 1f  the vaporization temperatures
     are low enough, residence  time short enough  and  if  few
     troublesome compounds are  vaporized and condensed with the
     sulfur.

Updated process designs and process cost estimates will  be prepared  for
commercial  size plants  as a final task in the current bench-scale  program
(EPA Contract 68-02-1336).  These cost data  and a preliminary  assessment
of potential benefits from gravity  and size/gravity separation  prior to
leaching will be important in selecting  the  goals for further  process
improvement and cost reduction.
                                    13

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                           3.   PILOT  PLANT  DESIGN


The process flowsheet and mechanical design of a pilot plant to evaluate

the Meyers Process are complete.  Ehrhart Division of Procon Incorporated,

under a subcontract to TRW, provided the mechanical design and assisted

TRW in the process design and preparation of the flowsheet.


Key ground rules in the design of the coal desulfurization pilot plant

were established by the EPA in the Scope of Work of the Design Contract.

These were :


    (1)   The pilot plant shall be designed to have the capability of
          processing up to approximately one-half ton of coal  feed per
          hour and shall be capable of processing the coal automatically
          in both batch and continuous flow modes.

    (2)   The pilot plant design effort shall  be directed toward a flow
          scheme capable of total removal of pyritic sulfur from coal.

    (3)   The process design shall provide for sufficient instrumentation
          and sampling points as are necessary to obtain complete material
          and energy balances around the entire plant as well  as around
          each major processing or material handling operation.

    (4)   The process design shall also allow for the determination of
          the fate of ash and other potentially pollutant-forming constit-
          uents in addition to determination of the fate of sulfur.

    (5)   Analytical techniques and equipment which can provide rapid,
          reliable and relevant process data shall  be designed to provide
          for the collection of information on the performance of all
          major items of equipment and shall be designed to have sufficient
          flexibility to permit, with little difficulty, the timely incor-
          poration of alternate processing units, as may be required from
          further process development, into the pilot plant.

    (6)   The pilot plant shall be designed to provide optimal economic
          supply of process heat requirements and shall provide an
                                    15

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          environmentally sound system and one which results in the
          most desirable utilization of fuel resources in recognition
          of the requirements for commercial application.
     (7)  Considerations during pilot plant design shall be devoted  to
          the establishment of pilot plant control variables which are
          required  for processing different types of coals.

The above plant design basis  is  almost  unique  in  scope  for pilot units  in
that (1) the plant will  be  an  automated unit capable  of continuous and  batch
operation, while (2) the plant will  be  capable  of maximum flexibility of
operation with provision for incorporation of  alternate processing units.
In addition, the plant will be thoroughly  instrumented  for extensive  deter-
mination of both the performance of all major  items  of  equipment and  the
fate of all pollutant-forming constituents.

 The  plant was  designed  to  be  constructed  at TRW's 2700-acre Capistrano
 Experimental  Facility on an existing four-level  test stand which  has ready
 access to power,  cooling water, steam  and potable water.  The pilot  plant
 plot plans  and  an  artist's sketch of the  facility are  presented in Appendix
 C.   The detailed  design and specification of equipment,  piping and instru-
 tation diagrams,  vendor specifications, etc.,  are included in the design
 package which  is  in a separate volume.  Section  3.1 presents a description
 of the pilot  plant  process design (process flow  diagrams are presented
 in Appendix A), Section 3.2 discusses  the design basis  (including the mass
 balances) and Section 3.3  discusses materials  of construction.

3.1  PROCESS DESIGN

The process design  consists of six major operations, namely  (1)  grinding
and feeding coal to a mixer,  (2) concurrent pyrite leaching and regeneration
of the  iron sulfate leach solution, (3) secondary leaching to reach  the
design  level of pyrite removal,  (4)  water washing to remove leach solution
and soluble sulfate from the  coal, (5)  toluene extraction to remove  elem-
ental sulfur from the coal, and (6)  steam or nitrogen stripping of the
coal  to recover the solvent.   These six main operations, the alternate
processing modes and the supporting process equipment will  be described  in
the following  12 subsections  with  references  to stream numbers and

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equipment numbers shown on the flow sheet (Appendix A foldouts).  A detailed
pilot plant equipment  list is  presented  in Appendix  D.

3.1.1  Feeding and Grinding

Coal of about 1-1/2" top size  is brought from storage by conveyor A-l to
the pulverizer system A-3.  Pulverized coal is conveyed to surge tank T-l.
The pulverizing system and surge tank are designed for operation under a
nitrogen rich atmosphere and will vent excess gas through fabric filters
for dust removal.  The tank is equipped with a water spray system for fire
protection.

3.1.2  Mixing

Ground coal is passed  through  the bin discharge A-4 to the weigh belt
feeder A-5.  The weighed coal  is continuously fed through rotary feeder
SP-8 to the first stage of the three-stage mixer T-2 (stream 1) where it
is slurried with return leach  liquid (stream 2) and heated to boiling by
live steam  (stream 3).  Gas carried in with the pulverized coal and any
gases  (such as C02)  liberated  by reaction are washed by the incoming leach
solution in SP-1 and with water in T-3 before being vented through blower
B-2.  The slurry and gases from any of the three stages can be sampled and
analyzed.

3.1.3  Reaction and  Regeneration

The heated slurry is pumped by P-l to the reaction vessel R-l (stream 4).
The interior of the  cylindrical reaction vessel is divided into ten com-
partments with a length approximately equal to slurry depth.  Baffles are
are provided to allow  for  cascade flow from stage to stage and to inhibit
return of slurry to  an upstream stage.  The first five stages can be by-
passed by the incoming slurry  in order to operate as a five-stage reactor.
Continuous regeneration of the leach solution in each compartment or stage
is carried out by injection of oxygen (stream 5) into the discharge line
of a slurry re-circulation pump connected to each stage (pumps P-2A

                                    17

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through P»20).  Each stage is  provided with  an  agitator with  an impeller
installed near the vapor-liquid interface  in order to reduce  the possi-
 bility of any significant build-up of solids in the  vapor  space.

In addition, two agitators are provided  with a  second impeller suitable
for gas dispersion so as to demonstrate  mechanical  aeration as a means of
leach  solution regeneration.  The two gas  dispersion  agitators can be
installed in any compartment.   A manifold  system equipped with static
mixers suitable for installation in a single stage is also provided for
demonstration of a third means of leach  solution regeneration.  Injection
connections for steam and for cool recycle leach liquor are provided for
temperature control.

Steam, excess oxygen and inert gases are drawn  from the reactor (stream 6),
then washed and cooled by recycle leach  solution (stream 17).  Any water
condensed from stream 6, water soluble components  and mist are added to
stream 17 to  give the mixer feed  (stream 2).  The washed, cooled gas is
split.  A small portion (stream 9) is vented through  scrubber T-3 while
the major portion (stream 8) is recycled to the reactor through compressor
K-l.   Makeup oxygen is provided by stream 7.

3.1.4   Secondary Reactor

Slurry from reactor R-l, under pressure  (stream 10),  ts reduced to about
atmospheric pressure and introduced to a flash  drum (T-4).  Flash steam
(stream 11) is condensed with cooling water. The remaining slurry, at its
boiling point (stream 12), is introduced to the secondary reactor (R-2).
This two-stage vessel is similar to R-l  but each stage is about an order
of magnitude larger in volume.  Alternate  piping is provided so that the
secondary reactor can also be operated as  a two-stage primary  reactor
where  the two stages are geometrically about ten times btgger  than  the
stages of reactor R-l.   Using R-2 in this  fashion will provide data
on the geometric scalability of the reactor system.
                                    18

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3.1.5  SI lurry Concentration

The effluent from reactor R-2  (stream 13) Is pumped (P-3) to the first
filter (S-2).  Slurry concentration may be as low as 15% solids in stream
13.  Significant saving in filtration cost can be realized if preconcen-
tration of the slurry into the 30 to 50% solids range can be achieved.
Two off-line processes with potential for slurry concentration are shown.

A demonstration thickener (R-3) is provided to intermittently test a
portion of the secondary reactor effluent to determine the extent that
slurry thickening can be achieved and whether a thickener can function as
a secondary reactor.  Design is based on manufacturer's recommendations
for a pilot thickener operation.  Underflow is pumped (P-4) to the filter
(S-2) and the overflow (if it  is sufficiently clear) will go to surge (T-9).
A further task of the thickener operation is to test acid resistant con-
crete lining of steel equipment and to test rubber coated thickener inter-
nals.

Piping and flow controls are provided for testing the slurry thickening
achieved in a hydroclone.  Several sizes from 1/2 in. to 3 in. are pro-
vided to examine the separation achieved for coal slurries varying in
particle size from  100% -8 mesh to 100% -100 mesh.  This system generally
will be operated off-line with slurry from R-2 pumped (P-26) through the
hydroclones to mixed surge tanks for the underflow (T-26) and overflow
(T-27).  Provisions are also made to operate two hydroclones in series so
as to reduce the solids content of the overflow.

3.1.6  First Filtration and Hashing

The nominal operating mode of  the plant involves filtering the slurry from
reactor R-2 (stream 13) to provide recycle leach solution and then further
washing the cake to reduce the residual sulfate on the coal.  Filter S-2
is a fully enclosed rotary vacuum filter.  The filtrate  (stream 19) from
the initial separation of the  feed slurry is pumped (P-8) from the vacuum
                                    19

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 receiver (V-2) to the recycle surge tanks (T-9 and T-10).   The filter cake
 is spray-washed in the filter with a dilute leach solution (stream 22) and
 the wash liquid is drawn to the second vacuum filtrate receiver (V-3).
 Pump P-9 draws liquid from V-3 (stream 20) and sends a portion (stream 18)
 to the  disposal tank (T-25) and a portion (stream 15) to the makeup tanks
 (T-6 and T-7).  Any makeup materials are added to T-6 and T-7 and the
 resultant  stream 16 is pumped (P-5) to the surge tanks (T-9 and T-10). The
 combined filtrates and makeup contained in tanks T-9 and T-10 are pumped
 to the  reactor knock out drum V-l as stream 17, which was previously dis-
 cussed.  Vacuum for the filtrate receivers (V-2 and V-3) is provided by
 compressor K-2 operating through a barometric condenser (E-l).

 3.1.7   Cry stalli ze r Sy s tern

 It should  be  noted that the pilot plant process normally disposes of the
 iron sulfate  from the pyrite leach reaction as an aqueous solution
 (stream 18 principally).  The commercial design plans to recover wash
 water from the waste stream and to produce a solid iron sulfate product.
 The crystal!izer system (SP-3) is designed to investigate this aspect of
 the processing.  A separate package system is provided to test the effect
 of temperature and feed composition on the iron/sulfate ratio and the water
 of hydration  obtained in the crystal product.  The crystal!izer-evaporator
 will operate  intermittently on a portion of the leach liquor drawn from
 surge tanks T-9 and T-10.  The unit is designed to evaporate 1000 Ib  per
 hour of water operating at atmospheric pressure or under vacuum.  The
 product cyrstals will be separated from the rich liquor using the first
 centrifuge in the organic extraction section (S-5).  Filtration tests may
 also be conducted with filter S-2 without the spray-wash.

 3.1.8  Final Washing

The filter cake from the first filter (stream 21) is given additional
washing to  reduce the soluble sulfate level.  The steps include two
separate stages of repulping, filtration and filter  cake washing.  The
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first repulping occurs 1n contactor T-ll where the filter cake (stream 21)
is slurried with recycled wash water (stream 23) and then pumped (P-10)  to
the second filter (S-3).  The second filter is operated much like the first
filter with a wash stream (27) and two filtrate streams.  The receiver
effluents from the vacuum receivers V-4 and V-5 are separately pumped
(P-ll and P-12) to the common header (stream 54) which is sent to waste
disposal tanks (T-25A and B).  Vacuum for the receiver is provided by
K-3 through barometric condenser E-2.  The filter cake (28)  is repulped
with water (29) in a mix tank (T-13) and pumped (P-13) to the last filter
(S-4).  In this filter, the filtrate from the feed (stream 30) and from
the water wash (stream 31) are combined in the vacuum receiver (V-6).
The combined filtrate and wash (stream 32) is pumped (P-14)  to the surge
tank  (T-20).  This very dilute solution (stream 53) is pumped  (P-19)
back  to the first washing stage to provide the wash to the first filter
(stream 22) and the water for the first repulping mixer (stream 23).
Vacuum for the final filter (S-4) is provided by K-4 and condenser E-3.

3.1.9  Elemental Sulfur Removal

Removal of elemental sulfur from the coal is accomplished by extraction
with  hot toluene.  Water-wet coal from the final wash filter (stream 33)
is introduced to a jacketed vessel (T-14) through a rotary feed valve
(SP-7).  Sulfur lean toluene (stream 34) is added to T-14 and the water/
toluene azeotrope is removed (stream 35), condensed (E-6) and fed to
decanter T-19 for phase separation.  The water-free coal toluene slurry
(stream 36) from T-14 is pumped (P-15) to the first centrifuge (S-5).
Clean toluene  (stream 38) is used  to wash the cake and  a combined centrate/
wash  solution  (stream 37) is pumped  (P-16) from the receiver  (T-15)  to  the
rich  solvent surge tank  (T-22).  The cake from S-5 (stream  39) is repulped
in T-16 with fresh toluene  (stream 40) and the resultant slurry  (stream 41)
is pumped  (P-17) to the second centrifuge (S-6).  The cake  is washed with
additional toluene (stream 43) and the combined centrate wash  (stream 42)
is transferred to surge tank T-21.
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3.1.10  Coal Stripping

Coal, wet with toluene from the  second  centrifuge  (stream  44),  is  fed
through a rotary feeder (SP-6) to  the continuous rotary  shelf dryer (SP-4).
Hot nitrogen (or steam)is used to  strip the  toluene  from the  coal  to pro-
duce a dry coal (stream 47) which  is cooled  to  give  the  product coal.
When steam stripping is used,  the  input steam (stream 46)  is  removed from
the dryer (stream 45) with toluene from the  coal.  Stream  45  is condensed
(E-5) and separated in T-18 to give toluene  for reuse (stream 49)  and
water for disposal (stream 50).  With a hot  nitrogen loop, decanting is
not required; but  a knockout  drum would be  used to  separate  the toluene
from the recycle nitrogen.

3.1.11  Sulfur Recovery

Toluene, rich in sulfur, from the  first centrifuge is removed from the
surge tank T-22 by pump P-21 and fed (stream 56) to  the  solvent still
(C-l).  Clean toluene from the  still  overhead (stream 58)  is  condensed
(E-7) and sent to T-23 where it  is combined  with clean toluene from the
azeotropic still decanter (stream  51)  and from the dryer decanter (stream
49).  The clean, heated toluene  (stream 59)  from T-23 is pumped (P-22) to
the centrifuges (streams 38 and  43),  to the  second repulper (stream 40),
and to T-21 (stream 55) where  it is combined with  another lean sulfur
stream (42).  The lean sulfur  stream from T-21  (stream 34) is pumped (P-ZO)
to the azeotropic still as discussed in Section 3.1.9.

Returning to the solvent still  (C-l),  the sulfur rich bottoms  (stream  60)
are pumped (P-23) to the scraped wall  exchanger (E-9).  The sulfur by-
product (stream 61) is removed from the toluene in either of two  leaf
filters (S-7 and S-8).  In addition,  a  portion of  the stream from tank
T-22 is bypassed around the still  (stream 64) and  fed to the filter  to
hold the sulfur cake on the filter leaves.  The combined filtrate (stream
57) is  returned to the surge tank  (T-22).
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 3.1.12  Disposal

 Disposal tank T-24 contains water from the azeotrope decanter (stream 52),
 and, when steam stripping drying is used, water from the dryer decanter
 (stream 50).  Since  there may be traces of toluene mixed with the water,
 this stream  (63)  is  intermittently pumped (P-24) to the disposal truck.
 Commercial disposal  is  also used for tanks 25A and B, which contain the
 waste iron sulfate product from the pyrite reactor.  The effluent (stream
 62) is also  intermittently pumped (P-25) to a disposal truck.  A vapor
 absorber (SP-5) is used to control any vapor effluents.  The carbon drum
 has been designed to hold approximately 500 pounds of carbon and this has
 been calculated to be adequate for 16 weeks of operation, assuming one
 complete vapor displacement of all solvent-containing tanks once per week.

 3.2  DESIGN  BASIS

 The pilot plant mechanical design required nominal  values of many param-
 eters to be  specified and, in some cases, also required minimum or maximum
 values to be known.    The principal  process parameters which influence flow-
 rates and equipment  selection or sizing are identified in Section 3.2.1.
 The nominal  mass  balance and the influence of parametric variations are
 given in Section  3.2.2.  Additional  equipment design information if given
 in Section 3.2.3.

 3.2.1  Process Parameters

 3.2.1.1  Mixer/Reactor  Section - Stage-by-stage calculations of the extent
of reaction in the mixer and in the two reactors were completed based on
data from the bench-scale program as given in the final report .  It was
calculated that 17.4$ pyrite removal would occur in a mixer with three stages
each of 0.25  hour  residence time at about 100°C.  After ten 0.5 hour reactor
regenerated stages at about 120°C, the reaction was calculated to be 83.6%
complete.  The target 95% removal could be obtained with about 24 hours of
additional reaction at 100°C.  These values were taken as normal reaction

                                    23

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 extents.  The ferric to total iron ratio (Y) in the recycled leach solution

 is  dependent upon the amount of concurrent reaction and regeneration.  At a

 reactor total pressure of about 50 psig, the above pyrite removals are

 obtained  at a recycle Y of about 0.75 with nominal leach solution.

 Improved  estimates of these rates will be obtained (from a current bench-

 scale program recently completed) and some adjustments to residence time

 and pressure may  be  necessary to obtain these precise removals and Y values,

 The nominal values of parameters necessary to provide a mass balance around

 the mixer/reactor section are as follows:


      Coal feed  rate  (dry)                       1000 Ib/hr
      Coal moisture                                10 %
      Pyritic sulfur  (dry basis)                  3.2 %
      Iron in recycle leach solution              5.0 %
      Solids content  in mixer                      20 wt.%
      Steam/condensate to heat mixer              274 Ib/hr
      Reaction in  mixer                          17.4 %
      Pressure in  reactor R-l                      50 psig
      Temperature  in  R-l                          250 °F
      Water vapor  pressure in R-l                29.8 psi
      Oxygen concentration in R-l exit             90 wt.% (dry)
      Oxygen in  makeup                           99.5 wt.%
      Water vapor  pressure in vent (T=150°F)      3.7 psi
      Oxygen fed to R-I/oxygen consumed           8.0
      Flash steam  from R-l (stream 11)            150 Ib/hr
      Reaction in  R-l (83.6-17.4)                66.2 %
      Reaction in  R-2 (95.0-83.6)                11.4 %
      SO^/Fe ratio in R-2 effluent                1.5
      Y in R-2 effluent                            .75
 It should be noted that the basic overall reaction for leaching pyrite
 and regenerating the solution is:

     FeS2 + 2.4 02 -> 0.6 Fe+2 + 0.4 Fe+3 + 1.2 SO^ + 0.8S


 It can be seen that the inherent Y of this reaction is 0.4 and if  the  iron

 and sulfate are not removed in the ratios produced, the recycle stream

will  change composition with time.  The pilot plant process proposes to
                                    24

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remove  the  reaction  products  by  non-selectively  discarding a portion of
the  reactor (R-2)  effluent.   This  would  produce  an  imbalanced  iron/sulfate
ratio and Y in  the recycle  stream, if makeup  is  not correctly  chosen.  To
keep the stream in balance  the basic reaction also  must be regenerated to
equal the recycled Y (0.75  in the  nominal  design)..  The overall reaction
is:

     FeS2 + 2.4875 02 + 0.175 H2SOit + 0.25 Fe+2  + 0.75 Fe+3

                       + 1.375 SO^'2 + OJ75 H20  + 0.8S

It  is evident that sulfuric acid is consumed  when the removal  of iron forms
is  non-selective.   The baseline  design actually  adds enough sulfuric acid
that regeneration  to a Y =  1.0 could be  tested and  results in  additional
sulfuric acid makeup and discard as follows:

     FeS2 + 2.4875 02 + 0.3 \\2SOk  + 0.25 Fe+2 +  0.75 Fe+3 + 1.375 SO^

                       + 0.125 H2S04 + 0.175 H20  + 0.8S
3.2.1.2  Washing Section - The major parameters affecting the washing
section mass balance are the moisture content of filter cakes and the
effectiveness of spray-wash and repulping.  Based on vendor tests and bench-
scale filtration experience with Lower Kittanning coal of 100 mesh top-size,
the following design basis was formulated.  This coal (which is believed
to be typical of Appalachian bituminous coals) produces a filter cake which
has a liquid retention equal to 50% of the dry coal weight plus the weight
of dissolved salts.  For example, coal filtered from water has 50% liquid
but coal filtered from the 5% iron leach solution has 63.6% liquid because
the liquid contains 21.4% of dissolved iron sulfates and acid.

Cake washing appears to be best represented by considering the retained
liquid to be of two types.  "Pore" liquid is about 15% of the coal weight
                                    25

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plus dissolved salts.   Spray-washing on the filter, with water equal  to
1.4 times the water content  of the cake, appears to replace  substantially
all of the "surface" liquid  with wash liquid but does not change  the  "pore"
liquid.   The repulping step  has enough residence time that both the surface
and pore liquids equilibrate with the bulk liquid.

The nominal values of parameters used in the wash section mass balances
are:
     Filter cake pore water              15% of solids
     Filter cake surface water           35% of solids
     Filter spray-wash/cake water         1.4
     Repulped slurry concentration        33% solids
3.2.1.3  Toluene Section -  This  section  includes  azeotropic  drying  to
remove water, toluene washing to remove  sulfur, and  solvent  recovery.  Water-
wet filter cake is slurried with boiling toluene  and an  azeotrope of water
and toluene is removed.   The azeotrope theoretically contains  55.6  mole
percent water.  But, because of  imperfect contact, it was  assumed that 5%
excess toluene would be  present  in  the azeotrope.

The toluene-coal slurries are separated  by centrifuges which operate
effectively with the large  density  difference  between coal and toluene.
A division of the centrifuge cake liquid into  "pore"  toluene and "surface"
toluene was made.  The pore toluene is assumed to be 13% of  the dry cake
weight plus dissolved sulfur.  The  13% is slightly less  than 15% water
owing to the lower density  of toluene.   The total liquid was found by
vendor test and bench-scale experience to be about 33% which results in
a nominal "surface" toluene of 20%.   Considering  the lower density,
viscosity and surface tension of toluene compared to water,  this value is
reasonable.  Spray-washing  in a  centrifuge is  less efficient than on a
filter and it was assumed that two  (rather than 1.4) times the cake
toluene will be needed to displace  the "surface"  liquid.

                                   26

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The sulfur-rich toluene solution  is purified by distillation (C-l).  The
still feed containing  about 2% sulfur is concentrated to 10% sulfur, then
cooled  in a  scraped  tube exchanger to give a slurry of sulfur in sulfur-
saturated toluene.   The saturated stream will have nominally 2.7% dissolved
sulfur  at 95°F.   At  pilot  scale,  the flow rate of this stream is so low
that  a  bypass  stream (64)  has been added to the filter feed to hold the
sulfur  cake  to the leaves  of the  filter.  Based on vendor experience,
the liquid flow through the sulfur cake should be about 0.15 gallons per
minute  per square foot of  filter area.

Toluene is also recovered  from the coal in the dryer.  In the nominal case,
it was  assumed that  no toluene is lost with the coal.  In practice, there
will  be a small loss and a corresponding amount of makeup will be required.
If 0.1% of the coal  weight is assumed to be absorbed toluene, then about
0.94  Ib/hr of  makeup is required.

Nominal values of parameters used in the toluene section mass balance
are the following:

      Centrifuge cake pore  toluene         13% of solids
      Centrifuge cake surface toluene       20% of solids
      Centrifuge spray-wash/cake  toluene    2.0
      Repulped  slurry concentration         33% of solids
      Sulfur  in still bottoms               10 wt.%
      Sulfur  solubility of  filtrate         2.7 wt.%
      Filtrate  flow rate                    0.15 gpm/ft2
      Azeotrope-actual  toluene/             1.05
                  theoretical
      Steam for stripping toluene  in        260 Ib/hr
                  dryer

3.2.2.   Mass Balance

 The nominal  mass balance  for the pilot plant is given in Table 1.  The
flow rates are given for each of  the 64 streams as numbered on the flow-
sheet in Appendix A.   Table 2 correlates all  feed and product streams to
their composition and service.   Stream 47 shows that the coal product
                                    27

-------
                                          TABLE  1.   PILOT PLANT MASS BALANCE
ro
oo

STREAM NO.
COAL .
PVRITE
i Su LFUK
FES04
FEIS04»1.5
HZS04
MATER
TOLUENE
OXYGEN
INERT GAS
COAL
PYRITE
SULFUR "~
FES04
FE (S04)1.5
H2SD4
HATER
TOLUENE
QXTI>£N
INERT GAS
TOTBCTTT. -

1
72.3179
.4990
o.uuou
0.0000
0.0000
0.0000
5.5506
0.0000
0. ITU 00
0.0000
940.13
59. 87
~D™. TO
0.00
0.00
O.BO
100.00
0.00
	 O.OTJ
0.00
[iOD.ua

2
a.ooaa
o.aaao
.8953
2. £858
160.6976
0.0000
0.0 OHO
0.0000
0.00
o.ao
a.ou
136.00
537.02
57.55
2895.13
o.aa
0.00
a. oa
3626. OTJ
3
~FLawnw
0.0000-
0.0000
0.0000
0.0000
o.oaoo
0. OODO
15.2087
0.0000
ovoooa
o.oooa
TTD1TTW
a. oo
a. ao
TT70U •-'
0.00
0.00
U.OTT 	
274.00
9.00
0.00
0.00
274. Q"0

4
iftt LB-HOLAHR
7^.3179
.0695
1.7808
1.8870
181.0402
o.aaao
"0.01100 "
0.0000
TT; L3/w
944.13
49. .45
	 2.23
270.54
377..31
93i73
3261.62
0.00
-ir.w
0.00
5 4 0 
-------
                                      TABLE  1  (Continued).   PILOT PLANT MASS BALANCE
ro
to

STREAN NO.
COAL
PYRIfE
1 SULFUR
FES01
FE (SOD 1.5
H2S01
HATER
TOLUENE
OXYGtN
INERT GAS
COAL
PYRITE
SULFUR
FES01
FE (SOI) 1.5
H2S01
WATER
TOLUENE
OXYGEN
INERT GAS
TOTAL HI .

9
0.0000
0.0000
• U.UOUD
0.0000
0.0000
u.oooo
.0037
0.0000
. 0559
.0057
0.00
0.00
a. UB
0.00
0.00
a. oo
.07
0. 00
1. 79
.20
2. 0^
10
72.3179
.0818
.3337-
.1336
3.5616
.Z33S
171.5970
0.0000
oiornnr
0.0000
910.13
9.82
n.ro
65.86
712.71
3115.51
0.00
fl.OD
0.00
- 1W7.7T
11
I-LUN
0.0000
o.oooa
u.uyuo
0.0000
0.0000
O.DUUU
8.3259
0.0000
0.0000
o.oooa
FLOH
a. oo
3.00
o'ao
o.oa
u.uo
150.00
o.oa
o.oa
ibu.aa
12
MA It. LB-HOL/H
72.3179
.0818
.3337
.1336
3.5616
166.2711
0.0000
o.oaoo
0.0000
RATE. L3/HK
910.13
9.82
10.70
65.86
712.7*
2995lsi
0.00
U.UU
0.00
irb t *f i

13
\K"~
72.3179
.0209
.3792
1.013*
3.0113
.5069
165.9980
0.0000
~ O.OTJuO"
0.0000
910.13
2.99
1Z.16
151.01
608.10
2990.62
0.00
TJ.TIII
o.oa
1757.73



	 PAGE 2 Qf~,S
11 15 16
o.aooo
a. oooo
DVD ODD
.0000
.0000
• nzz
-.1715
0.0000
TTTOOOB
0.0000
O.OQ
o.oa
o.ou
.00
.00
11.95
-3.11
0.00
r.iro
0.00
ITT.BTJ ~ ~
a. ooao
0.0000
u.oooo
.0*31
.1302
. OZ17
11.1711
a. oooo
"T.mnnr
o.oooe
.0.00
0.00
0.00
6.59
26.01
2.13
255.36
0.00
u.uo
o.ao
~29Tin.2
0.0000
0.0000
u.AODfl
.0*3*
.130?
.1639
13.9995
0.0000
a. good
0.0000
0.00
0.00
0.00
6.S9
26.01
252.22
0.00
a. OB
0.00
3D0.9Z

-------
                                         TABLE  1  (Continued).   PILOT PLANT MASS BALANCE
CO
o
STREAM HO.
COAL
PYRITE
SULFllli
FES04
FE (504)1.5
H2SD4
HA TER
TOLUENE
INERT GAS
COAL
PTRITE
SULFUR
FES04
FEIS04I1.5
H2S04
MATER
TOLUENE
OXTGtN
INERT GAS
17
0.0000
0.0000
U.DOOO
' .8953
2.6858
.5898
153.4854
0.0000
0.0000
0.0000
0.00
0.00
	 D.Tnr
136.00
537.02
b/.«5
2765.19
0.00
	 ffiOTT
0.00
18
0.0000
0.0000
H.OODO
.0703
.2108
.0351
22.9429
0.0000
0.0000
0.0000
0.00
0.00
0.00
10.67
3.45"
413.34
• 0.00
TJ.TJO
0.00
19
FLOH
0.0000
0.0000
O.UOOO
.8518
2.5555
.4259
139.4859
0.0000
0.0000
0.0000
I-LUH
0.00
0.00
0.00
129.41
510.98
«i. ra
2512.98
0.00
u.uu
0.00
20
21
TTCTE, CB-HOT.7HIT
0.0000 72.3179
0.0000 .0249
0.0000
.1137
.3410
.0566
37,1170
0.0000
0.0000
0.0000
KAIEt LB/HR
0.00
0.00 '
O.DD
17.27
68.18
668.70
0.00
U.UU
0.00
.0494
.1*82
26.5122
0. 0000
"" "O.OOBT)
0.0000
940.13
2.99
1Z.T6
7.50
29.63
2.4Z~
477.64
0.00
O.TJO -
0.00

22
0.0000
0.0000
0.0000
.0011
.0034
.0006
37.1170
0.0000
o.auuo
0.0000
0.00
0.00
o.ao
.17
.69
.06
668.70
0.00
o.uo
0.00

P»BE 3
23
0.0000
ii.onoo
u.uuuu
.0025
.0074
• D01Z
79.5365
0.0000
a. OODO
0.0000
0.00
If. 00
0.00
.37
1.47
1432*93
u.oo
0.00
0.00

OF a
24
72.3179
.0249
.3792
.0518
.1555
106.0486
0.0000
Q.OOOD
0.0000
940.13
2.99
12. 16
7.88
31.10
2.54—
1910.57
0.00
O.OD
0.00
                 TOTAt
                             TW6.W
                                        469.60
                                                      14
                                                                       IV7Z.48
                                                                                                      Z9U7.3/

-------
                                     TABLE 1 (Continued).  PILOT  PLANT MASS BALANCE
CO

STREAM NO.
COAL
PYRITE
SULI-UK
| FES04
; FE
-------
                                        TABLE  1  (Continued).   PILOT PLANT MASS BALANCE
CO
ro

STREAK NO.
COAL
PYRITE
FES04
FEIS04I1.5
H2SD4
HATER
TOLUENE
INERT 6»S
COAL
PVRITE
SULFUR
FES04
FE (504)1. 5
HATER
TOLUENE
OXTGtN
INERT GAS

33
72.3179
.0249
-.0003
.0009
.0001
26.5122
0.0000
0.0000
0.0000
940.13
2.99
12.16
.04
.17
.Ul
477.64
0.00
0.00
0.00

34
0.0000
0.0000
.0430
0.0000
0.0000
0.0000
0.0000
42.7015
0.0000
0.0000
0.00
0.00
1.38
0.00
0.00
0.00
0.00
3934.56
U.UU
0.00

35
h LUW
0.0000
0.0000
U.UUUl)
0.0000
0.0000
u.uuuu
Z6.51ZZ
ZZ.Z302
a.ouuu
0.0000
I-LUW
3.00
0.00
0.00
0.00
0.00
U. nu
477.64
2043.31
0.00

36
HATE, LB-HOL/HR
72.5179
.3249
.<*2ZZ
.0003
.0009
.0001
0.0000
20.4714
0.0900
0.0000
KAIt, L'J/HK
940.13
2.99 •
.04
.17
. (Jl
0.00
1486.25
O.OU
0.00

37
0.0000
0.0000
.3736
0.0000
0.0000
J.TIOuD
0.0000
23.8491
B.Trono~
O.OOOQ
0.00
0.00
~TI.9B
0.00
0.00
U.DO
0.00
2197.48
~0.00
0.00

38
0.0003
0.0000
U.UUUU
0.0000
0.0000
0.0000
0.0000
6.7555
V.UDOU
0.0000
0.00
0.00
u.uu
0.00
0.00
o.ao
o.oa
622.46
0.00
0.00

p»i»e 5 OF a
39
72.3179
.0249
!oOQ3
.0009
.0001
0.0000
3.3778
o.uuua
0.0000
940.13
Z-.99
1.56
.04
.17
.Ul
0.00
.111.23
u.uu
0.00

40
0.0000
0.0000
o.oou
0.0909
9.9*09
a.oaofl
a.oooo
17.0936
n.Bvot
0.0999
0.00
0.00
fl.tfO
0.00
0.00
a. oo
o.ao
1575.02
0.00
0.00
                     TOTAL TTT."
                                           3935.9T.

-------
                                        TABLE  1  (Continued).  PILOT PLANT  MASS BALANCE
CO
CO
PAGE 6 OF 8"
STREAM 40.
— 	
COAL
PYRITE
StTLUJK "
FES04
FE1S04I1.5
HZS04" "~ "
MATER
TOLUENE
UXTUtN . ~
INERT GAS
	
COAL
PYRITE
SUEFUK '"
FES04
FE (504)1. 5
H2STT4 	
MATER
TOLUENE
OXTGE1T - "-
INERT GAS
41
—
72.3179
.0249
~ .0486
.0003
.0009
70001
a. oooo
20.4714
0.0000
3.0000
._.
340.13
2.99
~ r.56
.04
.17
.HI"
0.00
1886.25
— TT.OTI
0.00
42

0.1)000
0.0000
. 0470
0.0000
0.0000
a. oooo
0.0000
23. 8491
0". 0300
0.0000
- -
0.00
0.00
173U
0.00
0.00
0.TTB
0.00
2197.48
o.trtr
a. DO
43
TT.OW
o.aooo
0.0000
" u.uauu
0.0000
0.0000
OVOBW
a. oaoo
6.7555
~o.Tnnro"~
0.0000
	 -TLDH
a. oo
a. oa
D.OT
0.00
o.oo-
" Dvmr
3.00
622.46
- o.oo
0.00
44
RATtt LB-HOL/HR
72.3179
.0249
	 .BB5B
.0003
.0009
^OODl
0.0000
3.3778
O.OTTIJO
0.0000
TOSTE, LB/HR
943.13
2.99
.18
.04
..17
.01'
3.00
311.23
O.OT)
0.00
45

J .0000
o.aooo
0.0300
a.ooaa
a. oaoo
3.0000
a.aooa
30.6047
0.0003
a.aooa

0.33
0.00
0.00
o.oa
0.00
0.00
0.30
2819.95
0.00
0.00
46

a. oooo
3.0003
a. on oo
0.0000
0.0000
O.TJODT!
153.7705
0.0000
O.ODBO
0.0000

a. oa
3.00
O.TO
o.oa
o.oa
TT. OTT
2770.33
0.00
a.tro
o.oa
47
-, —
72. 5179
.0243
73056
.0003
.0009
— .QBT11
0.0000
0.0000
O.TBOIT
a. oooo
-
943.13
2.99
" " ilB
.04
.17
-... --jj^
J.OO
a. ao
O.ffB'
3.00
40

0.0000
0.0000
-o.Trmnr
a. oooo
a. oaoo
OVBTJOff
3.0000
0. OOOO
"O.TJODTJ
a.ooaa

a.oo
3.00
~ D.TIO
0.00
3.00
0.00"
0.00
.3.30
U.OO
0.00
                      TOTAL ₯T.
                                            2198.35
                                                                 1Z54.77
                                                                            2819.95
                                                                                      2770.33
                                                                                                              O.OH

-------
                                     TABLE 1 (Continued).  PILOT PLANT MASS  BALANCE
to
STREAK MO.
COAL
PYRITE
au ir UK
FESO<»
FEIS04I1.5
MATER
TOLUENE
OXVGit.pl
INERT GAS
COAL
PTRITE
SULF'UK
FES04
FECSUI1.5
wzsm 	
HATER
TOLUENE.
UXTbtN
INERT GAS
0.0000
0.0000
JB. UUDU
0.0008
0.0000
u. uuuu
0.0000
3.3778
Tj.Tnroo
o.ooao
0.00
0.00
~ Bnnr~
0.00
0.00
•~ U.OTT
0.00
311.23
0.00
0.00
50
a. oooo
o.oaoa
U.OOUD
0.0000
o.ooao
u. uuua
0.0000
a. aooo
u.uono
o.aooo
0.00
0.00
TT.TrO
0.00
O.OB
" O'.DTJ "
0.00
' 0.00
0.00
0.00
n it n
51 52
FLOW RATE; ta-HOt
a. oooo - o.aooo
u.aoao o.oooo
a.ooao
a.oooo
a.oooo
o.uooo
0.0000
22.2302
u.oouu
0.0000
hLUH
0.00
0.00
0.00
0.00
0.00
	 0.0TT
0.00
2043.31
II. Mil
0.00
• "J II .. II J« •
u.uuuu
0.0000
0.0000
0.0000
26.5122
0.0000
B.ffOOO
0.0000
KftlL, LB/HK
0.00 .
0.00
D.OD
0.00
0.00
«»77. 6<»
0.00
.... — p-.Tnr
0.00
53
/HR
0.0000
o.oooo
B . omto
.0036
.0108
.on a
116.6535
0.0000
g.omm
o.oooo
0.00
0.00
U.THJ • —
.55
2.16
.IV
2101.63
0.00
u.oo
0.00
"y * mr t;i
0.0000
0.0000
* TJ.TTOmi ~
Ho.6535
0.0000
o.ooon
0.0000
0.00
0.00
~ ~Tr.TTO —
7.29
28.77
2101.63
0.00
0.00
0.00
TTEIT' TTT1 "
55
o.oooa
a.oooo
u. uuuu
0.0000
o.aooo
U.DUUU
0.0000
13.8521.
a. uuuu
a. aooo
a. oo
0.00
0.00
0.00
0.1)0
0.00
1737.08
~ ~ TT.TTO
0.00
- 1 r t/.nn
56
0.0000
0.0000
l.bdl.1
0.0000
0.0000
u.uuuu
0.0000
29.11<>5
u.0ttti§
0.0000
0.00
0.00
0.00
0.00
~ inini
0.00
2682. 6J tK.BI. '

-------
                                    TABLE  1  (Continued).   PILOT  PLANT  MASS  BALANCE
CO
01
STREAN NO.
COAL
PYRITE
SULFUR
FES04
FE (504)1.5
H2S1T%
MATER
TOLUENE
OX YUEN
INERT GAS
COAL
PYRITE
iULFUH
FES04
FECS04I1.5
HZ304
MATER
TOLUENE
OXYGEN
INERT GAS
57
0.0000
0.0000
. 3 . 63 75
0.0000
0.0000
U.GUttU
0.0000
45.6188
O.DOOD
0.0000
0.00
0.00
Ilfa.b4
0.00
0.00
o. ao
a. oo
4203.36
0.00
0.00
58
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
23.8491
O.ODOO
o.ooao
0.00
0.00
ovoo" -
0.00
0.00
o. on
0.00
2197.48
tr.uo'
0.00
•rrr nT— r"a~ — • —
59
1-LlJw
3.0000
0.0000
U.Oudu
a. ooao
a.oaao
u.uouu
0.0000
49.4571
u.ouuu
a. oooo
I-LDH
a. oo
a. oa
D.DD
a. ao
0.00
0.00
o.oa
4457.02
	 onnr-
0.00
60
Kftltt UB-HOL/HK
0.0000
0.0000
0.0000
0.0000
u.auoo
0.0000
5.2653
u.uuuu
0.0000
KAIt, LB/Hk
0.00
0.00
53.91
0.00
0.00
0.00
0.00
485.15
TT. 00
a. oo

61
0.0000
0.0000
.3736
0.0000
0.0000
ff.OOOTT
0.0000
0.0000
V.OfTOO
a. oooo
0.00
0.00
11.98
0.00
0.00
a. DOT
O.OD
0.00
a. ao
0.00
»-l — nn

62
0.0000
0.0000
!l!82
.3546
139.5964
0.0000
0.0000 ~
0.00
o.oa
0.09
17.96
70.91
5.80
2514.97
0.00
uruo
0.00

PAbfc It
63
0.0000
o.ooao
o. liuau
0.0000
0.0000
U.UDHO
26.5122
0.0000
O.TTOT10
0.0000
•o.oo
0.00
O.OD
0.00
0.00
u.uu
477. «i4
a. oo
U • Q 0
0.00

OF B
64
0.0000
0.0000
Z.33DO
0.0000
o.OMa
O.ODBB
0.0000
40.3534
a.DvoO
a. 0000
0.00
0.00
fn.tt
0.00
o.oa
0.00
0.00
3718.21
	 O.UD
0.00

-------
                                       TABLE 2.  FEED AND PRODUCT PROCESS STREAMS
Stream No.
Service
Composition
Ib/hr
Coal
Pyrite
Sulfur
FeS04
Fe(S04)1>5
H2S04
Water
Toluene
(jityyan
Inert Gas
Total
Process Feed Streams
13 7 14 46
Steam to Leach Soltn. Wash Water
Coal Feed Mix Tank Oxygen Feed Makeup Feed

940.13
59.87



13.95
100.00 274.00 -3.14 2,770.33

19.11
0.20
1,100.00 274.00 39.72 10.80 2,770.33
Process Product Streams
11 18 47 61 62 63
Flashed Leach Soltn. Coal Sulfur Waste to Waste to
Steam to Disposal Product Product Disposal Disposal

940.13
2.99
0.18 11.98
10.67 0.04 17.96
42.14 0.17 70.91
3.45 0.01 5.80 *
150.00 413.34 2,514.97 477.64



150.00 469.60 943.54 11.98 2,609.64 477/64
CO

-------
(.944 Ib/hr) at 95% pyrite removal will contain the following-sulfur forms:

      Pyrite  sulfur                       0.17%
      Sulfate sulfur                      0.01%
      Elemental  sulfur                    0.02%

The mass  balance  also  shows  that the  makeup stream (14) contains 14 Ib/hr
of sulfuric  acid  and -3  Ib/hr  of water.  The  negative water means water
will  be  removed from the recycle loop.   In practice, significant quanti-
ties  of  water will be  evaporated into the vacuum  systems during filtration.
The water removed from the recycle  stream by  the  first barometric condenser
was not  included  in the  mass balance, but, from a separate estimate, it is
likely that  about 200  Ib/hr  of makeup water will  be needed.

The nominal  mass  balance given in Table  1 is  the  output from a computer model
of the process  written in Fortran for a  time-sharing computer.  The pro-
gram is  presented in Appendix  B.  The program also was used to examine the
effect of varying selected parameters on the  mass balance.  The resultant
calculated mass balances indicated  that  the largest differences in residual
sulfate  levels  tn the  product  coal  were  obtained  In runs where the
"pore" water on the filter cakes was  increased from the 15% nominal to
25%.   The sulfate sulfur increased  from  0.01% to  0,03%.  Similarly,
increasing the  "pore"  toluene  from  the nominal 13% to 25% increased the
elemental sulfur  from  0.02%  to 0.05%.

Other changes influenced stream  sizes and compositions, but had little
influence on the  coal  product.   It  was found  that, as the percent iron
in the leach solution  is decreased  from  5% to 2%, stream 20 contains
insufficient iron to dispose of  the reaction  product, thus requiring
that  a portion  of stream 19  be bled off  for disposal.  It was concluded
that  the  sizing and arrangement  of  the pilot  plant equipment and piping
should readily  accommodate the anticipated variable studies which are
discussed in the  test  plan.
                                     37

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3.2.3  Additional  Equipment  Criteria


For some of the major items  of equipment a brief description of additional

design parameters  are included in the following paragraphs:



      Coal  Pulverizer System (A-3):   the design rate for the coal  pul-
      verizer is 1000 Ib/hr.   Feed size is  1-1/2 in.   The unit is  designed
      to produce material 100% minus any required standard screen  size
      from  8 mesh to  100 mesh by changing the screens in the sieve unit
      or by changing  conditions in the pneumatic classifier.  The  unit
      is designed for operating under a nitrogen rich,atmosphere and
      will  vent excess purge gas through fabric filters for dust removal.

      Ground Coal Storage Tank (T-l): the ground coal storage tank is
      designed  for storage of 2-1/2  day supply of coal  based on a  consump-
      tion  rate of 1000 Ib/hr.

      Nix Tank  (T-2):  the slurry mixer is  designed to provide 15 minutes
      residence time  in each of three agitated stages so as to remove any
      foam  formed due to release of carbon  dioxide from reaction of car-
      bonate minerals with the acidic leach solution.
      The mixer is circular in cross section and operates 80% full with
      the length of each compartment approximately 80% of the diameter.
      The slurry cascades from stage to stage through an adjustable
      baffle (to reduce residence time) so  as to provide complete mixing
      in any one stage but prevent return of the slurry to an upstream
      stage.  Any gas evolved is evacuated  with a blower after first
      scrubbing with  incoming leach  liquor  to remove foam and finally
      scrubbing with  plant cooling water to remove traces of entrained
      material  from the first scrubber and  any visible water vapor.  Any
      possible entrainment is estimated to  add less than 1% of additional
      dissolved solids to the normal level  of approximately 1230 PPM total
      dissolved solids already present in the plant cooling water.

      Primary Reactor (R-1):   the primary reactor is designed for a hold-
      up of 5 hours operating 80 to  90% full.  Design pressure and tempera-
      ture  are 120 psig and 275°F with nominal operating conditions of
      50 psig and 250°F.


     Secondary Reactor (R-2):  the  secondary reactor is designed for a
     residence time  of 24 hours  operating  100% full.  The purpose of
     the secondary reactor is to complete  the conversion of the pyrites
     in the presence of leach liquor which has reached a relatively high
     level  of regeneration  in the primary  reactor.  The secondary re-
     actor  is  baffled to reduce  back mixing and to promote plug flow
     through  the  reactor.
                                   38

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Oxygen and Slurry Recirculation (P2A to J and K-1):  recirculated
oxygen is introduced into the discharge line of a reelrculating
pump connected to each compartment of the primary reactor.  The
pumps are designed to recirculate the contents of a reactor stage
about once every 9 minutes.   Sufficient oxygen recirculation
capacity is provided to feed  a volume of gas up to 1/2 the liquid
flow.

The oxygen is recycled and the inerts allowed to concentrate from
0.5% in the makeup oxygen (99.5% oxygen) to about 10% inerts
in the recirculating gas  (90% oxygen, dry gas basis).  The inerts
are then bled to atmosphere after scrubbing to remove steam and any
traces of entrained solids.

Fi 1 ters(S-2, S-3, S-4);  the filter section is comprised of three
types of filters.  The size of each filter, based on laboratory
filtration tests, is 40 sq.ft.

Slightly different types were selected so that a comparison could be
obtained on almost identical  slurries for future full-scale plant
filter selection.  Types of filters are as follows:

     (1) Standard rotary drum

     (2) Belt filter (to determine if back washing the
         filter cloth to prevent blinding is useful)

     (3) High speed rotary drum with blow-back cake
         discharge

Two of the filters will be equipped with separate filtrate and wash
water separators.  All the filters will be equipped with wash water
headers and cake steaming headers.  All the filters are equipped
with separate vacuum systems  designed to handle four SCFM/sq. ft
of filter area at vacuum of 24 in. of mercury.

Wash Water Contactors (T-ll,  T-13);  the filter cakes from the first
two filters are repulped with hot water in agitated vessels.   The
purpose of the vessels is to  provide adequate time for extraction
of the soluble sulfates from  the pores of the coal.  A residence
time of 30 minutes is provided.

Azeotrope Still (T-14):  design of the azeotrope still is based on
sufficient hold-up time to allow for displacement of absorbed water
with toluene, and for adequate heat transfer surface.  The basis for
design is a heat flux of 15,000 btu/hr/sq.ft.  This fixes a jacketed
vessel size of about 500 gals, and a residence time of about 80 minutes.

Centrifuges (S-5, S-6):  coal is separated from the azeotrope still
and solvent contactor slurries using solid bovl centrifuges.  The two
units specified are 12 in. diameter by 30 in. bowl equipped  for
Washing the cake.
                               39

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      Solvent  Contactor (T-16):  the solvent contactor is designed for a
      30-minute residence time.

      Solvent  Still (C-l):  the purpose of the solvent still is to
      concentrate rich toluene containing about 2% sulfur up toJO/o
      sulfur in the still effluent.  The still is a 200-gallon jacketed
      vessel sized to provide the required duty at a flux of 10,000 btu/
      hr/sq. ft.

      Sulfur Removal (E-9, S-7, S-8):  the toluene-sulfur solution from
      the  still is cooled to 95°F in a scraped surface cooler and the
      discharge containing the solidified or crystallized sulfur is
      pumped through a leaf-type filter and the toluene filtrate returned
      to the rich solvent surge tank.  The filter is periodically drained,
      blown dry with nitrogen and the sulfur cake discharged to a com-
      mercial  waste disposal bin located underneath.

      Dryer and Solvent Removal System (SP-4);  the toluene wet coal from
      the  final centrifuge is introduced through a screw conveyor into a
      rotary tray type dryer where the solids are contacted counter-
      currently with heated nitrogen (or steam).  The gas-toluene mixture
      from the top of the dryer is condensed and the toluene is returned
      to the process.

      The  coal from the exit of the dryer is cooled in a screw-type
      cooler and then elevated to the top operating level for loading
      the  coal into drums and removal to the storage area.

      Leach Products (T-24, T-25A and B):  ferrous and ferric sulfate
      formed from pyrite cTurfng the leach reaction are collected in waste
      disposal tanks along with dilute wash water which contains small
      quantities of iron sulfates.  Two 20,000-gal. polyester-fiberglass
      tanks are provided for collection of the waste material from six
      days of  continuous operation.  A separate stainless steel waste
      tank is  provided to dispose of water containing traces of dissolved
      toluene.  Both wastes will periodically be collected by commercial
      waste disposal firms.


 3.3  MATERIALS OF CONSTRUCTION


 Selection of  materials of construction for the various  pilot  plant equip-

 ment  and  hardware was based on (1) knowledge of the state of  the art of

 materials applications and (2) materials compatibility  studies  carried

 out by TRW as part of EPA Contract No. 68-02-1336.  The construction

 materials selected for utilization in all sections of the  pilot plant
facility  except those  in  hot  leach solution-coal slurry service were
                                    40

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determined through application of materials technology knowledge with
verification from equipment and hardware suppliers..  The materials
compatibility studies were performed to evaluate a number of materials
in hot leach solution-coal slurry service.   This testing was necessary be-
cause of an extreme lack of available information in regard to corrosion
and/or erosion characteristics of construction materials in contact with
ferric-ferrous sulfate solution-coal slurries in the presence of gaseous
oxygen (as in the primary reactor and circulation loops) at elevated
pressures and temperatures.  Results of the experimentation indicated that
316L stainless steel is the preferred material under reactor simulated
conditions.  Type 304/304L stainless, a more common and less costly alloy,
gave variable results.  The higher risk of failure did not justify its use.
Armco 22-13-5 and Carpenter 20 Cb-3 appear to be more resistant than 316L
under test conditions.  Although these alloys are normally more costly,
either one could be substituted for 316L in a situation when it offers a
cost advantage or if required for meeting delivery schedule.

The specific materials selected for utilization  throughout  the facility
are detailed in the Pilot Plant Bid Book in piping and instrumentation
drawings and equipment specifications.  However, the following summary
does present the general philosophy of materials selection as applied to
the pilot plant.

     t  Mechanical equipment in acid (leach solution) service - 316L
        stainless steel
     •  Mechanical equipment in organic solvent service - carbon steel
     •  Mechanical equipment in sulfur service - carbon steel
     0  Vessels and tanks in dilute acid, water, aqueous waste, or
        ambient leach solution service - fiberglass reinforced
        polyester
     •  Vessels and tanks in organic solution (including dilute
        organic waste solutions) service - carbon steel
     •  Vessels and tanks in hot leach solution service - 316L
        stainless steel
                                    41

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•  Piping in leach solution (concentrated and dilute)  service •
   316L stainless steel
•  Piping in oxygen service -  316L  stainless  steel
•  Piping other than that  in leach  solution and  oxygen  service
   carbon steel.
                            42

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             4.  PILOT  PLANT  START-UP AND OPERATIONAL VERIFICATION

 The  process  of initiating  pilot  plant  operation will include personnel
 familiarization with the facility,  initial  start-up and shut-down for the
 purpose  of functionally testing  all associated process equipment and tech-
 niques during  plant operation, and  the performance of an operational veri-
 fication test  run.  Necessary modifications  to the operational procedure
 and  to the plant itself will be  made during  the start-up period.  It is
 anticipated  that 3 months  will be required  to carry out the systematic
 start-up and verification  testing of the pilot unit and that this effort
 will  immediately precede pilot plant testing (Figure 1).  A schedule,
 detailing the  start-up and operational verification, is presented as
 Figure 2.

 4.1   PERSONNEL TRAINING

 The  initial  task of the start-up operation,  personnel training, will have
 as its primary goal the safe and orderly execution of the first pilot plant
 start-up and shut-down,  To  facilitate the achievement of that goal, all
 operating, laboratory  and  engineering  personnel will be familiarized with
 all  start-up and shut-down procedures, both  normal and emergency.  The
training procedure will consist of operating manual  study, safety manual
study and  on-site Inspection of the processing equipment and area to
familiarize  personnel  with types and locations of processing equipment,
valves,  service  facilities,  instrumentation and control  hardware, effluent
monitoring equipment and emergency control  points.

As indicated in  Figure 2,  the above mentioned training program will be
carried  out  over a 1-month time  period with  the second half of the program
overlapping  the  initial testing  of  the Coal  Feed  and Reactor Sections of
the process.   The familiarization program will, therefore, be organized to

                                    43

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                                                 MONTH OF OPERATION
Plant Start-Up
Operational Verification
Operation on 1st Coal
Operation on 2nd Coal
                         Figure 1.  Pilot Plant Operation Schedule

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                     ACTIVITY
                                                        5    1.0   1.5   2.0   2.5   3.0
START-UP AND OPERATION VERIFICATION
TRAINING OF PERSONNEL IN START-UP, SHUT-DOWN
     AND EMERGENCY PROCEDURES
FILL REACTOR SECTION WITH PROCESS WATER AND
     CHECK OPERABIL1TY (LESS OXYGEN COMPRESSOR)
OPERATE OXYGEN COMPRESSOR AND CHECK
     OXYGEN CIRCULATION
OPERATE COAL FEED SECTION AND GRIND FIRST
     COAL CHARGE
DRAIN PROCESS WATER
MAKE REQUIRED ADJUSTMENTS,  REPAIRS OR MODIFICATIONS
FILL REACTOR SECTION WITH DISTILLED WATER, FEED COAL
     AND CHECK SLURRY OPERATION THROUGH WATER WASH
     OPERATIONS (SULFATE REMOVAL SECTION)
CHARGE ORGANIC SOLVENT SECTION INCLUDING CARBON
     ADSORPTION EQUIPMENT AND CHECK OPERABILITY
     (LESS SOLVENT STRIPPER OPERATIONS) WITHOUT
     COAL FEED
FEED COAL AND CHECK SLURRY OPERATION THROUGH
     TOTAL SYSTEM (INCLUDING SOLVENT STRIPPER
     OPERATIONS)
MAKE REQUIRED ADJUSTMENTS,  REPAIRS OR MODIFICATIONS
GRIND SECOND COAL CHARGE
INITIATE FIRST TOTAL START-UP OF PLANT AND EXCHANGE
     DISTILLED WATER FOR LEACH SOLUTION
ANALYZE RESULTS OF  FIRST START-UP, EVALUATE COLLECTED
     DATA AND MAKE FINAL ADJUSTMENTS, REPAIRS OR
     MODIFICATIONS
PERFORM VERIFICATION START-UP AND CONTINUOUS FIVE
     DAY OPERATION AT FULL PLANT CAPACITY
                         Figure 2.   Pilot Plant Start-up
                                      and Operational  Verification
                                         45

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concentrate all  training associated with  these  two  processing  sections
during the first half of the  schedule with  the  remainder  of  the  processing
sections being covered during the  overlap period.

4.2  PILOT PLANT START-UP OPERATIONS

Following personnel  training, the  initial start-ups,  short-term  operations
and shut-downs of the processing sections will  be performed.   The  primary
goal of these operations is  to check out  equipment, personnel, procedures,
analytical techniques and overall  operability of the  integrated  system.
The initial start-up will require  elongated time schedules to  allow for
greater process  control  and more in-depth procedure and equipment  evalu-
ations than will be  required  during subsequent  start-ups.  During  plant
start-up and subsequent  operations, the process will  be segregated into  the
following functional processing sections  (equipment numbers  are  from the
flowsheet):

                             COAL  FEED SECTION
         Belt Feeder (A-l)                    Weigh Belt  (A-5)
         Apron Feeder (A-2)                   Storage Tank (T-l)
         Pulverizer  (A-3)                    Dust  Filter (S-l)
         Bin Discharger(A-4)                  Dust  Blower (B-l)
         Coal  Hopper (A-8)                    Rotary  Valve (SP-8)

                              REACTOR SECTION
         Primary Reactor  (R-l)                Flash Drum  (T-4)
         Slurry  Mixers (M-2a/J)               Cooling Water  Drum (T-5)
         Knock-Out Drum  (V-l)                 Pumps (P-2a/j, P-3)
         Oxygen  Recycle Compressor (K-l)      Feed Mix Tank  (T-2)
         Secondary Reactor (R-2)              Feed Tank Mixers (M-la/c)
         Cooling Water Drum (T-3)             Scrubber Blower  (B-2)
         Feed  Pump (P-l)                      Scrubber (SP-1)
         Secondary Reactor Mixers  (M-12.M-13)
                                    46

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                          SULFATE REMOVAL SECTION
    Thickener (R-3)
    Hydroclone (SP-2)
    Make-up Tank (T-6,7)
    Thickener Discharge Pump (P-4)
    Leach Solution Surge Tanks (T-9,
    Surge Tank Pumps (P-6,7)
    Evaporator Crystallizer (SP-3)
    Wash Water Contactors (T-11,13)
    Contacter Pumps  (P-10,13)
    Surge Tank Pump  (P-19)
    Hydroclone Surge Tanks (T-26,27)
    Hydroclone Mixers (M-10,11)
    Hydroclone Pump  (P-26)
     Receivers (V-2,3,4,5,6)
     Filtrate Pumps (P-8,11,14)
     Make-Up Tank Mixers (M-3,4)
     Make-up' Transfer Pump (P-5)
10)   Wash Water Pumps (P-9,12)
     Filters (S-2,3,4)
     Vacuum Pumps (K-2,3,4)
     Barometric Condensers (E-1,2,3)
     Contactor Mixers (M-6,7)
     Waste Disposal Tanks  (T-25A.B)
     Waste Transfer Pumps  (P-25)
     Wash Water Surge Tank (T-20)
                         ORGANIC SOLVENT SECTION
    Rotary Feeder  (SP-7)
    Azeotrope Still  (T-14)
    Still Mixer  (M-8)
    Solvent Centrifuges (S-5,6)
    Centrate Receiver  (T-15)
    Solvent Contactor  (T-16)
    Contactor Mixer  (M-9)
    Coal Cooler  (E-4)*
    Solvent Stripper (SP-4)*
    Azeotrope Still  Pumo  (P-15)
    Centrate Pump  (P-16)
    Contactor Pump (P-17)
    Surge Tank Pump (P-20]
    Waste Disposal Tank (T-24)
    Waste Transfer Pump (P-24)
     Coal  Elevator (A-6)*
     Stripper Condenser (E-5)*
     Stripper Decanter (T-18)*
     Still Condenser (E-6)
     Still Decanter (T-19)
     Surge Tank (T-21)
     Solvent Surge Tank (T-22,23)
     Solvent Still (C-l)
     Still Condenser (E-7)
     Solvent Cooler (E-9)
     Sulfur Filters (S-7,8)
     Solvent Surge Tank Pumps (P-21,22)
     Solvent Still Pump (P-23)
     Carbon Absorption Drum  (SP-5)
     Screw Conveyor (SP-6)
For purposes of discussion in this report, the above described sections

will be referred to as follows:


                  Section 1 - Coal Feed Section

                  Section 2 - Reactor Section

                  Section 3 - Sulfate Removal Section

                  Section 4 - Organic Solvent Section
*These items of equipment constitute the solvent stripping operation.

                                    47

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The estimated time required to perform all  of the necessary start-ups and
shut-downs, including anticipated equipment adjustment,  repairs and modi-
fications, is 1-1/2 months.  As shown in Figure 2, this  effort immediately
precedes the operational verification test  run.  It is anticipated that
all initial start-ups will be performed with the secondary reactor (R-2)
operating as an atmospheric pressure holding tank, and with all equipment
operating at low to moderate capacities on  the order of  250 to 500 Ibs/hr
coal feed equivalent.  The following paragraphs present  a description
of the Initial  start-up sequence.

During the initial week of start-up operations, the primary and secondary
reactors (R-l and R-2) will be filled to appropriate operating levels
with process water (simulating leach solution).  The aqueous effluent line
from the secondary reactor (stream 13) will be circuited to the leach
solution return line (stream 17) during this test operation, thus effecting
a  closed circulation loop around the knock-out drum (V-l), scrubber mist
eliminator (SP-1), slurry feed mix tank (T-2), primary reactor (R-l) and
secondary reactor (R-2). Section 2, with the exception of the oxygen
circulation equipment, will then be put into operation utilizing ambient
temperature process water at atmospheric pressure in the following manner:

     (1)  Start water flow through all scrubbers and check operability.
     (2)  Start all mixer motors and check  for operability,
     (3)  Start reactor recirculation pumps and check for operability.
     (4)  Start slurry feed pump, reactor discharge pump and check
          operability.

With Section 2 (less oxygen compressor) operating at ambient temperature
and pressure conditions, associated equipment such as pressure, temperature,
flow and level  controllers, valves, recorders and indicators will be
checked for integrated operability, as will be all instrumentation  circuits,
compressor cooling water circuits and seal  flush systems, etc.  After
achieving successful  operation of the Reactor Section, with  liquid  circu-
lating at ambient temperature and pressure, oxygen compressor  operations
will be initiated and oxygen system pressure will be increased to

                                    48

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approximately 50 psig.  At this point, such additional  items  as compressor
system integrity and pump seal operation will be checked.  Following suc-
cessful operation of the primary  reactor at 50 psig oxygen pressure and
ambient temperature, the process  water will be steam heated to approx-
imately 250°F where operation will be checked, as will  be sampling equip-
ment and techniques.  Section 2 will then be shut-down  (reverse order of
start-up).  During the  initial start-up of Section 2, no processing data
will be collected.

Also scheduled  (Figure  2) for operation during the first month of start-up
is Section  1.   The apron feeder,  feeder belt, rotary valve, pulverizer,
elevator, weigh belt, dust filter and dust blower will  sequentially be
started to  insure system integrity and operability without coal feed.  The
nitrogen blanketing system will also be tested to insure operability.
During this period all  associated equipment will be checked and the weigh
belt zero point will be verified.  Following the mechanical check of
Section 1,  coal will be fed onto  the apron feeder and transported to the
pulverizer where the first grinding operation will take place.  The
ground coal will then be transported to the coal storage tank (T-l), where
it will be  held until required for slurry operations.  A total of approx-
imately 30  tons of coal will be pulverized to -100 mesh particle size and
stored following an initial sampling of the pulverizer product to ensure
proper sizing.

During the  third week of start-up operations, Section 2 will  be drained
of process water utilizing the emergency dump lines and waste disposal
tanks (T-25A and T-25B).  The water will then be pumped from the disposal
tanks and returned to the process cooling water pond.  This operation will
ensure the operability  of the emergency dump system under non-slurry con-
ditions.  In addition to draining Section 2, any adjustments, repairs or
modifications to either Section 1 or 2 (indicated during the first start-up)
will be made during the second week of operations.  Additionally, the by-
pass lines between streams 13 and 17 will be removed and the washed coal
feed line (stream 33) to the azeotrope still (a solid transport chute)
                                    49

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will be diverted into dumpster waste containers.   This  modification to
normal flow will bypass Section 4 and allow simultaneous  operation of
Sections 1, 2, and 3 of the plant.   Also, the wash water  line to con-
tactor T-13 (stream 29} will be temporarily connected to  the output of
the wash water surge tank (stream 53) to allow for complete recirculation
of the aqueous streams with no make-up or blow-down.

The second month of start-up operations will  begin with the refilling of
Section 2 with purchased distilled water (not process water).  The reactor-
sulfate removal operations will then be started,  utilizing ambient temp-
erature distilled water and 50 psig oxygen pressure in  the primary reactor.
Section 2 will be started as previously discussed.  Section 3 equipment
will be sequentially started as the fluid (distilled water) flows from
one processing unit to another.  This sequential  start-up will ensure
against such problems as "dry dumping" (i.e., pumps operating with no
fluids in lines) and "slugging" (i .e., insufficient liquid levels in vessels
allowing air to mix with pumping fluid resulting  in two-phase flow).

As the distilled water fills the vessels in Section 3,  a  make-up of fresh
distilled water will be fed to Section 2 utilizing the  leach solution
make-up tanks (T-6 and T-7) and transfer pump (P-5).   This make-up will be
required until total recycle of the distilled water is  achieved, including
the recycling of water through all  wash streams.   During  the initial oper-
ation of Section 3 with ambient temperature distilled water, all associated
equipment such as gauges, controls, valves, sampling equipment, sampling
techniques, instrumentation, barometric leg condensers, vacuum pumps, water
systems, seal flush systems, etc,,  will be checked for integrated oper-
ability.   Also, the secondary processing equipment in Section 3, namely the
thickener and hydroclones, will be  operated at this point, only to demo-
strate mechanical  integrity and operability.   Following the ambient water
temperature operation,  the distilled water will be steam heated to
appropriate nominal  processing temperatures and circulated through
Section 3.
                                   50

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After the equipment is checked for operability under elevated temperature
conditions, Sections 2 and 3 will be ready to be slurry tested, utilizing
Section 1.  The weigh belt and rotary valve will be activated and pulver-
ized coal will be fed into the slurry feed mix tank (T-2).  A 20% coal-
distilled water slurry will be mixed and fed to the primary reactor.
During this mode of operation, special care will be taken to follow the
advance of the slurry through the process (over an approximately 2-1/2 day
period) with careful attention being paid to all rotary equipment seeing
slurry service for the first time.  During this start-up, an indication of
the time required for the slurry to reach steady concentration levels in
each processing unit will be obtained.  As slurry operation is attained,
all pumps will be checked for turn-down limits and bypass loop requirements
will be determined.  Filters and their internal wash-water spray systems
will be evaluated for operability and all solids transfer operations will
be checked.  The wet coal cake exiting the third filter (S-4) will  be
collected in dumpsters (utilizing a solids diverter valve in the coal cake
transport chute), sampled, and trucked to disposal sites.  After steady
state operation has been reached in Sections 1, 2, and 3, operating para-
meters will be recorded and samples will be withdrawn, analyzed, recorded
and reported as a water blank, noting such things as sulfate build-up in
the water (water soluble sulfate leaching from the coal).

Section 4 will undergo its first start-up simultaneously with Section 3
during the second week (Figure 2).  The primary objective of this  initial
start-up is to check liquid toluene circulation operations without intro-
ducing pulverized coal.  During its initial start-up, this section will be
separated and operated in a closed loop fashion.  This mode of operation
will be accomplished with the slurry feed port of the azeotrope still
(T-14) sealed.  Also, since no coal will be fed into the section, the
solvent wet coal cake transport chute between the last centrifuge (S-6)
and solvent stripper (SP-4) will be valved shut.  The solvent stripper
operations (SP-4, E-4, A-6, E-5, T-18) will not be started up until the
next run which will include process slurry operations.
                                    51

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Prior to operation, the carbon absorption  drum (SP-5)  will  be charged and
the entire section will be purged with  an  inert gas  (N2).   Extreme care
will be taken to ensure against the occurrence of flammable mixtures
(toluene-air) in this processing section.   The azeotrope surge tank
(T-21) and rich solvent surge tank (T-22)  will  then  be charged with
toluene.  The transfer pump will then be started and the remaining equip-
ment will be filled with solvent to the appropriate  level.  Make-up toluene
will be continuously fed into the lean  solvent surge tank (T-23)  until
continuous recycle of ambient temperature toluene is achieved.   The
section will be checked for operability and integrity under ambient
operation conditions and then steam header and cooling water circuits
will be put into operation, thus bringing the Organic Solvent Section to
nominal processing temperature operation.   While circulating process
temperature toluene, all associated equipment such as level, temperature
and pressure control equipment, instrumentation, lubrication systems, pump
and mixer seals, sampling devices and techniques, etc., will be checked
for operability.  At this point, the process sections in operation will
be shut down and the coal cake transfer chute between the final filter unit
and the azeotrope still (stream 33) will be reconnected as will be the
transfer chute between the last centrifuge and the solvent stripper
(stream 44).

The total processing unit, including the solvent stripper operations, will
then be readied for start-up with coal  slurry feed throughout the system
(utilizing water as the leaching solution) during the fourth week of
operations.   Prior to this start-up, a thorough check-out of the nitrogen
recirculating and blanketing system associated with  the stripper unit will
be conducted to ensure that all safety devices are operable.  Following
that precautionary measure, the total system will be started up sequen-
tially.  The slurry advance through Section 4 will be closely monitored  to
ensure operability of all rotating equipment seeing  slurry service for  the
first time.   Also, start-up of the stripper unit will be carefully watched
to ensure maximum safety of that potentially dangerous first-time  operation.
ftfter steady-state operation has been attained, feed, water,  solvent,
                                   52

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slurry and product coal samples will be collected, analyzed and reported
as blank run results (utilizing distilled water as substitute leach
solution in Section 2).  During this run, the product coal will be col-
lected in dumpsters and trucked to disposal.  The pilot unit will then
be shut down.

During the fifth week of operation, the pilot plant will undergo any
repairs, adjustments or modifications to Section 2 and/or Section 4 which
were indicated during test runs.  Also, the previously modified wash water
supply lines allowing total recirculation of wash water (detailed in the
Sulfate Removal Section start-up discussion) will be reconnected for normal
process operations.  This mechanical work may require some equipment to be
drained.  If this is the case, the equipment will be drained into the
appropriate waste disposal tanks for storage (T-24, T-25A, T-25B),
depending upon the nature of the fluid (i.e., organic or aqueous).  The
adjustments, repairs or modifications will then be made and the fluids
pumped back to their point of origin utilizing transfer pumps  (P-24, P-25).
Also, during the fifth week of operation, a second charge of coal  (approx-
imately 30 tons) will be pulverized and stored in the coal storage tank
(T-l).  The pilot plant will then be readied for the next start-up.

During the sixth week of start-up operations, the pilot plant  will undergo
an additional start-up and short-term (2 to 3 days) operation  for the
purpose of exchanging the distilled water 1n the Reactor Section with
leach solution.  The exchange will be accomplished by feeding  ferric
sulfate crystals directly into the feed-mix tank (T-2) through the pulver-
ized coal feed mechanism.  The operation will be carried out so as to
leave the reactor system filled with dilute leach solution (approximately
2%) and ready for the verification test and subsequent pilot plant oper-
ation.
                                   53

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During the start-up, all equipment seeing leach solution for the first time
will be checked for operability in that service.   Special  attention will be
paid to mechanical seals and seal  water flush systems.   As the distilled
water is exchanged for leach solution, samples will  be  collected and data
obtained on plant operation throughout the unit.   This  information will
serve as baseline data and indicate transient operational  effects and time
requirements.  The plant will be operated long enough to ensure that steady-
state operation is effected and then shut down.  During this start-up oper-
ation,the product coal and byproduct sulfate and sulfur will be collected
and temporarily stored at the test site.  The products  will eventually be
trucked to disposal.

During the seventh and eighth weeks of operation, the initial start-up pro-
cedures and all operational data gathered during previous runs will be
thoroughly analyzed as will be sample analysis results,  The test data will
be analyzed with respect to the units  capability of sustaining continuous
operation and attaining desired processing objectives.   Additionally, the
detailed test plan for initial pilot plant operation will  be reviewed and
modifications submitted for approval by EPA, if the  start-up test data and/or
operating experiences indicate changes in test sequence or schedule are
desirable.   Also, during this time period, any further adjustments, repairs,
or modifications to the processing unit will be made.

The plant will then be readied for a 5-day, full capacity  (1000  Ib/hr
coal feed)  verification start-up and continuous operation test.  Additional
coal will  also be pulverized and the coal feed storage tank (T-l) filled
to capacity.

4.3  PILOT  PLANT OPERATIONAL VERIFICATION

During the  final 2 weeks of the start-up and verification  operations
(Figure  2),  the pilot unit will be started up and continuously operated  for
a 5-day test period at  full design  capacity.   The probable processing
                                    54

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parameters to be utilized during this operation are:

           Coal feed rate                    -  1000 Ib/hr
           Coal particle size                -  -100 mesh
           Slurry concentration              -  20% coal
           Leach solution concentration      -  2% iron
           Reaction-regeneration temperature -  225°F
           Oxygen pressure                   -  50 psig
           Excess oxygen circulation         -  4 x consumption

The time period required for the system to reach steady-state operation
(after start-up) will be about 2-1/2 days.  This corresponds to the resi-
dence time of the coal in the system from coal feed storage tank (T-l)
through the solvent stripping unit  (SP-4).  The unit will then be operated
for approximately 2-1/2 days at full capacity.  During the start-up oper-
ation, the system throughput will be increased from the 250 to 500 Ib/hr
of coal feed equivalent previously  utilized to 1000 Ib/hr.  This will
require that additional leach solution, of appropriate concentration, and
toluene be fed into the unit during simultaneous increase of coal feed.
During the course of the operation  fresh coal will be pulverized so as to
maintain continuous coal feed.  Data on transient process operation will be
obtained during this operation.  While in operation, complete sampling
procedures will be performed at all sampling points.  All monitored oper-
ational data will be recorded.  The operational data collected and sample
analysis results obtained will be analyzed as soon as possible so that on-
line operational adjustment can be made during the course of the test.  All
data will be analyzed, recorded and reported following the test run and the
pilot plant will be approved for pilot operations.

At the conclusion of the test run, the process unit will be shut down with
all solid process effluents being collected and temporarily stored at the
site and liquid waste effluents being trucked to disposal.  Results obtained
during the verification test will be reviewed and changes in equipment and
procedure will be made where deemed necessary.
                                     55

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                          5.   PILOT PLANT OPERATION

 Following  start-up  and  operational verification,  the  pilot  plant will  be
 put  into operation  to characterize process  operability on two  coals.   The
 general philosophy  of plant  operation  will  be  to  operate initially on  one
 coal to completion  of a test matrix aimed at characterizing  both the unit
 operations within the plant  and  the applicability of  the coal  being tested.
 This operation  is expected to require  approximately 6 months of testing
 with an additional  month of  data evaluation.   The second phase of the
 test program  will involve the second coal and  require an estimated 3
 months for completion.   During the second phase of the test  program,
 emphasis will be placed on determining the  coal's applicability to the
 process.   Much  less effort  (than in the first  part of the test program)
 will be required to characterize unit  operations  within the  plant since a
 large number  of those operations are expected  to  be substantially inde-
 pendent of coal type.   Also, during the entire test program, the operational
 and  process chemistry testing to be performed  will be segregated into three
 categories:  (1) primary test variables,  (2) secondary test  variables, and
 (3)  supportive  process  monitoring.  The primary test  variables are those
 which are  independent of process operation  and will be varied for study
 throughout a  given  test run.  The secondary test  variables are those which
 are dependent upon  the  primary variables  and change when changes in the
 primary variables occur.  For instance, the slurry concentration (coal/
 leach solution) being evaluated  in the primary reactor (R-l) is a primary
 variable while  this variable's resultant  effect upon  operation of the coal
 feed-mix tank (T-2), secondary reactor (R-2) and  the  first filter (S-2) is
 a secondary test variable for which data  will  be  collected and evaluated.
 Supportive process  monitoring is that  monitoring  required to ensure de-
 sired, safe,  and environmentally acceptable process operation.   The primary
objective  of  the pilot  plant test program is to prove  out the technology
for chemical desulfurization of  coal in an  integrated, continuous, process
system.   That objective will  be  accomplished by (1) evaluate parametrically
each processing section and/or major piece  of  equipment with respect to its
operability on the  subject coals,  (2)  thoroughly  characterize all feed
                                     57

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materials, coal products, sulfur and sulfate by-products and all  other

effluent streams, and (3) generate sufficient quantities of products and

by-products for future large-scale testing evaluation.


The data obtained during the performance of the pilot plant studies will

be utilized as a foundation for:

    .(1)  Recommendation of techniques for efficient operation
          and design optimization of the process while achiev-
          ing maximum sulfur removal.

      (2)  Recommendation of techniques for minimizing capital
          and operational costs while maintaining optimum sul-
          fur removal.

      (3)  Recommendation of methods for ensuring environmental
          integrity and safe operability of the process.

      (4)  Generation of up-dated pilot plant flow sheets and
          equipment and material specifications with appro-
          priate continuous operation mass and energy balances.

      (5)  Generation of data to permit performance of sound
          process design and economic studies.

      (6)  Development of the methodologies for effective
          process system measurement and monitoring.

The following paragraphs describe in detail how the above mentioned objec-

tives will be met with respect to each major section of the pilot plant

(pilot plant sections as defined in Section 4.3 of this document) and pre-

sent  an anticipated test matrix and schedule of operation for utilization
during evaluation of the two coals.


5.1  EQUIPMENT TESTING AND ANALYSIS REQUIREMENTS


Presented in this section is a detailed description of the operating param-

eters  to be evaluated for the equipment in each of the four major processing

sections of the pilot plant.  Additionally, chemical analysis requirements

associated with operational  or process chemistry evaluations  are discussed.
                                    58

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5.1.1  Coal Feed Section Testing

The primary functions of this section are to deliver coarse coal, from the
coal storage pile to the pulverizing equipment (see process flow diagrams
in Appendix A) and transport the pulverized coal to the pulverized coal
storage tank (T-l).  Since it is anticipated that the mechanical oper-
ability of all equipment in this section will have previously been demon-
strated during start-up and verification operations, the only testing to
be performed in this section will be that of obtaining pulverizer input
and output and performing sieve analysis to ensure proper particle size
feed to the reactor section and periodically monitoring the pulverizer
system purge gas effluent for particulate.

5.1.2  Reactor Section Testing

In this section of the process the pulverized coal is mixed and wetted
with leach solution while maintaining minimum foam generation.  Also, the
pyrite contained within the coal is converted to elemental sulfur and
soluble iron sulfate and regeneration of the spent leach solution takes
place.

Anticipating that mechanical operability of all equipment will have been
previously demonstrated during pilot plant start-up and check-out, the
only equipment in this section  requiring thorough operational character-
ization is the slurry feed-mix tank (T-2), the scrubber-mist eliminator
(SP-1), the primary reactor CR-0» and  ^e secondary reactor  (R-2).  The
secondary  reactor  (R-2) will be characterized while operating both as a
holding tank (also simulating a large thickener), a true secondary
reactor with no regeneration taking place, and as scaled-up (approximately
10 times larger than R-l) primary reactor with regeneration.

Operational variables to be evaluated during reactor operation include
(1) coal characteristics,  (2) coal particle size, (3) slurry  residence
time (1-10 hours, controlled through slurry feed pump  (P-l) rate and
                                     59

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number of reactor sections utilized),  (4)  reaction temperature (220°F-275*F),
controlled by varying inlet slurry temperature and steam injection,  (5)  oxy-
gen partial pressure and circulation rates,  varied through  changes  in com-
pressor recycle, oxygen bottle pressure and  blow-down  pressure setting,
(6) mode of three phase (oxygen-coal-leach solution) mixing,  which  will  be
evaluated utilizing oxygen injection in slurry pump-around  loops, static
mixing and oxygen injected through gas  dispersion  agitators,  (7) slurry
concentration (coal/leach solution ratio), and (8) salt concentration in
solution.  The parameters to be evaluated  during slurry feed-mix tank (T-2)
operation are (1) coal characteristics, (2)  coal particle size, (3) slurry
residence time (15 min to 1 hr) which  will be varied through  the use of
liquid level control and feed rate, (4) slurry temperature  (180°F-215CF)
which will be varied by steam injection, and (5) mixer horsepower  require-
ments .

Sampling requirements during reactor (both R-l and R-2) operation will
include slurry samples drawn from each reactor section of both reactors,
with the coal being separated and analyzed for pyrite  and elemental sulfur
to determine degree of pyrite conversion to  sulfur and sulfate, and leach
solution being analyzed for ferric and ferrous ion to  determine degree of
regeneration.  The reactor (R-l and R-2) liquid effluent (slurry)  will
also be analyzed for trace materials to evaluate the problem of impurities
build-up in the leach solution due to recycling.  The  gaseous effluent
from the primary reactor (R-l) will be sampled prior and subsequent to the
knock-out drum (V-l) and analyzed for particulate  and  the presence of foam.
Sample requirements for slurry feed-mix tank (T-2) characterization include
(1) pulverized coal feed sampling to determine particle size distribution,
(2) coal slurry sampling from the feed-mix tank effluent (from individual
stages) which will be analyzed for pyrite  conversion  and examined to
determine degree of wetting and general slurry composition, and (3) gas
sampling from gas effluent lines running from the  feed-mix tank to the
scrubber mist eliminator (SP-1) which will be analyzed for carbon dioxide
content (carbon dioxide must be evolved prior to entrance into the reactor
section in order to minimize oxygen bleed requirements) and foam content.

                                    60

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In addition to the above, the effluent from the scrubber-mist eliminator
(SP-1) will be monitored for the presence of coal and acid mists and the
gaseous effluent from the blower (B-2) and aqueous effluent from the
cooling water drum (T-3) will be sampled and analyzed for particulate and
sulfate presence.  The oxygen blow-down will be sampled and analyzed for
impurities build-up with oxygen consumption then being determined by mass
balancing around the reactor (R-l).  Also, the cooling water drum (T-5)
effluent will be sampled and analyzed for particulate and acid content.

5.1.3  Sulfate Removal System Testing

The equipment in this section requiring thorough operational characterization
are the thickener (R-3), hydroclone  (SP-2), evaporator-crystallizer (SP-3),
filters (S-2,3,4) and wash-water contactors (T-11,13).  The remainder of
the equipment will require minimal characterization since mechanical
operability will have previously been demonstrated during start-up.

The thickener (R-3) will be operated either off-line or in parallel to the
secondary reactor (R-2).  Its ability to thicken the coal slurry, and hence
lower subsequent filtering duty, will be evaluated as a function of (1)
coal characteristics and particle size, (2) slurry residence time, (3) inlet
temperature and (4) slurry concentration (coal/leach solution ratio).  This
evaluation will require sampling of  thickener effluents (overflow and con-
centrate) and determination of coal-to-leach solution ratios.  The hydro-
clone (SP-2) will be operated in series with the secondary reactor (R-2).
Its ability to thicken the coal slurry will be evaluated as a function of
coal characteristics, slurry flow rate (i.e., residence time in the hydro-
clone), slurry composition (coal/leach solution ratio), slurry temperature
and coal particle size.  This characterization will be accomplished by
sampling hydroclone effluents (overflow and concentrate) and determining
coal-to-leach solution ratios.

The evaporator-crystallizer (SP-3) will be operated off-line and be
evaluated with respect to output product (crystalline iron sulfate salts)

                                     6]

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characteristics as a function of operation parameters.   Variables which
will be studied include (1) input leach solution composition, (2) feed
rate,  (3) operating pressure (sub-atmospheric to one atmosphere), and
(4) concentrate circulation rates.  Evaluation of the unit will  require
that concentrate samples be taken and that the crystalline product be
analyzed and chemically characterized.  Quantities of this by-product will
be  retained for future study.  Samples of the barometric condenser efflu-
ent will also be analyzed for particulate and sulfate presence for deter-
mination of any possible environmental impact.

The three filter stages (S-2,3,4) in this processing section will each be
characterized separately since they represent three different types of
filtration equipment (as discussed earlier in Section 3.0).  Each filter
will be evaluated while operating in each of the three positions of the
filtration sequence.  Filtration and wash efficiencies of each unit will
be  determined as a function of (1) input slurry concentration and tem-
perature, (2) coal characteristics and particle size, (3) drum speed
(i.e., cake thickness), (4) wash-water feed rate, (5) suction pressure,
and (6) filter cloth type.

In  general, all filter influents and effluents will require sampling and
analysis for complete characterization.  The slurry feed, filtrate, spent
solution and filter cake will be analyzed for iron sulfate to evaluate
wash and filtration efficiencies and determine the fate of the soluble
salts.  Additionally, the moisture content of the cake will be determined.
The wash water will also be analyzed for sulfate if it is not fresh, unre-
cycled (uncontaminated) water.  Also, the effluents from the vacuum pumps
(K-2,3,4) and barometric condensers (E-1,2,3) will be sampled and analyzed
for particulate and sulfate presence for evaluation of possible  adverse
environmental impact.

The wash-water contactors (T-11,13) will be evaluated with respect to
their ability to induce dilution of the soluble sulfate within the coal
matrix.  Operational  variables to be evaluated include (1) input cake
                                    62

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and diluent composition,  (2) temperature,  (3) coal characteristics and
particle size, (4) residence time, and  (5) mixer horsepower input.  Samples
will be obtained from input and output  streams with the coal being sepa-
rated from the slurry and analyzed for  sulfate presence to determine the
degree of sulfate concentration reduction  in the coal matrix.

5.1.4  Organic Solvent Section Testing

The primary functions of  this section of the process are to effect a sepa-
ration and recovery  of the elemental sulfur from the coal matrix, recover
the organic solvent  utilized in the extraction, and dry the product coal.
The equipment in this section requiring complete operational character-
ization are  (1) the  azeotrope still  (T-14), (2) the solvent centrifuges
(S-5,6),  (3) the solvent  contactor (T-16), (4) coal cooler (E-4), (5) the
solvent stripper (SP-4),  (6) the  solvent still (C-l), (7) the solvent
cooler (E-9), (8) the sulfur filters (S-7,8), and  (9) the carbon absorption
drum  CSP-5).  The remainder of the equipment in this section are auxil-
aries to  the major equipment cited and  require only mechanical operability
check-out during the start-up phase of  this program.

The azeotrope sttll  (T-14J will be evaluated with  respect to its ability
to effect essentially total displacement of the absorbed water on the
feed  coal cake with  toluene.  Variables to be evaluated include (1) coal
characteristics, (2) coal particle size, (3) residence time, (4) cake com-
position, (5) cake/toluene ratio, (6) mixer horsepower requirements, and
(7) heat  transfer requirements.   Samples of the overhead will be collected
and analyzed for toluene  and water content and organic impurity build-up
due to recycling.  The bottom product,  a coal toluene slurry, will be
sampled with the coal being separated and  analyzed for moisture content,
elemental sulfur content  and sulfates.  This data  will indicate the
efficiency of the organic wetting.
                                    63

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 The  operation  of the solvent centrifuges (S-5,6) will be evaluated from
 the  standpoint of washing and filtering efficiency.  Variables to be
 evaluated  include  (1)  input slurry composition and temperature,  (2) coal
 characteristics and particle size, (3) centrifuge rotational speed, and
 (4)  wash  solvent feed  rate.  The feed slurry and wash solvent will be ana-
 lized for  composition, elemental sulfur and sulfate content.  The centrate
 and  product  coal cake will be analyzed for coal to toluene ratio, elemental
 sulfur and sulfate content.  This data will indicate the wash and filtra-
 tion efficiences of centrifuges in this application.

 The  solvent  contactor  (T-16) will be evaluated with respect to its ability
 to promote dilution of the organic soluble elemental sulfur within the
 coal  matrix.   Operational variables to be tested include (1) input cake
 and  diluent  composition,  (2) temperature, (3) coal characteristics and
 particle size, (4) residence time, and (5) mixer horsepower requirement.
 Samples will be obtained  from input and output streams with the  coal
 being separated from the  slurry and analyzed for elemental sulfur content
 to determine the degree of dilution obtained during this operation.

 The  solvent stripper (SP-4) is essentially a tray drier with solvent
 recovery capability.  The drying medium is primarily nitrogen but may also
 be steam.  The operability of this processing unit will be determined as a
 function of  (1) input  cake composition  (i.e.,  solvent content),  (2)  coal
 characteristics and particle size, (3) feed rate and temperature,  (4)
 solids residence time  (i.e., tray rotational speed), and (5) stripping
 media quantity  and temperature.  Cake input and product samples  will be
 analyzed to determine solvent and moisture content in order to evaluate
 the drying efficiency of the unit.  Inlet and outlet temperature will also
 be monitored.

The coal cooler (E-4)  is essentially a water-cooled, hollow-screw  type
cooler.  Its ability to cool the product coal to safe-handling temperatures
will  be determined.  Variables to be checked include  (1) cooling water
                                    64

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rates, (2)  screw rotation speed (i.e., residence time), (3) inlet coal
temperature, and (4) coal characteristics and particle size.  Inlet and
outlet coal temperatures will be monitored and samples of the product coal
will be analyzed for elemental sulfur and sulfate to determine overall
sulfur removal efficiency of  the process.  Also, the physical characteristics
and toluene retention of the  coal will  be determined.  The product coal will
be stored  for future use.

The solvent still (C-l) is designed to concentrate the sulfur-rich toluene
solvent from about 2.0 wt% sulfur to about 10 wt% sulfur.   The operation of
this unit will be characterized by varying feed compositions (i.e., sulfur
content), feed temperature, and heat duty.  Samples of feed and product
streams will be analyzed for sulfur as well  as other organo-sulfur com-
pounds, such as H2S, which might form during operation.   Also, any heavy
bottoms product, whtch mtght  form durtng continuous operation wtth recy-
cling, will be sampled and characterized.

The solvent cooler  (E-9) is a scraped surface heat exchanger.  This unit's
operability will be characterized by determining its ability to promote
sulfur crystallization as a function of (1) feed solvent sulfur content
and feed rate, (2)  cooling water temperature,  (3) feed rate, (4) inlet
solvent temperature and  (5) scraper rotation speed.  Samples of the inlet
solvent stream will be analyzed for dissolved sulfur content, while
effluent solvent will be analyzed for dissolved sulfur as well as crystal-
lized sulfur content.  The crystallized sulfur will then be chemically
characterized.  This data will indicate the degree and form of crystal-
lization which takes place during this  operation.

The sulfur filters  (S-7,8) are leaf-type filters.  The primary objective
of their operation  is to remove all crystallized sulfur by-product from
the recirculating solvent.  The operation of the filters will be evaluated
as a function of (1) feed solvent composition, (2) sulfur crystal content,
(3) feed rate and temperature, and (4)  filter cloth type.  Samples of the
sulfur-crystal-containing feed solvent  and the filtrate will be analyzed
for sulfur content to determine the filtration efficiency of this unit.

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The solid sulfur by-product will  be  sampled  and  analyzed  for toluene  con-
tent, other impurities  content,  and  sulfur form.   Quantities of the dry
product will be stored  for future use  in  application  studies.
                           s
The carbon adsorption drum's (SP-5)  primary  function  is to  handle  waste
organic vapors and ensure environmental integrity  of  the  plant  surroundings,
The iriput and effluent  from the  carbon drum  will be monitored for  hydro-
carbon presence so that any breakthrough  can be  detected  and a  fresh  charge
of carbon be put into operation.

5.2  Plant Operational  Schedule  and  Test  Matrix

The pilot plant test program is  scheduled over a 9-month  period.  The
first 6 months of the test program will  be devoted to the evaluation
of one type of coal while the remaining 3 months will be  utilized to
evaluate a second type  of coal.   The testing period will  be further broken
into individual test runs or test sequences  (TS).   It is  anticipated  that
20 test sequences will  be run during the  entire  test  program with  the
initial 12 being concerned with  the  evaluation of  the first coal type and
the final eight concerned with the second coal  type.   The anticipated
schedule of operation is presented in  Figure 3.  The  general philosophy
behind the schedule is  as follows:

     0  All  test sequences except TS-4 and TS-16 involve  complete
        process operation less the off-line evaporator-crystallizer
        (SP-3).
     •  TS-4 and TS-16  involve only  the evaporator-crystallizer
        (SP-3) and its  support equipment.
     t  Each TS will  require approximately 1 week  of operation.
        Following each  sequence,  there will  be 1 week to  evaluate
        data, make required repairs, adjustments and  modifications
        for  the next  TS.
     t  Test sequences  involving  only  the evaporator-crystallizer
        (SP-3) and its  support equipment  will be run  on "off weeks".
                                    66

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5123456789
WEEKS
 10       11
                                                                                            I        I
                                                                                                                                   I        I
12       13      14      IS      16       17      IS      19
                                                                                                                                                          I
                                                                                                                                                          20
  TS*-1
                  TS-2
                                 TS-3    TS-4
                                                        TS-S
                                                                        TS-6


                                                                         FIRST COAL
                                                                                       TS-7
                                                                                                       TS-8
                                                                                                                              TS-9
                                                                                                                                             TS-10
I                                                                           WEEKS                                                                  I
:0     21      22      23      24      25      26       27      28      29      30      31      32      33      34      3S       36      37      38       39
          TS-11           TS-12


         	   FIRST COAL
                                                 TS-13           TS-14
   TS-1S    TS-16    TS-17


  	     SECOND COAL
                                                                                                              TS-18           TS-19
                                                                                                                                             TS-20
           •Test Sequence Number.

            Individual tests are detailed
            in Table 2'.
                                       Figure  3.   Anticipated  Mine-Month  (39  Week)  Test Schedule

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      •   An  additional  "off week" has been added to the schedule
         periodically  (6th, 15th, 20th and 25th weeks) to allow
         for schedule  slippage due to (1) unforeseen occurrences,
         such  as  equipment failure, or longer than expected time
         requirements  to complete specific operation studies,
         (2) the  running of additional sequences if operating
         experience  indicates the need, or (3) the rerunning of
         previous sequences or specific unit operations if the
         operating data collected were inconclusive.
      •   The additional "off weeks" are onlv scheduled during the
         initial  6 months of operation (the first coal  type)
         since it is anticipated that most of the "surprises" will
         occur during  that time.  Previous operating experience
         should help in anticipating the prevention of such
         occurrences during the last  3 months of operation.

 Based on previous pilot plant operating experience, the above outlined
 philosophy  should result in a realistic rather than optimistic test
 schedule.
 During the  course of  operation, virtually every piece  of equipment in the
 processing  scheme, including several  alternates, will  be thoroughly char-
 acterized with respect to Meyers Process applicability.   Table 3 presents
 a summary of  the equipment to be tested and the operational variables to
 be evaluated.  As mentioned previously (Section 5), the variables are
 categorized as primary (independent)  and secondary (dependent).  A third
 type  of  operation indicated on Table 3 is that of supportive process
 monitoring  to ensure  acceptable plant operation.  It is intended that
 throughout  any test sequence, all  variables (both primary and secondary)
 will  be  monitored and that specific primary (independent) variables will
 be varied and the resultant changes in overall  operation (including all
 dependent variables) evaluated.   Also, supportive process monitoring
 activities will be carried out during every test sequence.

A test program has been prepared and is presented in Table 4 in the form
of 20 test sequences.   The test sequences are, for the most part (all  but
TS-4 and TS-16),  built around the  testing of the reactor section of the
process   (specifically the primary  reactor).  This was done since the
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                               TABLE 3.   TEST VARIABLES TO BE EVALUATED DURING OPERATION
VO
OPERATIONAL VARIABLE
COAL FEED SECTION
Pulverizer System (A-4)
• Monitor Coal Particle Size
• Monitor Gas Effluent
REACTOR SECTION
Slurry Mix Tank (T-2)
• Coal Particle Size Effects
• Slurry Residence Tine Effects
• Slurry Temperature Effects
• Mixer Power Requirements
Primary Reactor (R-l)
• Coal Particle Size Effects
• Residence Time Effects
• Reaction Temperature Effects
• Oxygen Pressure Recycle
Rate S Injection Effects
• Slurry Concentration Effects
• Leach Solution Salt
Concentration Effects
Secondary Reactor (R-2)
• Coal Particle Size Effects
• Slurry Residence Time
Effects
• Slurry Concentration
Effects
• Leach Solution Salt
Concentration Effects
• Scaled -up Primary Reactor
Operations
Knock-Out Drum CV-1)
• Monitor for Foam and
Particulate
Cooling Water Drum '(T-3,T-5)
• Monitor for Acid and
Particulate
SULFATE REMOVAL SECTION
Thickener (R-3)
• Residence Time Effects
• Slurry Temperature Effects
• Coal Particle Size Effects"
• Slurry Concentration Effects
Hydroclone (SP-2)
• Coal Particle Size Effects
• Slurry Temperature Effects
• Slurry Concentration Effects
• Slurry Flow Rate Effects
Evaporator-Crystallizer (SP-3)
• Feed Solution Composition
Effect
• Feed Rate Effects
• Concentrate Recirculation
Rate Effects
• Operating Pressure Effects
Type*


SPM
SPM


SV
PV
PV
PV

SV
PV
PV
PV

PV
PV

SV
SV

SV
SV

PV

SPM


SPM

PV
PV
SV
SV
SV
PV
SV
PV
SV

PV
PV

PV
OPERATIONAL VARIABLE

Barometric Condensers (E- 1,2,3)
• Monitor Aqueous Effluent
for Acid, Sulfate and
Particulate
Vacuum Pump (K-2,K-3,K-4)
• Monitor Effluent from
Belt Filter Vacuum Pump
for Acid, Sulfate and
Particulate
Filters (5-2,8-3,5-4)
• Coal Particle Size Effects
• Drum Speed Effects
• Slurry Concentration Effects
• Slurry Temperature Effects
• Nash Water Feed Rate Effects
• Filter Cloth Type Effects
• Suction Pressure Effects
Wash Water Contactors (T-ll.T-13)
• Feed Cake/Diluent Ratio Effects
• Coal Particle Size Effects
e Slurry Temperature Effects
• Residence Time Effects
• Mixer Horsepower Requirements
ORGANIC SOLVENT SECTION
Azeotrope Still (T-14)
• Coal Particle Size Effects
• Residence Time Effects
• Cake/Toluene Ratio Effects
• Mixer Horsepower Requirements
• Heat Transfer Rate Effects
Solvent Centrifuges (S-5,S-6)
• Coal Particle Size Effects
• Slurry Concentration Effects
• Slurry Temperature Effects
• Rotational Speed Effects
• Wash Liquor Feed Rate Effects
Solvent Contactor (T-16)
• Cake/Diluent Ratio Effects
• Slurry Temperature Effects
• Coal Particle Size Effects
• Residence Time Effects
• Mixer Power Requirements
Solvent Stripper (SP-4)
• Coal Particle Size Effects
• Feed Cake Solvent Content
• Feed Rate Effects
• Temperature Effects
•"Residence Time
• Stripping Media Circulation Rate
• t&trogen vs Steam Operation
Effects
Type*


SPM



SPM




SV
PV
SV
SV
PV
PV**
PV
PV
SV
SV
PV
PV


SV
PV
PV
PV
PV

SV
SV
SV
PV
PV

PV
SV
sv
PV
PV

SV
SV
SV
PV
PV
PV
PV

OPERATIONAL VARIABLE Type*

Coal Cooler (E-4)
• Residence Time Effects PV
• Coal Particle Size Effects SV
• Feed Temperature Effects SV
• CoolinK Water Rate PV

Solvent Still (C-l)
• Feed Composition Effects SU
• Heat Duty Requirements PV
• Feed Temperature m SV
Solvent Cooler (E-9)
• Feed Solvent Sulfur Content SV
Effects
• Feed Rate Effects SV
• Inlet Temperature Effects SV
• Scraper Rotation Rate Effects PV
Sulfur Pilfers (S-7,5-8)
• Feed Solvent Composition SV
Effects
• Feed Rate Effects SV
• Temperature Effects SV ,
• Filter Cloth Type Effects PV**
• Sulfur Crystal Content SV
Carbon Adsorption Drum (SP-5)
• Monitor for Hydrocarbon in SPM
Vent Stream



* PV = Primary Variables (independent variables)
SV « Secondary Variables (dependent variables)
SPM = Supportive Process Monitoring
** May be omitted if previous test results
indicate satisfactory operability for
original filter cloths.














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                                   TABLE  4.   TEST SEQUENCE  DETAIL
Test Sequence 1 - First Coal

Reactor, R-l
         Coal particle sl:o - -100 mesh
         Percent iron in leach solution - 2%
         Slurry concentration - 20"t coal
         Reaction temperature - 220°F
         Feed rate - 250 Ib/hr coal equivalent
         Oxygenatirn mode - pimp around

   Primary Variable                          (
         •  Oxygen pressure - 30 psig 60 psiS, 100 psig

Slurry Mix Tank - T-2

   Primary Variables
         •  Slurry temperature effects
         •  Mixer power effects
         •  Slurry residence time effects
Filters, S-2, S-3. S-4

   Primary Variables
         •  Drum speed effects
         •• Suction pressure effects
         •  Hash water feed rate effects
         •  Filter type effects
 Test Sequence 2 - First Coal
                            \.
 Reactor, R-l

         Coal particle size - -100 mesh
         Percent iron on leach solution -  2%
         Slurry concentration - 20% coal
         Feed rate - 250 Ib/hr coal equivalent
         Oxygenation mode - pump around
         Oxygen pressure - 100 psig

   Primary Variable

         •  Reaction temperature - 240°F,  265°F

 Wash Water Contactors, T-ll, T-13

   Primary Variables
         •  Feed cake/diluent ratio effect
         •  Mixer horsepower effects

 Solvent Contactor. T-16

   Primary Variables

         •  Cake/toluene ratio effects
         •  Mixer horsepower effects
         •  Residence time effects

 Sulfur Filter, S-7, S-8
   Primary Variable

         •  Feed solvent composition effects

Filters,  S-2,  S-3,  S-4

   Primary Variable

         •  Filter  type  effect
  Test Srqmmce 3 - First Coal

  Reactor, R-l
          Coal particle size - -100 mesh
          Percent Iron in leach solution - 2\
          Slurry concentration - 20% coal
          Reaction temperature - 265°F
          Oxygenation mode - pump around
          Oxygen pressure - 100 psig

     PriMry Variable
           • Feed rate - 500 Ib/hr, 1000 Ib/hr coal equivalent

  Azeotwf* Still, T-14

      PriMry Variables
           • Residence time effects
           • Mixer horsepower effects
           • Cake/toluene ratio effects
           • Heat transfer rate effects
 Solvent Centrifuges, S-S, S-6

     Pri»ry Variables
           • Rotational speed effects
           • Wash liquor feed rate effects
 Filters, S-2, S-3, S-4

     Primary Variable
           • Filter type effects

Solvent  Still (C-l)

     Primcy Variable
          • Heat Transfer rate effects

  Test Sentence 4  - First Coal

  Evaporator-Crystallizer, SP-3
           Feed -  rich  leach  solution obtained during TS-3
                  and stored  in storage tank  T-2SA or B.

      Primary Variables
           • Feed rate  - 250 Ib/hr, 1000  Ib/hr coal equivalent
           • Concentrate circulation rate
           • Operation pressure -  atmospheric, vacuum
                                                          70

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                           TABLE  4  (Continued).    TEST  SEQUENCE  DETAIL
Test Sequence 5 - First Coal

Reactor, R-l

         Coal particle size - -100 mesh
         Slurry concentration - 201 coal
         Reaction temperature - 2bS"F
         Oxygen pressure - 100 psig
         ttcygonation mode - pump around
         Feed rate - SOO Ib/hr coal equivalent

   Primary Variable

         •  Percent iron in leach solution - 3.5%, 5%

Filters, S-2, S-3, S-4

   Primary Variables

         •  Wash water feed rate affects
         •  Washing with dilute leach solution effects

Coal Cooler, E-4

   Primary Variable

         •  Coal residence tine effects
Test Sequence 6 - First Coal

Reactor, R-l
         Coal particle size - -100 mesh
         Percent iron in leach solution -  5%
         Reaction temperature - 265°F
         Oxygen pressure - 100 psig
         Oxygenation mode - pump around

   Primary Variables
         •' Slurry rate - 40* coal
         •  Feed rate - 500 Ib/hr, 1000 Ib/hr coal equivalent

Filters, S-2, S-3, S-4

   Priaary Variables
         •• Drum speed effects
         •  Suction pressure effects
         •  Wash water feed rate effects

Solvent Cooler, E-9

   Primary Variable
         •  Scraper rotation rate effects

Slurry Mix Tank, T-2

   Primary Variables
         •  Mixer horsepower effects
         •  Slurry temperature effects
Test Sequence 7 - First Coat

Reactor, R-l

        Coal particle  size -  -100 mesh
        Percent iron in leach solution - SI
        Reaction temperature  - 2
-------
               TABLE  4   (Continued).     TEST  SEQUENCE   DETAIL
  Test Sequence 9 - First Coal

  Reactor,  R-l
           Coal particle sise - -32  e«ih
           Percent iron in leach solution - S^
           Slurry concentration - 201 coal
           Oxygen pressure - 100 fsig
           Feed rate - SOU Ib/nr coal'equivalent
           Oxytcnatlon mode - pump around

     Primary Variable
           *  Reaction teaperature - 220'F, 240*F, 265*P

  Fitters S-2, S-3, S-4

     Primary Variables
           *  (hut speed effects
          • *  Suction pressure effects
           •  tfaah tater feed race effects

  Nub Hater Contactors, T-ll, T-15

     Primary Variables
           *  Feed cake/diluent ratio effects
           *  Mixer horsepower effects

  Solvent Centrifuges, S-S. S-4

     Primary Variables

           • ^Rotational speed effects
           •  IJash toluene feed race effects

  Solvent Contactor,  T-16

     Primary Variables
           *  Cake/toluene ratio effects
           *  HUer horsepower effects

  Slurry  Mix Tank.  T-2

     Prlaary Variable

          w  Mixer horsepower effects
         Coal particle  size - -10 «esh
         Percent Iron in  leach solution - St
         Slurry concentration - 201
         feed rate  - 500  Ib/hr coal equivalent
         Oxyfetution aoie * punp around
         Oxygen pressure  - 100 psig

            Variable
            Reaction temperature - 220*P, 240'P, CfiS'F
FUtexs. S-2. S-3. S-4

          • Variables
         *  DTUB  speed effects
         *  Suction pressure effects
         •^Ihksh  vater feed rate affects

        •r Omtactors. T-Il, T-13

            Variables
         •  Feed  cake/diluent ratio effects
         •  Mixer horsepower requirements

Soiree* Centrifuges,S.5, S-4

            Variables

         •  Rotational speed effects
         •  Vash  toluene feed rate effects

        Contactor. T-U
            Variables

         •  Cake/toluene ratio effects
         •  Mixer horsepower effects

Slurry MX Tank.  T-2

    Primry  Variable
         *  Hi*er horsepower effect*
 Test Sequence IQ  -  Flrit Coal

 Reactor, a-1

          Coal particle site - -52 nesh
          Percent  iron in leach solution  -  5%
          Slurry concentration - 20^
          Feed rate  - 500 Ib/hr coal equivalent
          Ogtygenation eodn - punp around
          Reaction temperature - 26S*F

    Primary Variable

          *  Oxygen presture - 30 p*l». 60  psif

 Thickener, R-l

    Priatary Variables

         *   Residence tine effects
         *   Slurry temperature effects

 Hydroclone,  SF-2

    Priamry Variables
         •  Slurry flow rate  effects
         •  Slurry temperature effects

 Azeotrope Still, T-U

    Primary Variable

         •  Mixer  horsepower effects

Solvent Stripper.  S?-4

   Prt-Bury Variables

         * Operational temperature effects
         • Stripping Bwlia circulation rate effects
         • Residence tine effects

Coal Cooler,  C-4

   PrUary Variable

         • Coal residence time effects
Tint Seqience 12  -  First Coal

tractor. R-l

         Coal particle site - -10 aesh
         Percent  iron in leach solution -  5%
         Slurry concentration - 2Q\
         Peed rate  - SOO Ib/hr coal equivalent
         feygenation node - pump around
         Reaction traeprature - 26S'F

          '  Variable
         * Oxygen pressure - 30 psif, 60 psig

Ibickcsjer.  R-2
         * Residence tiete effects
         • Slurry teaperature effects
          ,  SP-2

    Priomry  Variables

          •  Slurry flow rate effects
          *  Slurry temperature rate effects

Ateatrope  Still, T-U

    Priaory  Variable

          *  HUer horsepower effects

folvent Stripper, SP-4

    Priiury  Variables

          •  Operational temperature effects
          •  Stripping media circulation rate effects
          *  Residence ti«e effects

bail Cooler, E-4

    Pruury  Variable

          •  Coal residence tine effect*
                                                        72

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                           TABLE  4   (Continued).    TEST  SEQUENCE  DETAIL
'Tmst Sequence  13  - Second Coal

 Reactor.  R-l

          Coal  particle sUe - -too mesh
          Percent  Iron in lench solution  -  5\
          Slurry concentration - 20t
          Feed  rate - JSO Ib/hr coal equivalent
          Oxygenation aoJe - punp around
          Reaction tcnpcrature - 220*F

    Primary Variable

          • Oxygen pressure - 50 psig, 60  psig, 100 psig

 Slurry Mix Tank.  T-2

    Primary Variables

          • Slurry temperature effect]
          • Mixer power requirements
          • Slurry residence time effects
 Thickener, R.I

    Primary Variables

          • Residence tine effects
          • Slurry temperature effects

 Hydroclone. SP-2

    Primary Variables
          • Slurry flow rate effects
          a* Slurry temperature effects

 Solvent Stripper, SP-4

    Primary Variables
          • Operational temperature effects
          • Stripping media circulation  rate effects
          • Residence tine effects
                     i
 Coal Cooler, E-4

    Primary Variables
          • Coal  residence time effect
Test J-iuence IS - Second  Coal

•nets*. R-l

        Coal panicle site - -100 mesh
        Percent caan in leach solution - S%
        Slurry nanentration - 20\ coal
        Reaction eneperature - ;t»S*F
        Oxygcnazvim node  - pimp around
        Oxygen measure - 100 psig

    Mmmry VarimUo

         • PeeJ nee . SOO Ib/hr. 1000 IbAr coal equivalent

Axeotasf* Still, T-U

    Cdury VazimMe
         or Cake/ntuene ratio effects
         m Mixer tarsepower effects
         • Reii*m:« time effects
         • Heat Ksansfer  rate effects
Test
         ice 16 - Second Coal
EvapcKxor-CryioUizer, SP-3
                   leach solution obtained durin;
                   and stored in storage lank T-25A or 3
        • FMaaate - 2SO Ib/hr, 500 Ib/hr, 1000 Ib/hr
                     coal equivalent
        • Conoamlrata circulation rate
        • upeaftiion pressure - atmospheric, vacuum
 Test Sequence  14  - Second Coal

 Reactor, R-l
          Coal  particle size - -100 mesh
          Percent  iron in leach solution  - 5%
          Slurry concentration - 20%
          Feed  rate - 250 Ib/hr coal equivalent
          Oxygenation mode - punp around
          Oxygen pressure - 100 psig

    Primary Variable
          •  Temperature - 240'F, 26S'F

 Filters.  S-2,  S-J, S-4

    Primary Variables
          •  Drum speed effects
          •  Hater uash feed rate effects
          •' Suction pressure effects

 Solvent  Centrifuges, S-S, S-6

    Primary Variables
          •  Rotational speed effects
          •  Wash toluene feed rate  effects
                                                              73

-------
                       TABLE  4  (Continued),  TEST  SEQUENCE DETAIL
 Test Sequence 17 - Second Coal

 Reactor, R-l
         Coal particle size - -32 mesh
         Percent iro" in leach  solution - 5%
         Slurry concentration - -0 S coal
         Oxygen pressure - 100  psig
         Oxygenation mode - pump around
         Feed rate - 500 Ib/hr coal equivalent

    Primary Variable
         • Reaction temperature - 220°f, 240°F, 26S°F

 Filters, S-2, S-3, S-4

    Primary Variables
         •  Drum speed effects
         •  Suction pressure effects
         •  Wash water feed rate effects

 Solvent  Centrifuges, S-S, S-6

    Primary Variables
         •  Rotational speed effects
         •  Wash toluene feed rate effects
Test SeqMUce 19  - Second  Coal

Reactor. *-l
         Ceal particle  size  - -10 mesh
         flrrcent  iron in  leach  solution - St
         Slurry concentration - 20a«
         Oiygenation mode  -  pump around
         feed rate - 500  Ib/hr  coal equivalent
         feygen pressure  - 100  psig

    Primary Variable
         • Reaction temperature - 220°F, 240°F, 265°F

Solvent Centrifuges, S-5,  S-6

    Primary Variables
         • Rotational  speed effects
         • Wash  toluene feed rate effects_

Solvent Stripper, SP-4

    Primary Variables

         • Operational temperature effects
         • Residence time effects
          • Stripping media  circulation rate effects
Test Sequence 18 - Second Coal

Reactor, R-l
         Coal particle size -  -32 mesh
         Percent iron in leach  solution - 5%
         Slurry concentration  -  20%
         Oxygenation mode - pump around
         Feed rate - SOO Ib/hr  coal  equivalent
         Reaction temperature  -  265 °F

   Primary Variable

         •  Oxygen pressure - 30 psig, 60 psig

Thickener, R-3

   Primary Variables
         •  Residence time  effects
         •  Slurry temperature effects

Hydroclone, SP-2

   Primary Variables

         •  Slurry flow  rate effects
         •  Slurry temperature effects
Test Sequence  20  - Second Coal

Reactor, i-1

         Coal  particle  size - -10 mesh
         fercent  iron in leach solution - 5%
         Slurry concentration - 20%
         fcygenation mode - pump around
         feed  rate - SOO Ib/hr coal equivalent
         •eaction temperature - 265°F

    Primary Variable

         • Oxygen pressure - 30 psig, 60 psig

Thickener,  R-3

    Primary Variables

         • Residence time effects
         • Slurry temperature effects

Hydroclone, SP-2

    Primsry Variables

         • Slurry flow rate effects
         • Slurry temperature effects

Solvent Stripper, SP-4

    Primary Variables

         • Operational temperature effects
         • Stripping media circulation rate  effects
         • Residence time effects
         • Steam vs nitrogen operation affects

Coal Cooler, E-4

    Prlnwy Variable

         • Coal  residence time effects
                                                        74

-------
characterization of process chemistry and reactor design is considered of
primary importance to this project and also because of the long residence
times required in that processing section.  The test sequences are set
up to evaluate process chemistry and characterize equipment operation.
The proposed test program is likely to undergo modifications as plant
operating experience indicates the need for additional or repeated equipment
or process chemistry testing.  Also, schedule rearrangement may become
necessary if the need to test some specific operation (scheduled for later
testing) becomes apparent during early sequences.

5.2.1  Primary Reactor (R-1) and Process Chemistry Evaluations

Process chemistry and reactor operability will be evaluated throughout the
majority of the test program (all but TS-4 and TS-16) through a systematic
variation of reactor primary (independent) variables.  TS-1  through 12 are
concerned with operation utilizing the first type of coal.   TS^l  through 8
utilize 100 mesh top-size coal feed while TS-9 and 10 utilize 32 mesh top-
size coal feed.  Sequences  11 and 12 utilize 10 mesh top-size.  The data
obtained during test runs operating with similar conditions except for coal
particle size differences will be utilized to determine particle size
effects on process chemistry and mechanical operability of such reactor
associated equipment as mixers and oxygen injection systems.  During the
evaluation of particle size effects in the primary reactor, this same
variable will be studied in all other coal handling operations throughout
the process such as the secondary reactor, mix-feed tank, filter, centri-
fuges, solvent stripper, etc.

Test Sequences 1, 2, 3, 5, 6 and 7 evaluate primary reactor (R-1) operation
and process chemistry with  -100 mesh coal feed.  The primary intent during
these early operations is to characterize process chemistry when utilizing
the -100 mesh feed to optimize reactor operation.  TS-1 and 2 utilize the
mild leach solution (2% iron), fairly dilute slurry (20% coal) and maximum
reactor residence time (coal feed equivalent of 250 Ib/hr) to evaluate
                                    75

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 reaction pressure and temperature effects at these conditions and ensure
 process control under maximum temperature-pressure conditions,  TS-3,
 utilizing the mild leach solution, evaluates reactor residence time effects
 on process chemistry as well as reactor operability and control while oper-
 ating at maximum temperature-pressure conditions.  It should be noted that
 all other processing equipment will be evaluated for residence time effects
 during this test.  TS-5 will evaluate process chemistry and characterize
 reactor operation as a function of leach solution concentration when the
 percent iron in solution is increased from 2% to 3.5% and finally to 5%
 while operating at maximum temperature-pressure conditions and moderate
 residence times (500 lb/hr coal feed equivalent).  TS-6 will then evaluate
 the effects of residence time and slurry concentration on process chemistry
 and reactor operation by increasing system feed rates from 500 lb/hr to
 1000 lb/hr coal feed equivalent (design capacity of plant) while maintaining
 strong leach solution, maximum temperature-pressure conditions and then
 increasing slurry concentration from 20% to 40% coal.  If during the course
 of this test, reaction and regeneration rates appear to be sufficiently
 high  so as  to  allow for even shorter residence  times  in  the  reactor,  the
 reactor feed will  be injected into the ten-stage  reactor in  a downstream
 stage  (such  as  the third or fifth  stage)  thus decreasing residence  times
 even  further.   During the slurry  concentration  increase, primary  variables
 of all  processing  equipment handling that slurry  will  also be evaluated.
 TS-7 will be utilized to evaluate  process chemistry effects  and mechanical
 operability of alternate methods  of oxygenation.   Sequences  9 and 10 evalu-
 ate temperature  and pressure effects on process chemistry utilizing -32
 mesh  coal while  TS-11 and 12 evaluate temperature and pressure effects
 utilizing -10  mesh coal  feed while operating with moderate residence times
 (500  Ib/hr coal  feed equivalent),  moderate slurry concentration (20% coal),
 and strong  leach  solution (5% iron).

TS-13,  14,  15,  17,  18, 19 and 20 are designed to evaluate  reaction chemistry
 and reactor operability on  a second type of coal.  TS~15 will be used to
 evaluate residence time  effects on process chemistry while operating with
                                    76

-------
 strong  leach  solution (5% iron), moderate slurry concentration (20% coal),
 and maximum reaction temperatures and pressures (265°F and 100 psig).
TS-13, 14, 17, 18, 19 and 20 will evaluate the effects of operating tempera-
ture and pressure on process chemistry and operab-ility while operating with
 -100 mesh,  -32 mesh  and -10 mesh coal feed.   During these  operations,  all
 other processing equipment will  be evaluated with respect  to its  operability
 on type 2 coal feed  of various particle  sizes.

 5.2.2  Secondary Reactor (R-2) Evaluation

 During  TS-1  through  3,  5 through 7, 9 through 15, and 17 through  20, the
 secondary reactor (R-2) being utilized as a  hold tank (true  secondary
 reactor operation),  will have all operating  and process chemistry parameters
 monitored and analyzed.  During its operation as a holding tank R^2  requires
 no primary variable  (independent variable) testing since its operation is
 totally a function  of primary reactor (R-l)  operation.  However,  TS-8 will
 be devoted to utilizing the secondary reactor as a scaled-up primary reactor
 design  scalability.   During this operation,  the effects of oxygen pressure
 (utilizing pump around oxygenation technique) will be evaluated while
 operating at  design  capacity, maximum temperature, moderate  slurry  con-
 centration  and strong leach sjolution.

 5.2.3   Slurry Mix Tank  (T-<2)  Operation

 Slurry  mix tank  (T-2) primary  variables will  be  evaluated during  Sequences
 1,  6, 9,  11 and  13.   It is  intended that  the  operation of this unit be well
 established early to ensure properly mixed feeds  to the reactor (R-l).  It
will, therefore,  be  tested  during the first sequence.  TS-1  and 6 will
 determine primary variable  effects  on 20% and 40% coal slurry  operation
while TS-1, 9 and 11  will determine effects while operating  with  -100,
-32 and -10 mesh  coal feeds at moderate  (20%) coal  slurry conditions.
                                    77

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 5.2.4 Thickener  (R-3) and Hydroclone (SP-2) Operations

 Stnce thickener and/or hydroclone operations represent economically attrac-
 tive alternates or supplements to filtration (especially for the 20% coal
 slurries)  their primary variable effects will be carefully evaluated during
 TS-8, 10,  12,  13, 18 and 20.  During these sequences, the primary variables
 will be  independently evaluated during operation on -100, -32 and -10 mesh
 type 1 and type 2 coals present in a 20% coal slurry feed.

 5.2.5 Evaporator-Crystal 1izer (SP-3) Operation

 TS-4 and 16 are devoted solely to the evaluation of the evaporator-crystal-
 lizer in off-line operation.  The feed to the crystal!izer will be obtained
 from either of two waste storage tanks (T-25A or T-25B).  During TS-4, the
 feed will  be reactor effluent leach solution generated during TS-3, which
 operated with  -100 mesh type 1 coal feed in a 20% slurry 2% iron content
 leach solution at 265°F and oxygen pressure at 100 psig.  The primary
 reactor  variable evaluated during TS-3 will have been coal feed rate (i.e.,
 residence  time).  During TS-16, the feed will be reactor effluent leach
 solution generated during TS-15, which operated with -100 mesh type 2 coal
 in  a 20% slurry with 5% iron content leach solution at 265°F and oxygen
pressure at  100 psig.   Again, the primary reactor variable evaluated during
TS-15 will have been coal  feed rate (i.e., residence time).

Crystalline product (formed during independent primary variable testing)
recovery from the evaporator-crystallizer will  be evaluated utilizing both
centrifuge and filtration  techniques.   The evaporator-crystal!izer oper-
ation will be further  evaluated,  if this  need becomes apparent during
operation, by inserting additional  test sequences involving this operation
during "off weeks".
                                   78

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5.2.6   Filter  (S-2.  S-3.  S-4)  Operation

Filter  primary variables  will  be  evaluated  during TS-1, 2, 3, 5, 6, 9, 11,
14  and  17.   Primary  variable effects will be evaluated during TS-1 to ensure
acceptable  (not necessarily optimum) filter operation during following test
sequences.   During Sequences 5 and  6,  filter operation on two slurry con-
centrations  (20% and 40%  coal)  will be characterized.  A comparative evalu-
ation of the operability  of each  of the  three  filter types, while operating
in  similar  service,  will  be performed  during TS-1, 2 and 3.  This will be
accomplished by utilizing each of the  three filters as the lead unit during
the three sequences  (a different  filter  during each sequence).  The filters
will then be ordered in the most  efficient  way (as so indicated by data
obtained during TS-1, 2 and 3) for  the remainder of the test program.
 During  TS-5, 9 and 11, filter operation  with  -100,  -32  and -10 mesh  type 1
 coal will be evaluated.  During TS-5,  the effect  of iron  concentration in
 the leach solution will also be determined, as will  be  the effect of wash-
 ing with leach solution contaminated wash water.   During  TS-14 and  17,
 filter operability on -100 and -32 mesh  type  2 coal  will  be  examined.  In
 addition to the above mentioned testing, the  belt filter  will  also  be
evaluated with respect to its  ability  to countercurrently wash coal  during
filtration  during one test of  each  of  the coal types.  This test will be
performed when schedules  and operator  availability permit.  Also, during
evaluation  of  each of the two  drum  filters  in  the last filtration position
(prior  to the  azeotrope still), steam  drying of the filter cake prior to
discharge from the drum will be evaluated.

5.2.7   Wash  Water Contactor (T-11. T-13)  Operation

Wash water contactor  primary variables will be independently evaluated
during  TS-2, 9  and 11.  During  these evaluations, the effects of operating
with -100, -32  and -10 mesh coal  sizes will be determined with respect to
mixer power  requirements  and coal cake to wash water ratio requirements.
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5.2.8  Azeotrope Still  (T-14)

Azeotrope still operation will  be Independently evaluated  during  TS-3,
10, 12 and 15.  During  TS-3 and 15,  the operation  will  be  characterized as
a function of coal throughput  (500 Ib/hr and 1000  Ib/hr) utilizing  each of
the two coal types at -100 mesh particle size.   Sequences  3,  10 and 12  will
evaluate operation of -100, -32, and -10 mesh coal  at  a throughput  of
500 Ib/hr.

5.2.9  Solvent Centrifuge (S-5, S-6) Operation

Solvent centrifuge variables will be evaluated independently  during TS-3,
9, 11, 14, 17 and 19.  Centrifuge variables  will be characterized as a
function of throughput during  Sequence 3 utilizing -100 mesh  coal.   Centri-
fuge variables will also be evaluated for -100, -32 and -10 mesh  coal slurry
operation with both the type 1  and type 2 coals.  These determinations  will
be obtained during TS-3, 9 and 11 for the type 1 coal  and  TS-14,  17 and 19
for the type 2 coal.

5.2.10  Solvent Contactor (T-16) Operation

Solvent contactor primary variables  will be  evaluated  as a function of  coal
feed particle size for  the type 1 coal.  Test sequences to be utilized  are
TS-2 (-100 mesh coal),  TS-9 (-32 mesh coal)  and TS-11  C-10 mesh  coal).

5.2.11  Solvent Stripper (SP-4) and Coal Cooler (E-4)  Operation

Solvent stripper and coal cooler primary variables will be independently
tested during TS-5, 10, 12, 13, 19 and 20.  Variables  will be evaluated as
a function of coal type and particle size.  Sequences  5, 10 and  12  will
utilize -100, -32 and -10 mesh type 1 coal, while Sequences 13 and  19  will
utilize -100 and -10 mesh type 2 coal.  TS-20 will utilize steam instead
of nitrogen as the stripping media.   In the steam stripping operation  (TS-20)
the coal  feed is -10 mesh type 2 coal.

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 5.2.12  Solvent Cooler (E-9) Operation

 The solvent cooler will be independently evaluated during  TS-6  at  a  function
 of feed rate (solvent residence time).

 5.2.13  Sulfur Filter (S-7. S-8) Operation

 Sulfur filter primary variables will  be evaluated independently during
 TS-2 as a function of toluene sulfur content.

 5.2.14  Pulverizer System (A-3), Knock-Out Drum (V-l).Cooling  Hater Drum
         (T-5), Barometric Condenser (E-1.2,3).  Vacuum Pumps  (K-2,3.4),
         Solvent Still (C-1), and Carbon Absorption Drum (SP-5)  Operations
 The operations of these pieces of equipment will  not  involve any indepen-
 dent primary variable testing; however, all dependent secondary variables
 will be monitored throughout every test sequence to characterize equipment
 operation as a function of all process operating conditions  studied.

 5.3  MATERIALS TESTING

 In addition to the above described equipment operations testing, a mate-
 rials testing program will be conducted throughout the entire 9-month
 test schedule.  The test program will involve the evaluation of test
 samples of various materials of construction.   These  various test  samples
 will be subjected to the most chemically active and corrosive environment
 in  the  process;  namely,  the  elevated  temperature  (to  265°F),  highly
 oxidative  (to  100  psig  dispersed oxygen),  strongly  acidic  (pH as low as I),/
 highly  reactive  (ferric/ferrous  sulfate),  highly  erosive (as  high  as 40%
 coal  slurry) primary  reactor environment.   Test samples of pipe elbows
 and  straight piping will  be  fabricated for placement  into  the slurry-oxygen
 injection  recirculation  loops.   It  is  here that the highest  slurry flow
 velocities  are obtained  and  that maximum corrosion  and/or erosion  is to be
expected.  The elbows should be  most  susceptible  to stress corrosion.
Also, test  coupons of the  various candidate  materials will be fabricated

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and mounted on the inner walls of the reactor.   These samples will be sub-
jected to the most chemically reactive environment found in the process.
Both types of samples will have welded joints so that mechanical and heat
induced stress corrosion can be evaluated.   Dissimilar materials will also
be welded together and put into test service so that galvanic type corro-
sion can be evaluated.
                                      6,
Material samples will be periodically removed and visually inspected.
Sample inspections will take place after every  4th week of process
operation (during down-time) unless sample  failures indicate the need for
more frequent inspections.  If significant  visual damage is present on the
samples, the corroded part (either pipe or  coupon) will be replaced with
another test specimen of the same or different  material.  The spent speci-
men will then be metallurgically evaluated.   Special effort will be made
to accurately profile the test environment,  including both operation and
stagnant down time.   This effort will yield  a large data base of infor-
mation with respect to materials of construction for this specific service.
This data will find direct application to full-scale process evaluations.
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                            6.  REACTOR TEST UNIT

The complete and  highly automated  pilot plant for evaluating the Meyers
Process  (described  in  Section  3.0  of this report) includes coal grinding,
leach/regeneration  of  fine  coal slurry, washing for sulfate removal, sol-
vent extraction for elemental  sulfur removal, drying for solvent recovery,
crystallization for iron  sulfate disposal and alternate processing equip-
ment in  the coal  separation steps.  Since flexibility was required for pilot
plant testing, an unusual amount of complexity was necessarily introduced
into both the reactor  section  and  downstream operations so as to permit an
adequate variable test range in the reactor sections.  As a consequence,
well over 100 items of major equipment, and nearly 1000 instruments and con-
trols were included in the  design.  Therefore, preliminary design was also
prepared for a less complex test plant which could be used to assess key
process  variables at reduced construction and operating cost.  The result
of this  effort was  the development of a dual reactor testing system with
capability to evaluate critical processing variables.  The design and
operation of that less complex plant, The Reactor Test Unit (RTU), is the
subject  of the following  sections  of this report.  Section 6.1 presents
the process design, 6.2 presents unit start-up procedures, and 6.3 discusses
unit operation and  supplier testing considerations.

6.1  RTU PROCESS  DESIGN

The primary objective  of  the RTU process design effort was to obtain the
key reactor/regeneration  information on fine to intermediate coal sizes and
on a readily shippable coarse  coal at a scale where equipment representative
of commercial types could be utilized.  A secondary objective was to reduce
the installed cost  of  the RTU  substantially below that of the complete pilot
plant without compromising  primary objectives.  The resultant RTU design is
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 shown in the process flow diagram which appears in Appendix F.  The plot
 plans and an artist's sketch of the facility are presented in Appendix 6.

 In  the paragraphs which follow, a description of the equipment and the prin-
 cipal factors considered in the process design are presented.  A detailed
 reactor test unit equipment listing is presented in Appendix H.

 6.1.1  Fine Coal Feed System

 Coal ground to a top size of 8 mesh or less can be handled by the fine coal
 processing train (Appendix  F).  The coal is received in commercially avail-
 able tote bins of 2 ton capacity (A-l) filled to a small positive pressure
 with inert gas to minimize coal weathering.  The fine coal storage tank
 (T-l) is equipped at the top with a tote bin tipping and unloading mechanism
 available from the tote bin supplier.  The tote bins are lifted and posi-
 tioned in the unloader by a small electric motor driven crane.  The tank is
 sized for about 1-1/2 tote bin loads to allow for continuous operation,
 although a single bin (4000 Ibs) will provide 2 shifts of operation at the
 nominal 250 Ib/hr coal feed rate. .

 The storage tank is discharged (A-2) to the weigh belt (A-3).  The weigh
 belt which controls the coal feed rate, feeds the coal through the rotary
 feed valve (SP-1) into the mix tank (T-2).  Nitrogen purge and a pressure
 control relief valve provide an inert atmosphere in the storage tank and
 nitrogen purge of the rotary feeder prevents steam in the mix tank from
 entering the dry coal feed system.  A sliding door and a hopper on the mix
 tank feed pipe allows solids, such as makeup iron sulfate, to be added to
 the system.

 6.1.2  Fine Coal Wetting

A three-stage mix tank (T-2) equipped with mixers (M-l to M-3) provide  for
slurrying and wetting the dry coal.   Warm leach solution from  the  scrubber
mist eliminator (SP-2) is introduced into the first stage.  At nominal  feed

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rates (250 Ib/hr coal and 500 Ib/hr leach solution), the residence time is
15 min per stage  when the tank is three-fourths full.  The slurry cascades
from stage to stage through adjustable baffles that adjust the residence
time.  Complete mixing is provided in each stage and the baffles prevent
return of slurry to an upstream stage.  All liberated gases and the nitro-
gen purge gas are removed by a blower (B-l) after first scrubbing in SP-2
with incoming leach liquor to remove foam, and finally with plant cooling
water in the cooling water drum (T-3) to remove traces of entrained material
and visible water vapor.

6.1.3  Fine Coal Primary Reactor

The primary reactor  (R-l) is designed for a hold-up of 5 hours operating 80
to 90% full at the nominal feed rate.  Slurry at pressures up to 125 psig
is fed by a diaphragm-type slurry pump (P-l).  The  reactor design pressure
and temperature are  125 psig and 275°F with nominal operating conditions of
50 psig and 250°F.

The interior of the cylindrical reactor vessel is divided into ten compart-
ments, each with a length approximately equal to a slurry depth.  Baffles
are provided to allow for cascade flow from stage to stage and to prevent
return of slurry to an upstream stage.  Continuous regeneration of the
leach solution in each of the first five compartments or stages is carried
out by injection of oxygen into the discharge line of a slurry recirculation
pump connected to each stage (P-2 to P-6).  Each stage is provided with an
agitator (M-4 to M-13) with an impeller installed near the vapor-liquid
interface in order to reduce the possibility of any significant build-up of
solids in the vapor space.

The agitators also may be provided with a second submerged impeller suitable
for gas dispersion so as to demonstrate mechanical aeration as a means of
leach solution regeneration.  The gas dispersion agitators can be installed
in any compartment.  A manifold system equipped with static mixers is
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 installed in each of the last five stages to provide for demonstration of a
 third means of leach solution regeneration.

 Injection connections for steam and for cool recycle leach liquor are pro-
 vided for temperature control  The last five compartments can be bypassed
 and  slurry withdrawn from the fifth compartment in order to operate with
 only five stages if desired.

 Oxygen  is obtained from liquid oxygen storage, vaporized and supplied at
 regulated pressure.  The excess oxygen saturated with water vapor at the
 operating temperature is vented through knock-out drum (V-l) where it is
 scrubbed and cooled by cool return leach solution.  The warmed leach solu-
 tion containing water condensed from the vent oxygen is fed to the mix tank
 (T-2) through the scrubber  (SP-2).  The cooled, scrubbed vent oxygen is re-
 duced to ambient pressure and washed by plant cooling water in T-3 before
 being vented to the atmosphere.

 The  flash drum (T-4) is designed to provide a means to disengage the steam
 flashed after reduction in  pressure of the primary reactor effluent to at-
 mospheric pressure.  The drum is equipped with a tangential entry and a
 mesh pad mist separator on  the steam discharge line.  The steam is condensed
 and  scrubbed with cooling water in T-3 prior to venting any residual gas.

 6.1.4   Fine Coal Secondary  Reactor

 Slurry  from the flash drum  (T-4) may go directly to filtration or may be
 charged to the secondary reactor (R-2).  The reactor is sized to hold two
 hours of reactor effluent at nominal flow.  It is planned that after filling
 with slurry the reactor will be held for times up to about 24 hours while
 the  temperature is maintained near the boiling temperature by insulation
 containing electrical heaters.  Coal slurry in the secondary reactor may be
 stirred, to simulate a flow through reactor, or unstirred, to simulate  a
 thickening tank.   It is planned that an acid resistant concrete lining  will
be applied to the internal of the reactor to explore the potential

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 usefulness of  this material  for commercial  scale  process  equipment.   When
 the reaction period  is  complete the  secondary  reactor will  be discharged
 to the filter  through slurry pump  P-7.  Although  the higher pressure  rating
 of P-7 is not  required  for secondary reactor discharging, the pump selected
 is identical to the  primary  reactor  feed  pump  (P-l) and serves as its spare.
              »•
 6.1.5  Coal Filtration

 A belt filter  (S-l)  has been selected for the  separation step since it is
 applicable to  coal of all particle sizes.  The skid mounted package filtra-
 tion unit includes the belt  filter,  the filtrate receiver (V-2)  and pump
 (P-9), the wash water receiver  (V-3) and pump  (P-10), and the vacuum pump
 (K-l).  The filter is equipped with  filter cake wash sprays for hot water
 or steam and has provision for filter cloth washing and disposal  of the
 waste wash water by  pump (P-l3).  Normally the filtrate from V-2 will  be
 pumped to the  leach  solution  tank (T-6) containing solution with high
 Fe  /Fe ratio  (Y).*  The wash water  from V-3,  which contains some residual
 leach  solution, will  be pumped to the waste tank (T-7).   In  those tests
 where  the slurry has  a low Y  (such as slurry from the  secondary  reactor
 (R-2)  or  the coarse coal reactor (R-3) effluent),  filtrate from  V-2 will  be
 pumped to leach solution tank (7-5) containing  low Y solution.   Wet  filter
 cake will  be discharged  from the filter into covered dumpsters for disposal
 or be  retained  for subsequent testing or evaluation.

 6.1.6   Coarse CoalReactor

 The coarse coal reactor  (R-3) will  contain approximately 4000 Ibs  of coal
 from tote bins  (A-4)  identical to those  used in the  fine coal feed system
 and will use the same type of tipping and  discharging equipment.   The  re-
 actor will be equipped with insulation containing  electrical heaters to
maintain reactor temperature  at the desired  level.  Coarse coal leaching
will be a batch operation and will  include the  following steps:
*  As used in the process description, high Y solution contains about 5%
   iron with 90% Fe+3 and 10%  Fe+2  (Y =  .9) while low Y solutions will
   have an Fe+3/total Fe ratio of about  0.75.
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     (1)  One tote bin of coarse coal (about 2 tons) will be placed
          in the reactor.

     (2)  Steam will be purged through the coal until the desired
          coal bed temperature is reached.

     (3)  Leach solution (normally high Y solution from T-6) will
          be pumped at high rate (P-12) through heat exchanger E-l
          where it will be heated to the reaction temperature be-
          fore entering R-3.

     (4)  Reactor R-3 will be filled with solution (nominally 15
          to 30 minutes) while exhaust gases removed by blower B-2
          are scrubbed in T-3 before venting.

     (5); When the reactor is full, the leach solution feed rate
          will be reduced to the exchange flow rate (typically
          less than 1 gpm) with overflow solution returning to
          the low Y solution tank (T-5).

     (6)  Solution circulation will be continued for the desired
          time (nominally 25 to 100 hrs) with solution temperature
          controlled by exchanger E-l and reactor temperature main-
          tained by controlling the reactor heaters,

     (7)  When the planned reaction time is reached, the reactor
          will be drained of leach solution by pump P-8 and coal
          samples drawn from several levels and radial positions
          in the reactor.

     (8)  The wet reactor contents may be discharged through A-6
          to a conveyor (A-5) and washed on the filter (S-l) or
          may be conveyed directly to a dumpster.

     (9)  As an alternate to Step 8, the coal may be washed in
          place by pumping (P-15) water from T-8 through ex-
          change E-l.  The overflow wash water will be taken to
          waste tank T-7.

    (10)  The washed coal can then be drained, sampled and dis-
          charged as in Steps 7 and 8.


Leaching and washing of coarse coal is believed to be an important  aspect

of the reactor testing program.  At present there is insufficient design

data to address two anticipated design problems.  The height to  cross  sec-

tion ratio and requirements, if any, for internal flow distributors are

both unknown.  Special provisions for reactor discharging to prevent bridg-

ing also may be required.  Presently, it is thought  that a  reactor

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3' x 3' x 9' high is a likely design, but a longer reactor 2-1/2' x 2-1/2'
x 13-1/2' high is shown in  the  initial design.  The support structure
planned for the taller reactor  can  readily accommodate a shorter reactor
but the reverse situation would lead to difficulties.

6.1.7  Primary Reactor as a Regenerator

The RTU design allows for the primary reactor  (R-l) to serve as a regenera-
tor for leach solution.  Solution with low Y from tank T-5 may be pumped
(P-ll  or P-12) to the reactor at rates up to 20 gpm for separate examination
of the regeneration  rates.   Leaching of each batch of coarse< coal will pro-
duce up to  10,000 gal. of low Y solution so that up to about 10 hours of
continuous  regeneration testing can be accommodated even at near maximum
rates.  It  should be noted  that normally the low Y solution will be regener-
ated during fine coal processing rather than by separate regeneration.  The
test plan will arrange the  tests so that solution of the correct Y is avail-
able without unnecessary solution adjustments.  About two or three test
weeks  of fine coal processing per batch of coarse coal will keep the solu-
tion in balance.  Solution  tanks sized for 15,000 gal. provide an adequate
margin for  off-nominal operation conditions.

6.1.8  Sizing the Reactor Testing System

In the preceding paragraphs, the discussion indicated that the initial pro-
cess design was based on nominal throughputs of 250 Ib/hr of fine coal
(continuous operation) and  4000 Ib/batch of coarse coal.  These sizes pro-
vide for a  test program which balances fine and coarse coal testing.  Coal
of appropriate size  is obtained and handled in 2-ton tote bins which are
the largest standard size available commercially.  A single bin is a con-
venient coarse coal  reactor batch and one bin  also provides for two shifts
of operation of the  fine coal system.  The total quantity of coal to be
processed is estimated to be about  150 tons divided between cleaned coal
and run-of-the mine  coal.   This  quantity, while large, is reasonable to
transport from mine  to grinding  to  use in bin  quantities.
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The process equipment, however, has a wide range of coal throughput.  At
nominal slurry concentration and coal feed rate, the flow rate through the
fine coal system is about 1.2 gpm.  Pump capacity would allow at least a
threefold increase to 750 Ib/hr and may be capable of reaching 1000 Ib/hr.
At 20% slurry coal feed rates from 100 to 500 Ib/hr should be available.  It
is believed that the belt filter will handle any of these feed rates except
possibly the highest rates with a -100 mesh high ash uncleaned coal.  Heat-
ing, cooling and storage capacities have been selected to provide for the
high testing flexibility felt to be necessary.

6.2  RTU START-UP

The initial start-up, short-term operation and shutdown of each of the two
reactor trains will be performed and safety procedures will  be practiced.
The primary goal of these operations is to check out equipment, personnel,
standard and emergency procedures, analytical techniques and overall opera-
bility of the integrated systems.  The initial  start-ups will require elon-
gated time schedules to allow for greater process control and more in-depth
procedure and equipment evaluations than will be required during subsequent
start-ups.  A typical start-up test sequence that would be appropriate for
this type of operation is presented in Table .5.  it is anticipated that
unit start-up operations will immediately precede the RTU testing program
and require approximately 2 months to complete.

The philosophy of the start-up operation, as outlined in Table 5, is to
initially check out mechanical operation and structural integrity of both
the fine and coarse coal treating systems while operating under conditions
which vary from very mild to quite severe (i.e., initial water circulation
testing at ambient temperature and pressure to final start-up testing utiliz-
ing strongly acidic coal slurry at elevated temperatures and pressures).
It is also intended that during the course of start-up operations, all pro-
cess  monitoring, data gathering, physical sampling and chemical analysis
techniques will  be evaluated with acceptable techniques being demonstrated
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                                            TABLE  5.    GENERALIZED  START-UP SEQUENCE
              System

1     Fine Coal Reactor System



2     Fine Coal Reactor System


3     Coarse Coal Reactor System



4     Fine Coal Reactor System



5     Fine Coal Reactor System





6     Fine Coal Reactor System




7     Coarse Coal Reactor System
                   Operations

Process water circulation at ambient temperature
to maximum expected operating  temperatures.  No
coal. Iron sulfate or oxygen present.

Flow oxygen at ambient to 100  psig through pump
around and static mixer Injection systems.

Process water circulation at ambient to normal
boiling point temperatures.  No coal or Iron
sulfate present.   Drain reactor.

Drain process water from entire system and refill
with purchased distilled water.
Charge fine coal  (-100 mesh) to the storage hopper,
feed reactor and  operate system at 20-30% slurry
with oxygen injection. at 50 psig and 250°F reactor
temperaturet  (Ne iron sulfate added, distilled
      only.)
Charge coarser fine coal  (-8 to -12 mesh) feed
reactor and operate system at 20-30* slurry with
oxygen injection and 250°F reactor temperature.
(No iron sulfate added, distilled water only.)

Charge Coarse Coal  (-3/8  inch) Reactor System and
operate utilizing hot (212°F) distilled water cir-
culation operation, back  wash coal charge in situ
and discharge coal  utilizing filtration and wash
systems.
                            Objectives

Check integrated operability of pressure,, temperature, flow, an
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                                                      TABLE 5  (Continued).   GENERALIZED  START-UP  SEQUENCE
                                                                    Operations
                                                                                                           Objectives
to
ro
8     Fine Coal  Reactor System
                    Coarse Coal Reactor System
               10    Coarse Coal Reactor System
               11    Fine Coal Reactor System
Make up leach solution to approximately 2-3* total
Fe by feeding Iron sulfate crystals Into the mix
tank (T-2) utilizing  the pulverized coal feed
mechanism while circulating hot distilled water
(no coal feed)

Circulate hot leach solution (2-3X Fe)  through sys-
twn.

Perform first total test run.  Charge -3/8 Inch coal
and circulate hot (210°F) leach solution (2-3% Fe)
for two to four days.  Upon run completion,  grab
sample the reacted coal, back wash the coal  in situ,
grab sample the washed coal and discharge utilizing
the filter.

Perform first total test run.  Charge with -100 mesh
coal, operate with 2-3% Fe leach solution, 20-30%
(wt.) coal slurry, oxygen injection pressure of 50
psig and a reactor temperature of 230°F.  During
operation (over an approximate 16 hour period) sam-
ple all appropriate processing streams including
washing and filtration operations.
Check operabllity of system (especially all rotary equipment,
seal flush  systems, etc.) and insure system Integrity during
operation with hot strongly add  leach solution.
                                                                                        Check operabllity and Integrity of the system while operating
                                                                                        under hot strongly acid conditions.

                                                                                        Demonstrate total Coarse Coal Reactor System operabllity,
                                                                                        demonstrate adequacy of sampling and analysis techniques and
                                                                                        generate a complete set of process evaluation data.
                                                                                        Demonstrate total Fine Coal  Reactor System operabllity,  demon-
                                                                                        strate adequacy of sampling  and  analysis techniques and  generate
                                                                                        a complete set of process evaluation data.

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during final  start-up  runs.   Additionally,  it  is  during  start-up  testing
that reference  data  using pure  water feed simulating  the iron sulfate leach
solution will be  generated.

6.3  REACTOR  TEST UNIT OPERATION  AND EQUIPMENT SUPPLIER  TESTING

Following  start-up operations,  the  reactor  systems  (both coarse and fine
coal) will  be put into operation  to characterize  process chemistry and
equipment  operability  on  two  classes of  one type  of coal  (cleaned and un-
cleaned).   The  purpose of the test  program  will be to operate the reactor
system to characterize mixing operations, reaction, and  regeneration
operations  and  to evaluate initial  filtration  parameters.  Another objec-
tive of the test  program  will be  that of generating sufficient quantities
of reacted  coal product to be sent  to equipment manufacturer testing
facilities  for  pilot scale testing  of downstream  process equipment (filtra-
tion, centrifugation,  solvent stripping,  steam stripping, drying, crystalli-
zation, etc.).

6.3.1  Task 3-A,  Reactor  System Test Operation

The following paragraphs  will describe the  anticipated approach to meeting
the above mentioned  objectives  for  each  major  section of the reactor test
facility and  present a possible generalized test  plan for utilization during
process evaluation.  It is anticipated that the reactor  testing program will
require approximately  7 months  to complete.

6.3.1.1  Fine Coal Reaction System  - The fine  coal reaction system is com-
prised of all equipment with  the  exception  of  six items  specific to coarse
coal processing,  namely the coarse  coal  blower (B-2), the coarse coal
reactor-washer  (R-3),  the portable  conveyor belt  (A-5),  the coarse coal
heat exchanger  (E-l),  the wash  water storage tank (T-8), and the water
transfer pump (P-15).   For purposes  of discussion, the fine coal reactor
system (all other equipment)  will be further subdivided  into the following
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functional sections: 'the feed/mixing section, the reaction section, and
the filtration section.

                        Feed/Mixing Section

The primary functions of this section are to deliver pre-ground coal to the
fine coal storage tank, sufficiently mix the pulverized coal and leach
solution  to ensure wetting and defoaming, and to deliver the slurried coal
to the reactor.  The equipment which constitutes the feed/mixing section is
listed below:

                       Feed Bin (A-l)
                       Bin Discharger (A-2)
                       Weigh Belt (A-3)
                       Rotary Feeder (SP-1)
                       Storage Tank (T-l)
                       Feed Mix Tank (T-2)
                       Feed Tank Mixers (M-l, 2, 3)
                       Scrubber Blower (B-l)
                       Scrubber (SP-2)
                       Cooling Water Drum (T-3)
                       Feed Pump (P-l)

Anticipating that mechanical operability of all equipment will have been
previously demonstrated during plant start-up, the only equipment in  this
section requiring operational characterization is the slurry feed-mix tank
(T-2) and the scrubber-mist eliminator (SP-2).  The parameters to be  evalu-
ated during slurry feed-mix tank operation are (1) coal characteristics,  (2)
(2) coal particle size, (3) slurry residence time (15 minutes to 1  hour)
which will be varied through the use of liquid level control,  (4) slurry
temperature (1SO°F-215°F) which will be varied by steam injection;  (5)  iron
sulfate concentration, and (6) slurry concentration.

Sampling requirements for characterization of this operation  include  (1)
pulverized coal feed sampling to determine particle size distribution,  (2)

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coal slurry sampling  from the  feed-mix  tank effluent which will be  analyzed
for pyrite conversion and examined to determine  degree  of wetting and gener-
al slurry composition,  and (3)  gas sampling from gas effluent  lines running
from the feed mix  tank  to the  scrubber-mist eliminator  (SP-2)  which will be
analyzed for carbon dioxide content (carbon dioxide must be evolved prior
to entrance into  the  reactor section in order to minimize full scale oxygen
bleed  requirements) and foam content.   In addition, the effluent  from the
scrubber-mist  eliminator (SP-2) will be monitored for the presence  of foam
and acid mists  and both the gaseous effluent  and aqueous effluent from the
cooling water  drum (T-3) will  be sampled and  analyzed for particulate and
sulfate presence.

                             Reaction Section

In this section of the system  the bulk  of the pyrite contained within the
coal is converted  to  elemental  sulfur and soluble iron  sulfate and regener-
ation  of the spent leach solution takes place.   This section of the process
consists of the following group of equipment:

                  Primary Reactor (R-l)
                 Reactor Mixers (M-4 through  13)
                 Knock-Out Drum (V-l)
                  Flash  Drum (T-4)
                 Secondary Reactor (R-2)
                 Secondary Reactor Mixer (M-14)
                 Reactor Circulation Pumps (P-2  through 6)
                 Secondary Reactor Discharge  Pump (P-7)
                 Leach  Solution Surge Tanks (T-5, 6)
                 Leach  Solution Circulation Pump (P-ll)
                 Leach  Solution Feed Pump (P-12)

The equipment in this section  requiring operational characterization are
the primary and secondary reactors (R-l,  2).   The primary reactor (R-l)
will  be characterized in a steady state operating mode while serving as a
                                     95

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simultaneous reactor-regenerator.  The secondary reactor (R-2) will be
characterized while operating in a stirred batch mode, essentially simulat-
ing a holding tank, and also unstirred, simulating a thickener.  During
this operation, no regeneration will take place.

Operational variables to be evaluated during reactor operation include
(1) coal characteristics, (2) coal particle size, (3) slurry residence time
(1 to 10 hours), controlled through slurry feed pump (P-l) pumping rate and
number of  reactor stages utilized, (4) reaction temperature (205°F to
265°F), controlled by varying inlet slurry temperature and steam injection,
(5) oxygen partial pressure and flow rates, varied through changes in oxygen
supply pressure and inlet flow rate adjustment, (6) mode of three phase
(oxygen-coal-leach solution) mixing, which will be evaluated utilizing oxy-
gen injection in slurry pump-around loops, static mixing, and oxygen injec-
ted through simple agitation, (7) slurry concentration (coal/leach solution
ratio), and (8) salt concentration.

Sampling requirements in this section of the process will include slurry
samples drawn from each stage of the primary reactor and samples drawn from
the secondary reactor effluent.  The solid/liquid ratio will be determined
and the coal will be separated and analyzed for pyrite and elemental sulfur
to determine degree of pyrite conversion to sulfur and sulfate.  The leach
solution will also be analyzed for ferric and ferrous ion to determine de-
gree of regeneration.  The reactor (R-l) liquid effluent (slurry) will also
be analyzed for trace materials to evaluate the problem of impurities build-
up in the  leach solution due to recycling.  Oxygen consumption will be de-
termined by mass balancing around the reactor system.  The gaseous effluent
from the primary reactor (R-l) will be sampled prior to the knock-out drum
(V-l) and analyzed for particulate, acid mist concentration and the presence
of foam.  The cooling water drum (T-3) effluent will be sampled and analyzed
for particulate and acid content.
                                    96

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                            filtration  Section

In this section  of  the process  the  slurry  leaving  the  reactors  is separated,
leach solution collected,  and the soluble  sulfate  washed  from the coal ma-
trix and  removed from the  system as by-product.  This  section consists of
the following equipment:

                         Filter (S-l)
                         Filtrate Receiver  (V-2)
                         Wash  Water  Receiver  (V-3)
                         Waste Disposal  Tank  (T-7)
                         Waste Disposal  Pump  (P-14)
                         Filter Waste  Pump  (P-13)
                         Filtrate Pump (P-9)
                         Wash  Water  Pump (P-10)
                         Vacuum  Pump (K-l)

The only  equipment  in this  section  requiring thorough  characterization is
the filter  (S-l).   The remainder of the equipment will not require charac-
terization  since its  mechanical  operability will have  been previously demon-
strated during start-up.

Filtration  and wash efficiencies of the belt type  unit will be  determined
as a function of (1)  input slurry concentration and temperature, (2) coal
characteristics  and particle  size,  (3)  belt  speed  (i.e.,  cake thickness),
(4) wash  water feed rate,  and (5) suction  pressure.

In general, all  filter influents and  effluents will require sampling and
analysis  for complete characterization.  The slurry feed, filtrate, spent
wash solution and filter cake will  be analyzed for iron sulfate to evaluate
wash and  filtration efficiencies and  determine the fate of the  soluble salts.
Additionally, the moisture  content  of the  cake will be determined.   Also,
the effluent from the vacuum  pump (K-l)  will be sampled and analyzed per-
iodically for particulate sulfate presence for evaluation of possible ad-
verse environmental impact.

                                    97

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6.3.1.2  Coarse Coal Reactor System - The coarse coal  reactor system is com-
prised of three functional  sections, the Coarse Coal  Reactor-Washer Section,
the Leach Solution Regeneration Section, and the Filtration Section.

                    Coarse Coal Reactor-Washer Section

The primary functions of this section are to demonstrate pyritic sulfur
conversion to elemental sulfur and soluble sulfate in large particle size
(as large as -3/8 inch) coal and to evaluate in situ washing of the reacted
coal  to  remove the  soluble sulfate.  The equipment comprising this section
is listed below:

                  Coarse Coal Reactor-Washer (R-3)
                  Coarse Coal Feed Bin  (A-4)
                  Coarse Coal Bin Discharger (A-6)
                  Coarse Coal Blower (B-2)
                  Cooling Water Drum (T-3)
                  Heat Exchanger (E-l)
                  Leach Solution Surge Tanks (T-5, 6)
                  Leach Solution Circulation Pump (P-ll)
                  Leach Solution Feed Pump  (P-12)
                  Water Storage Tank (T-8)
                  Water Transfer Pump (P-15)
                  Wash Water Return Pump (P-8)
                  Portable Conveyor Belt (A-5)

Of the equipment in this section, only the coarse coal reactor-washer  (R-3)
requires thorough characterization.  Operational variables will be  examined
while the reactor is operating as a fixed-bed reactor and also when  it is
operating as a fixed-bed coal washer.  Operational variables to be  evaluated
include  (1) coal characteristics,  (2) coal  particle size,  (3) coal  resi-
dence time (1 to 4 days), (4) reaction temperature (to 215°F),  (5)  inlet
and outlet leach solution iron (Fe+2 and Fe+3) concentrations,  (6)  leach so-
lution circulation rate, (7) leach solution salt concentration,  (8)  wash
water circulation rates, and (9) wash water temperature.

                                     98

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Sampling requirements  in  this  section will  include  coal  samples withdrawn
periodically  (radially and  at  selected  heights  of the  reactor) which will
be analyzed for  pyrite, sulfate  and  elemental sulfur to  determine degree of
pyrite conversion  (during reaction)  and washing efficiency  (during washing
cycle).  The  inlet and outlet  leach  solution will be analyzed for ferric
and ferrous  ions to determine  reaction  rates.   Wash water exiting the  fixed-
bed unit will  also be  sampled  and  analyzed  for  iron and  sulfate contents so
as to determine  soluble sulfate  extraction  rates from  coarse coal.  Addi-
tionally,  the gaseous  effluent from  the cooling water  drum  (T-3) will be
periodically  sampled and  analyzed  for particulate and  acid mist content.

                    Leach  Solution  Regeneration  Section

The Leach  Solution Regeneration  Section will be utilized to characterize
leach solution regeneration operations  and  to supply regenerated leach so-
lution to  the process  surge tanks  (T-5  and  T-6)  as  required.  The equipment
which constitutes  this section is  as follows:

                 Primary Reactor-Regenerator (R-l)
                 Reaction  Recirculation  Pumps (P-2 through 6)
                 Reactor Mixers (M-4  through 13)
                 Flash  Drum  (T-4)
                 Knock-Out Drum (V-l)
                 Cooling Water  Drum (T-3)

Variables  to  be  evaluated during regeneration studies will include (1)
leach solution residence  time  in R-l, (2) regeneration temperature, (3) oxy-
gen feed rate,  (4)  oxygen pressure,  and (5) mode of oxygen injection.  Feed
and effluent  leach  solution samples  will be obtained from the regenerator
as well as samples  from each regenerator stage.  They will be analyzed for
iron (Fe+2 and Fe+3) content so  as to determine degree of regeneration.

                             Filtration  Section

The Coarse Coal  Filtration  Section will be  utilized to study filtration and
filter washing characteristics of  reacted coarse coal.   Descriptions of the
                                     99

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equipment which comprise thts section, as well as the test variables and
sampling requirements associated with its operation, are identical to those
presented previously in the Fine Coal Reactor System discussion (Section
6.3.1.1).

6.3.2   Equipment Supplier Testing

During  the  final  4 months  of  reactor system  operation,  large  quantities
 (up  to  several tons) of reactor processed coal (both fine and coarse) and
leach solution will be sent to major equipment manufacturers for evaluation
in specific types  of pilot scale equipment.  Operations such as filtration,
centrifugation, steam or nitrogen sulfur stripping, organic solvent removal
of elemental sulfur, crystallization, and drying will be evaluated.  Table 6
presents a  summary of information gathered during preliminary discussions
with typical equipment manufacturers.   Information outlining test facility
locations,  feed stock requirements, and anticipated test duration is pre-
sented.  The following paragraphs describe test objectives and sampling re-
quirements  associated with each type of test operation.

6.3.2.1  Filtration - Filtration tests will be performed to characterize
the  operability of different types of equipment (belt, drum, drum-belt)
with respect to filtration and washing capability.  The parameters to be
studied and sampling requirements for each evaluation are identical to those
presented earlier  (Section 6.3.1.1) during discussion of filtration testing
associated  with fine coal reactor system operation.

6.3.2.2  Centrifugation - Centrifuge operation will be evaluated from the
standpoint  of washing and separation efficiency.  Variables which might be
evaluated include  (1) input slurry composition and temperature,  (2)  coal
characteristics and particle size, (3) centrifuge rotational speed, and  (4)
wash liquor feed rate and temperature.  The feed slurry and wash solvent
will  be analyzed for composition, elemental sulfur and sulfate content.
The centrate and product coal cake will be analyzed for coal to  liquid ra-
tio as well  as sulfur content.  These  data will  indicate  the  wash and fil-
tration  efficiencies of centrifuges in this application.

                                    TOO

-------
TABLE 6.  SUMMARY OF MANUFACTURER TESTING CAPABILITIES
Operation
Filtration
Centrifugation
Steam and Solvent
Stripping
Crystallization
Drying
a Per coal sample.
b Requires coal product
c Must be received premi
Manufacturer
Ametec
Denver
Bird Machine Co.
Dorr Oliver
Ametec
Bird Machine Co.
Dorr Oliver
Denver Equipment
Denver Equipment
Eimco
Ametec
Wyssmont

and leach solution
xed in drums.
Location of
Test Facility
East Moline, 111.
Colorado Springs, Colo.
Walpole,.1%ss,
Oakland, Calif.
East Moline, 111 ,
Walpole, Mass,
Oakland, Calif.
Colorado Springs, Colo.
Colorado Springs, Colo.
Salt Lake City', Utah
East Moline, 111.
Fort Lee, N.J.

to be mixed to slurry speci

Test
Duration9
3^5 Days
5 Days
2-3 Days
5 Days
3-5 Days
5 Days
5-10 Days
Not known
Not known
Not known
4-5 Days

fi cation at

Quantity Required
For Testing3
5 to 50 gal. slurryb
2000 to 2500 Tb slurryb
500 to 1000 gal. slurry0
30 to 40 gal. slurryb
5 gal . minimum
500 to 1000 gal. .slurry
1000 gal. slurry"
Not known
Not known
Not known
Not known
4000 to 6000 Ib wet coal
cake

the test facility.


-------
6.3.2.3  Solvent Extraction and Vapor Stripping - Several techniques for
the  removal of elemental sulfur (a co-product of the leach reaction) from
previously water washed (to remove soluble sulfate) coal may be evaluated.
An effective technique used in bench-scale studies involves extraction of
washed coal with an organic solvent followed by drying to remove residual
solvent.  Alternate approaches which have been briefly investigated in the
laboratory will be examined and those found to be potentially attractive
may  be included in the supplier testing.

Variables which might be evaluated include (1) coal characteristics and
particle size, (2) stripping temperatures and pressures, (3) feed solvent
sulfur content, (4) coal residence time, (5)  coal to stripping media ratio,
and  (6) type of solvent (toluene, xylene, kerosene, etc.).  Evaluation of
this operation will require that samples of feed and product coal as well
as influent and effluent stripping media be analyzed for sulfur content so
as to determine overall operation efficiency.  Additionally, solvent and/or
moisture retention of the product coal will be determined.

6.3.2.4  Crystallization - The crystallizer operations will be evaluated
with respect to output product (crystalline iron sulfate salts) character-
istics as a function of operational parameters.  Variables which might be
studied include (1) input leach solution composition, (2) feed rate, (3)
operating pressure (sub-atmospheric to one atmosphere); (4) concentrate
circulation rates, and (5) heater temperature (i.e., concentrate tempera-
ture).  Evaluation of this operation will require that concentrate samples
be taken and that the crystalline product be analyzed and chemically char-
acterized.   Quantities of this by-product will be retained for future study.

6.3.2.5  Drying - Drying operations will be evaluated to determine the
efficiency of solvent recovery from coal which has previously undergone
organic solvent stripping of elemental sulfur.  It is anticipated that
inert gas (N2) and steam circulation techniques will be studied.  The char-
acterization of this operation will be determined as a  function  of  (1)  input
cake  composition  (i.e., solvent content),  (2) coal characteristics  and
                                   102

-------
particle size, (3) feed rate, (4) temperature (5) solids residence time,
and (6) steam quantity and quality.  Cake input and product samples will
be analyzed to determine solvent and moisture content in order to evaluate
the drying efficiency of the unit.  Inlet and outlet temperatures will  also
be monitored.
                                      103

-------
                             7.  REFERENCES
1.  Hamersma, J. W., E. P. Koutsoukos, M. L. Kraft, R.  A. Meyers, G.  J.
    Ogle, and L. J. Van Nice, "Chemical Desulfurization of Coal:   Report
    of Bench-Scale Developments", EHSD 71-7, prepared for the Office  of
    Research and Monitoring of the Environmental Protection Agency,
    Research Triangle Park, N. C., February 1973.

2.  Koutsoukos, E. P., M. L. Kraft, R. A. Orsini, R. A. Meyers, M. J.
    Santy, and L. J. Van Nice, "Meyers Process Development for Chemical
    Desulfurization of Coal", Contract No. 68-02-1336,  prepared for the
    Office of Research and Monitoring of the Environmental Protection
    Agency, Research Triangle Park, N. C., May 1976.
                                    105

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APPENDIX    A
PROCESS FLOW DIAGRAM
         107

-------
                           A-1
                       COAL FEEDER BELT
                      MATL: CARBON STEEL
       A-8
   COAL HOPPER
 WITH LIVE BOTTOM
MATL: CARBON STEEL
        A-3
COAL PULVERIZER SYSTEM
  MATL: CARBON STEEL
          A-2
      APRON
COAL STORAGE
A-e
k A
                                                                                   •AA

                                                                                   ! BB
                                    A-l
                                                 HOPPER
                                                                     A-3
                                                    NITROGEN
                                     108

-------
      A-4
 BIN DISCHARGER
A-5
                    T-l
                   WEIGH BELT FEEDER    COAL STORAGE TANK
                  MAIL: CARBON STEEL
                                     ROTARY FEEDER
      T-3
SCRUBBER COOLING
    WATER DRUM
    SIZE:  3' X 3'
    MATL: FRP

         B-2
    SCRUBBER BLOWER
  MATL: CARBON STEEL
  125 ACFM 1/8 HP
            B-1
      COAL DUST BLOWER
     MATL: CARBON STEEL
                                    T-2
                            SLURRY FEED SURGE TANK
                                SIZE: 3' X91
                                MATL: 316 S.S.

        	                 M-1A. M-1B&M-JC
SCRUBBER & MIST ELIMINATOR   SLURRY SURGE TANK MIXERj
       SIZE:2'X4'                MATL: 316 S.S.
      MATL: 316 S.S.
                                                                  TO ATMOS
          SP-1
                                                               COOLING
                                                               WATER TO
                                                            2  TRW POND
                                               SLURRY FEED PUMP
                                                MATL: 316 S.S.
                                     109

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   COOLING WATER DRUM
       SIZE: 3' X 5'
       UATI  COD
       MATL: FRP
                                      fi7f .  t> y «i
                                      Jlitt  4 A JJ
                                     MAIL:  3165.5.
        V-l
 COMPRESSOR SUCTION
  KNOCK-OUT DRUM
SIZE: 1' X5-61 (APPROX)
MATL: 316 S.S.
                                                                    OXYGEN RECYCLE
                                                                       COMPRESSOR
                                                                      MATL:  3 16 S.S.
                                                                       14.65 ACFM
SECONDARY REACTOR
 SIZE:  10'6" X 29'
    MATL:  316 S.S.
LEACH LIQUOR FLASH DRUM
     SIZE: 2'  X 4'
     MATL: 316 S.S.
                                                                                                   SECONDAI
FF
         TYPICAL FOR PUMPS P-2A,
         P2B, P-2C, P-2D, & P-2E
                                                                                                        SLURRY MIXERS
                                                                                                        MATL: 316 S.S.
                                                                                                                  IQR
                                                                                                                  iRS
                                                                                                                    — KK
                                                TYPICAL FOR PUMPS P-2F,
                                                P-2G, P-2H,  P-21 & P-2J
                                                    REACTOR RECIRCULATION PUMPS
                                         PUMPS P-2A THRU P-2H 316 S.S. & ALLEY 20
                                         PUMPS P-21, P-2J BAR CHEM II (EPOXY) WITH SHIELD
                                                        no

-------
          M-3 AND M-4
         LEACH SOLUTION
        MAKE-UP TANK MIXERS
           MAIL: 316 S.S
             T-26 & T-27
      HYDROCLONE SURGE TANKS
           SIZE: 3' X 41
           MATL: 316 S.S.
                        THICKENER
               SIZE: 8' X51  STRAIGHT SIDE
               MATL: WALL-C5 W/ GUNITE LINING
                     RAKES- C5 W/VITON COVERING

                          T-6 & T-7
                 LEACH SOLUTION MAKE-UP TANKS
                         SIZE: 4'X6'
                        MATL: FRP
                                        SP-2
                                 SLURRY HYDROCLONE
                                      5.5 GPM
                                   MATL: 316 S.S
                                         OR CERAMIC

                                      M-10 & M-11
                               SLURRY HYDROCLONE MIXERS
                                     MATL:  316 S.S.
GG
HH
1
I




SP-2V
M-ion I M-II n
^T~TTj — IT II

1 i**.ir
T-26 T-27 ••=)
*";





 JJ-
 KK-i
                                                        BY GRAVITY
                   N.C.
       ,P-3
    _E=2_
   REACTOR
  DISCHARGE
    PUMP
 MATL:316S.S.
         P-26
    p-26
   SLURRY
HYDROCLONE
   PUMP
MATL: 316 S.S.
                                                        MAKE-UP
                                                       MATERIALS
                                                                           M-4
                                                                 LT-4J

                                           P-4
  THICKENER
  DISCHARGE
    PUMP
MATLs 316 S.S.
                                                                            LL
                                                                            GG
                                                                            HH

                                                                            MM
                                                                            NN
                                                                            00
    _E=5_
MAKE-UP TANK
TRANSFER PUMP
 MATL: 316 S.S.
                                            Ill

-------
         T-9 AND T-1
-------
                                  S-2
                            F-l
                               -
                                                                            K-2
       SIZE: 3' X 3'6"
       MATL: 316 S.S.
LEACH LIQUOR FILTER   BAROMETRIC CONDENSER   LEACH LIQUOR FILTER
 SIZE: 3' X 5' DRUM     MATL: CARBON STEEL      VACUUM PUMP
 MATL: 316 S.S.                                  SCFM AIR
                                            MATL: CARBON STEEL
LL
                                                   WASH WATER
                                                  FILTER CAKE TO T-ll
                                             COOLING WATER TO
                                             COOLING SYSTEM
                                                  COOLING WATER
                                              LEACH LIQUOR
                                                RECEIVER
                                              SIZE: 3' X3'6"
                                              MATL: 316 S.S.
                                                  COOLING WATER TO
                                                  COOLING SYSTEM
        IFACH LIQUOR FILTRATE PUMP
              MATL:  316 S.S.
 THE COAL PULVERIZING SYSTEM IS DESIGNED TO PRODUCE IN THE
RANGE 100% MINUS 8 MESH TO 100% MINUS 100 MESH.
 NORMAL OPERATING CONDITIONS FOR THE FOLLOWING EQUIP-
MENT ARE 50 PSIG AT 250 °F AND ALTERNATE CONDITIONS ARE
100PSIGAT250°F
     A.  P-1 SLURRY FEED PUMP
        R-l PRIMARY REACTOR
        V-l  COMPRESSOR SUCTION KNOCK OUT DRUM
        P-2 A THRU J (TEN REACTOR CIRCULATING PUMPS)
        K-l  OXYGEN RECYCLE COMPRESSOR
        M-2ATHRUJ   SLURRY MIXERS
        R-2  SECONDARY REACTOR
        P-3 REACTOR DISCHARGE PUMP
        M-12 4 13  SECONDARY REACTOR MIXERS
              B.
              C.
              D.
              E .
              F.
              G.
              H.
              I.
TRW
ONf 8PACI PARK .'ES555S?..»CM. C»uf
TRW (MEYERS) COAL DESULFURIZATION
PILOT PLANT
PROCESS FLOW DIAGRAM
onrsiiA

3087-AF-l
S
1


                                              113

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             K-3
       WASH WATER FILTER
         VACUUM PUMP
      SCFM AIR (SATURATED)
      MATL: CARBON STEEL
                          M-7
                     FIMAL WASH WATER
                     rnNTACTOR MIXER
                      MATL:  316S.S.
      T-13
   f|[MAL WASH
WATER rONTACTOR
  SIZE:  2'6" X 3'
   MATL:  FRP
         T-11
        ^«««iiiiiiiiii^_fe

      WASH W
       CONTA
m
      SIZE: 2'6" X 3'
       MATL:  FRD
M-6
WASH WATER
CONTACTOR
MIXER
MATL: 316 S.S.
S-3
WASH WATER
flilFJt
(BELT FILTER)
SIZE: 2' X 18'
MATL: 316 S.S.
V-4
FILTRATE
RECEIVER
SIZE: 3' X 3'6"
MATL: 316 S.S.
V-5
WASH WATER
RECEIVER
SIZE: 3' X 3'6"
MATL: 316 S.
E-2
WASH WATER
FILTER BAROMETRIC
dONDENSER
MATL:
CARBON STEEL
TOFILTERS-2
DWG PDG
3087-AF-l  QF1
 FROM
 FILTER S-2
 DWG. PDF
 3087-AF-l
                                                                COOLING WATER
                                                                TO COOLING
                                                                SYSTEM
                                                                COO LING WATER
                                                                TO COOLING
                                                                 SYSTEM
           P-1P
         WASH WATER
         CONTACTOR PUMP
         MATL: 316 S.S.
                         P-11        P-12
                     FILTRATFPUMP  WASH WATER^ PUMP
                     MATL 316S.S.   MATL: 316 S.S.
                    FINAL WASH WATER
                    CONTACTOR PUMP
                    MATL: 316 S.S.
                                         114

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     T-15
soivEKIT STRIPPER
   DECANTER
SIZE: 26"X 21"
MATL:  CARBON STEEL
    SP-7
ROTARY FEEDER
        .T-14
     AZEOTROPE STILL
     SIZE 40" X 30"
      MATL: 316 S.S.
 FIRST SOLVENT
  CENTRIFUGE
 MAUs  316 S.S.
          VENT
CENTRATE RECEIVER
  SIZE:  26" X 421"
  MATL: 316 S.S.
                                                M-8
                                             AZEOTROPE
                                             STILL MIXER
                                            MATL: 316 S.S.
       FINAL WASH
      WATER FILTER
    SIZE: 33" X 51 DRUM
    MATL: 316 S.S.
        E-3
  FINAL WASH WATER
BAROMETRIC CONDENSER
   VTL: CARBON STEEL
                     FINAL WASH WATER
                       VACUUM PUMP
                     SCFM AIR SATURATED
                     MATL: CARBON STEEL
                            V-6
                      FINAL WASH WATER
                       FILTER RECElWj~
                        SIZE: 42" X 48"
                        MATL: 316 S.S.
  QQ
                                                        QQ _
              VENT TO SP-5
                                  COOLING (33
                                  WATER TO
                                  COOLING
                 MATL: 316 S.S.
                          ,   —*.	J STILL   RICH SOLVENT
                          7  TBAMffFR PUMP   CENTRATE PUMP
                              MATL: 316 S.S.    MATL: 316 S.S.
                                                        - CONDENSATE
                                            115

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          E-4
      COAL COOLER
    MATL: CARBON STEEL
                 ROTARY FEEDER
                                                E-5
                                           SOLVENT STRIPPER
                                             CONDENSER
                                            MATL: CARBON-
                                                    STEEL
        A-6
FINAL COAL ELEVATOR
 MATL:  CARBON STEEL
       SP-4                  T-16
  SOLVENT STRIPPER    SOLVENT CONTACTOR
MATL: CARBON STEEL     SIZE: 32" X 27"
                      MATL: 316 S.S.
                                                  SOLVENT
                                               CONTACTOR MIXER
                                                 MATL:  316 S.S.
                                                               S-6
                                                           FINAL SOLVENT
                                                            CENTRIFUGE
                                                           MATL: 316 S.S.
     QQ
                                                                                QQ
     UU
                                                                      UU _
    .. RR
                                                                      RR
                                                                                W
     WW
                                                                               WW
     XX
                                                                     XX
                                                                                AB
  YY
                                                                                YY
                                I   VENT TO SP-5
                                |	^^^B^^k
                                                    N2 15 CFM FOR LEAKAGE ONLY
VENT TO SP-5
     NITROGEN
                                                                 STEAM
                                                    ELECTRIC     	
                                                      HEATER „!,_ STEAM HEATER
SOLVENT CONTACTOR PUMP
    MATL: 316 S.S.
                                                                                    AC
                                                                        kDRY COAL
                                                                          TO STORAGE
                                         116

-------
   JM8.
SOLVENT
      m
UPPER
SIZE: 26"X21'
MATL: CARBON STEEL

    T-20
 WASH WATER
 SURGE TANK
SIZE: 78" X 67"
    MATL: FRP
   QQ
       T-19
 AZEOTROPE STILL
     DECANTER
   SIZE 36" X 30"
MATL: CARBON STEEL
                                         T-22
                                                RICH SOL
                                                SURGE T/
                                     RICH SOLVENT
                                           TANK
    T-2?
LEAN SOLVENT
SURGE TAN 1C
SIZE 34" X 81"
                        ZEO
                       SURG
                 E TANK
                                                SIZE :46" X84"
                                             MATL:  CARBON STEEL   MATL: CARBON STEEL
                                        E-6
                       SIZE: 40" X 133"
                    MATL: CARBON STEEL
                                   AZEOTROPLSTILL
                                     goNpr
                                  MATL7TST
                                                          TEEL
                                                                                QQ
                                                         VENT TO SP-5
                                                          VENT TO SP-5     VENT TO SP-5
          VENT TO SP-5
               VENT TO SP-5
                                P-19
                            WASH WATER
                            SURGE TANK
                            PUMP
                            MATL: 316 S.S
                          P-20
                      AZEOTROPE   RICH SOLVENT
                      SURGE TANK  SURGE TANK
                      PUMP       PUMP
                      MATL: 316 S.S MATL: 316 S.S
                                                            LEAN SOLVENT
                                                            SURGE TANK
                                                            PUMP
                                                            MATL: 316 S.S
                                           117

-------
SOLVENT STILL
SIZE: 40" X 38"
MAIL: CARBON
   STEEL
                   SOLVENT STILL
                    CONDENSEF
                   MATL: CARBON
                           STEEL
      SULFUR FILTER
     MATL: CARBON
              STEEL

          T-24
  WASTE DISPOSAL TANK
     (FOR SOLVENT
CONTAINING MATERIALS)
     SIZE: 12' X 16'
   MATL: CARBON STEEL
    S-7
SULFUR FILTER
MATL: CARBON
        STEEL
        E-9
   SOLVENT COOLER
  MATL: CARBON STEEL
   QQ
                                                                  QQ
           CONDENSATE
 3.11 LB/HR
 TO COMPENSATE
 FOR LEAKAGE
    SOLVENT STILL PUMP
      MATL: 316 S.S.
            WASTE DISPOSAL PUMP
                MATL: 316 S.S
                                   118

-------
QQ
                                                             SP-5
                                                        VAPOR ABSORBER
                                                          SIZE:  2' X 4'
                                                        MATUCARBON STEEL
T-25A 4 T-25B



AK









( "

AL
VENT FROM S-4
VENT FROM T-2
VENT FROM T-2
VENT FROM T-2
VENT FROM S-!
VENT FROM T-l
VENT FROM S-<
VENT FROM T-l
VENT FROM T-l

(18) LEACH - QUOR
w BLEED
FROM DWG. 3037 AF-1
I
1 ton

r
25A I 1 T-25B
. T~

?^ — » — n
»35 	 S
1 ^ *y ^
; % S 	 „
65 	 5>







r
)
©
	 a
WASTE DISPOSAL TANKS
SIZE: 12' X 23'
MATERIAL: CRP
M II Fl ID TA HDI IAA^
AND STORAGE
* 	 ?

FLAME 1
ARREST OR Cp
x' *«\

SP-5
\^_ '' 	 3
~T
' **



' 	 ->
                                              TO WASTE DISPOSAL SYSTEM
             P-25
         WASTE DISPOSAL PUMP
            MATL: 316 S.S.
TWIT
si«rn»Ma«p
ONE SPACE PARK • REQONaa BEACH. CALIFORNIA
TRW (MEYERS) COAL DESULFURIZATIOK
PILOT PLANT
PROCESS FLOW DIAGRAM

3087-AF-2
                                      119

-------
APPENDIX    B
PROCESS MASS BALANCE
  COMPUTER PROGRAM
         121

-------
                               APPENDIX  B
                  PROCESS  MASS  BALANCE COMPUTER PROGRAM
A Fortran computer code prepared for the TRW time-sharing  computer is
reproduced in the following nine pages.   The design basis, upon which
the mass balance is based, was  discussed in  detail  in  Section  3.0 of the
report.   The internal  data and  input data are as  follows:
   ZIN and Z are the molecular  weight of the 10 components.
   AA are the names of the 10 components.
   X(I,J) is the mole  matrix (I=component, J=stream number).
   W(I,J) is the identical weight matrix.
   XT and WT are the total moles and weight  for each stream.
   P is  the reactor pressure (psig).
   Y is  the recycle Fe+3/Fe total  ratio.
   SOL is the solution/coal weight ratio in  the mixer  feed,
   FE is the weight percent iron in the  mixer feed.
   S is  the weight percent pyritic sulfur in the  coal.
   RX(1) is the percent of pyrite reacted at mixer  exit,
     (2) is the percent of pyrite reacted at exit of R-l.
     (3) is the percent of pyrite reacted at exit of R-2.
   VENT  is the weight  fraction  oxygen in dry vent gas.
   W(7,l) is moisture  on feed coal  per 1000  Ibs of  dry coal.
    (7,3) is steam required to  heat mixer charge.
    (7.11)  is flash steam  from  R-l  exit.
    (7,46)  is steam required to strip solvent on  dryer.
   NEW is zero for current flow sheet (1  for a proposed change).
   POREW is pore water/dry coal  ratio.
   SURFW is surface water/dry coal  ratio.
   PORET is pore toluene/dry coal  ratio.
   SURFT is surface toluene/dry coal  ratio.
   RECYC is oxygen fed to  R-l/oxygen  consumed ratio.
   PI  is  partial  pressure  of steam in R-l  gas.
   P2  is  partial  pressure  of steam in vent gas,
   EXCESS is  actual  toluene vaporize/theoretical  azeotrope toluene.
   HOLD  is  the  gpm/ft2  in  the sulfur filter,
                                   122

-------
i
L
   	H^HASSBAL(INPUT,OUTPUT,TAPEl*iNPUT,TAPE2,TAPES
t     HRillkN  Ub/l//75TTJPUATEtr~ 127177T5	
      COMMON  WUQ,6<0,X(10,b<») f Z (10) .0(7) ,XTf 6<»)
      DIMENSION  RX(3),WT(6i»),NN(3»,AA(10l,
                     -TT
      era i A t i i N i i > TT^T", i u) /1 j. viTqrqnre, j£. u«? b'Ti^n TIT, T9T.
     *98.082, 18. 016, 92.1%1, 32., 35./,
     *(AA(n,I-l,10)/10HCOAL      ,10HPYRITE     ,
                                                 IIUHHESOI*""
     *10HWAT£R      ,10HTOLUEN£   ,10HOXYGEN     ,19H INERT  GAS  /
      REMIND  2
      KtWiNO  3              " ' '"
      DO 9b 1=1,10
   96 Z(II-ZIN(I)
      uo
      H(J,I)±Q.
   98 X(J,I»=Q.                      _____
   ~~ Hti t>Mt WA i HI x nrr~7TNTr" iioL~; HAFKIX  onr
      ACCEPT ^AHEt^ST INPUT AND START CALCULATIONS
                            !—1000 LSS
      OISPLAir*  ENTER CHANGES, THEN $»,
      Ht2,l)=X(2,l)*Zi2>
           HULSU»
j    :  CALL HOLS<3»

	X(o,^>=J.
      CALL L3SC2)
      00 100 1-1*
        7 t2)*l««0 .f (SOL+1.1 -HT (1^1 -WT (21 -WT I 3)
                                   123

-------
	TTrreiHTrre T * W I 772 T
      CALL KEACTCRXCl)I
      0(U=0.
      00^02 T^l»7
  102 X»X(Ifl>+X(I*2-)+X«-QUI
      CALL
C     STREAMS  1  THROUGH  <*  ARE  COMPLETE
C     BEGIN OXYGEN  BALANCE
      HTm=3X/(0.995-(Q. GOS'VENT/il. -
      W(9t7)s0.995*WTC7)
      H(9,9»=HC9»7)-OX
      WllO9=WClflt ?)
      X(7,9)=P2*(X{9»9H-X (10,9) )/(PSIA-P2)
      frrTV9-T=xT7,ir*
      CALL MOLS(7)
                           COIFLETE
fc     3ESIN DXYGtM LOOP  CALCULATIONS
      H ( 9 » 6 ) = W T915) -OX
      W(10,6I=K(9,6)* (l
      CALL HOLS (6)
      WC7,6)=XI7,6i*Z(7)
     "YX = P2» fXTT, o )T
      XX=X(7,6»-XX
      'CALL sjMX(6f-9, 8)
      CALL SUHX(7,tt,5)
      CALL SAME (2t17}
     TT7TI7TS XT7T21 =
      CALL L3SC5)
      CALL L3SC8)
      WT{5)=HTOT(5)
                              124

-------
      HII1/I«MIOI IITT	
C     STREAMS 5,6,8,17  ARE  COMPLETE
C	BEGIN REACTOR  R-l CALCULATIONS
      CTStL SAMET5VTUT       "
      CALL REACTUX(2)-RX(1H
      00
      OXM=OX/Z(9)
                        * r 0 XTi
      X(b,ltJ)*X<&,10)-2.*OXM
      iiULAM  ifl  COffPLETE  FOR" REHCT£HTT?-1
      BEGIN REACTOR R-2
      X(7,ll)=t4(7,ll)/Z{7)
      GALL SAM£(12tl3)
      CALL REACT (RX(3>-RX< 2))
      DTT I0b  1=1,7
  106 X(Iv13)=X(If13) tOU)
      DO  108 I = lQ,i3
  108 MTCI
      STREA^^iltiZtia ARE  COMPLETE
      BEiiN CASHING  ANU FILTER ' UEG TTOH
      SOL ID=WC 1,131 tW<2»13)*WC3,13>
      WATER=SOLIO»(PORENfSURFNI
        *
      •i?o
  110
      UNMASHtU  CAKb  IhHHURAKlIY
      CALL SUMX(13,-19,53>
      F3*
      BEGIN ITERATION  OF  HASH LOOP
      DO 118 1-1, 100
  112
                              125

-------
      CALL SJH3 (32, -22, 231
      DO               '  " '
      X(J,20)=X(J,53)*F2*X(J,22)*F3
      CALL SJMXCS3,-20,2i)
         L su M 3 rzivzi 770 .....
      CALL SJM3C2i,23,2*»)
      00 116 J==»,6                 __
  116 X(J,33) = X(J,28) *F5
   	IFtABS< X (5,28 )* (1-F5 ) -X ($ ,,32)J_.LT.l. OE-7;i_GOi_ TO J.20

      IFtI.ea.99)OISPLAY*  SO**  LOOP  NOT CONVERGED*
  118 CONTINUE                                   _^	
  	FTRRIC SULFAIt  TS~BALSNC"ED TT3~U.HO0001 ~Ht>Ln.
C     CALCULATE STREAMS IN  WASH  LOOP
  120 XC7,201=1.4*WATER/Z(7)
 r
      CALL SJHX(21,23
      X(7,28I=X(7,21)
      00  122 I=*
  122 X4I-3,28»
      CALL SJMX(?8,29,3Q)
      CALL SUHX
-------
~~
      HO  126  I==X(I,20J*F2
      CALL  SJHX(2Q,-18,15)
      CALL
       CALL  SJHX(18,5<»,62I
£      COMPLETED RECYCLE, MAKEUP,  AND  BLEEQ  CALCULATION
C      SUKi  f ULUtNt "EXTRACT I O.T CALCUOTTD J5 -------------- .......
       SOLIDS (1,13)+W<2,13)
 _   TOL- (PQRET*SURFT)*SCLIO
       IT I 4 , 331 ~sRT37T3J              ........ ----    ------------ •
       W<8,l»0r=(2.*SOLID)-TQL
                           	
      wi»,t>y> =rii8,^y) +w i8,i»ii*W(a,
      W < » , 4<»* '* w I »» *if I * H 1 8 »
      TOLUEHi  WEIGHT BALANCE GOMPLEfE EXCEPT  STILL
      8£S IN f^i-^^^ a^ ^^ yjf 8Y ITERATING RECYCLE  L OOP
      Fl= IH 18, di&l-H <8,^9l ) /Hid* 36)
      F2=0.5*SURFr/CSURFT»PORET»
      00 128  I - 1,104
      IF(A3SCWC3,i»2)-WU,3^n.LT.1.0E-«»>GO  TO  130
  - i^iipfea>^JtUi^HLA<* i>UtmR LUUP NUI
  120
                              127

-------
C      SJJtFtfR  LOOP ''• CON VERGED TO 0»Q3Qt LO
  "Tiff" W C 3 1 3*»l = W ( 3 ,Ti2T~ ......
       W(3i3b)=HC3,33>+W(3t34)
                   3 61 ' -₯I 3 , 37T
       W(3,>i»=Wt3f39J
I       H(3
 ------
C      BEGIN  STILL CALCULATIONS--ST ILL  BOTTOM  10 POT SULFUR
C      FILTER FEEO SATURATED AT 95F, OR 2.7  PCT SULFUR
C ------ SHCfc.AH~b% Ii>"C»KE HffLaER ~ir.r GPH/FTZ=Zff3^iJ LB/ffR)
       IFiNEW.NE.UGO TO
c      TWO  OPTIONS:  132 FOR NE*, 13% FOS  OLD
t ---- gASLU  JN~HETT FfCFSH EEF-'-UTREUT ' REUrCTIE OF "KTJL Q Liu U ID
  132  Fl=0.1
       F2=0.027
       WC3,6ai=WC3,37)*F3/(F3-=HC3f60>
! -------- JrrST55T « H (8
      byIU
      DIRECT  RECYCLt NEW FLOWSHEET OPTION  COMPLETE
      8ASEO ON  OLO  FLOWSHEET--RECyCLE  THROUGH T-22
      H=U.l
      F2=0.027
      WT(57)=28.00.*HOLO
      «(8,57>=WT(57)-W(3,5/I
      F5=Fl*H(8,58)/
-------
[	Wt8i6lil»W<8,56>«HC8,98)
       M(3,61t=H(3,37)
p  -    «LL sKtftws THjfwufl THE ETTOrscrnrs  SECTION -ARE: DOMF
C      THE FINAL SECTION IS BASED ON NITKOGEN  STRIPPING
!C ___ STREAMS 48 AND 50 rfERE ELIMINATED BY  M2 STRIPPING
E      SI KtAHi ~Jf5"ANO *»6~WERE "REASSIGNED "
  136  W{7

       CUHPLtl t WETGTTT flTUT "HOL" C A UtTOL AT IDfTS"
       00  i38 1=13,33
       CALL L3S(II
       00  1<*U 1 = 1,2
       00  142 I=<*,b
|
       CALL L3SC«»6)
       CALL L3S(53)
       UALL
       CALL
       DO
                III
  144  WUI)=*TOTtI)
C      CALCULATIONS  COHPLETE, BEGIN OUTPUT
      DO  200  J=l,7
  200 NN(J*1I=NN(J)+1         	
  	WK11 fe M i-UU M111 iNN | K |> K»IT8T
                              129

-------
       rfRlTg(3»1002) AACJi IXIJ,K1,K-N,NF)
     WRIT£(3,100<»)
     00 2Qk J=l,10
     WKI it 1.5,1 DiFFFira" ij) t'~(WTJ»in
 20<» CONTINUE
     WRITE 13,1008) (HT «K) t K-N<>NF)	
"~2(T6 CUM I IN Jt
1000 FORMATi*l*////33X*PILOT PLANT  HASS OALANCfc*
    -t-33X*PASE *I1*  OF 8*//»  STREAM NO.*I1G,
L
 1002  FORMATI2X,Aifl,8F12.<»)
| I00«t  FQRHAT(/>^5X,*FLON RATE,  »-3/HR*|
 "TDTTE"
  1008  FORMAT(/»  TOTAL WT,*8F12.2)
       STOP
       ET?U        T "   ' ~ "   ' "	'
       SUBROUTINE HOLSCN)
       COMHOH WUO,fc<»l ,X<10»6*»»f Z(iO)
       UU  1U 1 =
    10  X(I,N)=W
       RETURN
I	
       tNU
       SUBROUriHE LBS(N)
       COHMON W(10,6^),X(iO,6!t),2(10),0(7)
   20
     uu
       RETURN
              =if lu
       SU3ROUT I NE «EAC T f PGT )
       COMMON H(lU,6t+) tX(10.fc'+l ,2(10»»OC7I
                            rrj~ ......        ~
      OI5)=9. 2*012)
               i fII
     Kt 1 UKN      '   '• .....
     END
     SUBROUTINE SUMX(I,J,KI
     UUHHUH M 1 10 y bi» ) , X MU
     XT(KJ=B.
                                           • »
                               130

-------
       TFTJTETTin
       J=J*H
       DO 30 1=1,10
    30  XT(K)=KT ,ZUO),om
       00  50  <=i,10
  ~~§B~XT
      RETURM
           _       .
      FU NO' T Iu N H i u i i N r
      COMMON  H(10,0i*) ,X(1U ,6
-------
APPENDIX     C
PILOT PLANT PLOT PLAN
  AND CONFIGURATION
          133

-------
 ftjut ei.af-tifa.MfW
PLAN a.uftrna.at'-tr
                                                                                                      \
                                                                              PLAN
                                                                                                                                        	
                                                                      1-1*1'111'Hi'lil MJ.!'!;.!'lit'Ui'm-lAI'lil'lAPf i  i»»»«i»««—w™««nnWr»I»T««» .<»
                                                                      '  6  "   *  "  "  •  »- ',  .*..,.  *   '   a   ijpm^mtmimmmmmmm.^mtwMHHmm,.
                                                                                                                      4fMnmM mfiNiMV
                                                                                                                                                       PILOT Ft ANT
                                                                                                                                                 —™" ap J-/f-yi m^.
\3087-AD-4

-------
CO
01

-------
u>
o»
                                                   PILOT PLANT CONFIGURATION

-------
      APPENDIX     D
COMPLETE PILOT PLANT EQUIPMENT LIST
                137

-------
CO
00
EQUIPMENT
NUMBER
P-l
P-2A-D
P-2E-K
P-2I-J
P-3
P-4
P-5
P-6
P-7
P-8
P-9
P-10
P-ll
P-12
P-13
P-14
P-15
P-16
P-17
P-18
P-19
P-20
P-21
P-22
P-23
P-24
P-2S
P-26
P-27
B-l
B-2
B-3
A-l
A- 2
A-3
A-4
A-5
A- 7
A-8
A-8a

SERVICE
SLURRY FEED PUMP
REACTOR RECIRCULATION PUMP
n ii it
ii it n
REACTOR DISCHARGE PIMP
THICKENER DISCHARGE PUMP
TRANSFER PUMP
REACTOR TEMPERATURE CONTROL
SURGE TANK PUMP
FILTRATE PUMP
WASH WATER PUMP
CONTACTOR PUMP
FILTRATE PUMP
WASH WATER PUMP
FINAL WASH WATER PUMP
PRODUCT COAL RECEIVER PUMP
AZEOTROPE STILL PUMP
SOLVENT CENTRATE PUMP
SOLVENT CONTACTOR PUMP
DELETED
WASH WATER SURGE PUMP
AZEOTROPE STILL PUMP
SOLVENT SURGE PUMP
LEAN SOLVENT SURGE PUMP
SOLVENT STILL PUMP
WASTE DISPOSAL PUMP
II II 'I
SUPPLY HYDROCLONE PUMP
TRANSFER PUMP
COAL DUST BLOWER
SCRUBBER BLOWER
COAL BLOWER
COAL FEEDER BELT
DELETED
COAL PULVERIZER SYSTEM
BIN DISCHARGER
WEIGH BELT FEEDER
RECEIVING HOPPER
LIVE BOTTOM BIN
LIVE HOPPER FOR A-8
VENDOR/FOB
POINT
McCANNA/Ill.
WEMCO/Cal .
FREDRICK/Tex .
GREGORY/Ohio
SOUTH LAND/Colo.
SOUTH LAND/CO lo.
EASTERN/Conn.
GREGORY/111.
GREGORY/111.
AMETEK/I11.
AMETEK/I11.
SOUTHLAND/ Colo.
AMETEK/I11.
AMETEK/I11.
SOUTHLAND/ Colo.
AMETEK/I11.
SOUTHLAND/ Colo.
EASTERN/Conn.
SOUTHLAND/Colo.
EASTERN/Conn.
EASTERN/Conn.
EASTERN/Conn.
EASTERN/Conn.
EASTERN/Conn.
DURI RON /Ohio
DURIRON/Ohio
WEMCO/Cal.
WEMCO/Cal .
EMPIRE/MO.
SHARPE/Ohio
EMPIRE/MO.
ND
EMPIRE/MO.
CARMAN/N.D.
K-TRON/N.J.
EMPIRE/MO.
ND
ND
DELIVERY
WEEKS
20
20
20
20
24
24
4
20
20
26
26
24
26
26
24
26
24
4
24
4
4
4
4
4
26
26
34
34
26
8
26
12
26
11
11
26
ND
ND
                                                                                                               EQUIPMENT
                                                                                                             CLASSIFICATION

                                                                                                                 Pumps
                                                                                                                Blowers
                                                                                                                Feeders
     REMARKS

2 pumps  (1 spare)
4 pumps
6 pumps  (2 spare)
2 pumps
                                                                                                                               Increased $100 over bid
                                                                                                                                 for increased size
                                                                                                                               Furnished with S-2 on skid
                                                                                                                                  ii        ii      ii

                                                                                                                               Furnished with S-3 on skid
                                                                                                                                  n        ii      it

                                                                                                                               Furnished with S-4 on skid
Increased  over $100 bid
  for increased size
  ti     it        „
Increased  $100 over bid for
  increased size, 3 pumps(2 spares)
                                                                                                                               Included in A-3

                                                                                                                               Included in A-3

                                                                                                                               Estimated, no quote received
                                                                                                                                Furnished with A-3
                                                                                                                                No quotations received
                                                                           COMPLETE  EQUIPMENT  LIST

-------
CO
vo
EQUIPMENT
 NUMBER

T-l

T-la
T-2
T-2a
T-3
T-4
T-S
T-6
T-7
T-8
T-9
T-10
T-ll
T-12
T-13
T-14
T-15
T-16
T-17
T-18
T-19
T-20
T-21
T-22
T-23
T-24
T-2Sa
T-25b
T-26

T-27

V-l
V-2
V-3
V-4
V-5
V-6

R-l
R-2
R-3
R-3a
                    K-l
                    K-2
                    K-3
                    K-4
    SERVICE

COAL STORAGE TANK

SLIDE GATE FOR T-l
SLURRY FEED SURGE TANK
HEADER FOR T-2
SCRUBBING COOLING DRUM
LEACH LIQUOR FLASH DRUM
COOLING WATER DRUM
LEACH SOLUTION MAtCE-UP DRUM
  ii       ii        ii     it
DELETED
LEACH SOLUTION SURGE TANK
  tl      II       IT     II
NASH HATER CONTACTOR
DELETED
WASH WATER CONTACTOR
AZEOTROPE STILL
RICH SOLVENT CENTRATE RECEIVER
SOLVENT CONTACTOR
DELETED
SOLVENT STRIPPER DECANTER
AZEOTROPE STILL DECANTER
WASH WATER SURGE TANK
AZEOTROPE SURGE TANK
RICH SOLVENT SURGE TANK
LEAN SOLVENT SURGE TANK
WASTE DISPOSAL TANK
                              HYDROCLONE SURGE TANK
                               COMPRESSOR  KNOCK-OUT DRUM
                               LEACH  LIQUOR RECEIVER
                               LEACH  WASH  RECEIVER
                               FILTRATE RECEIVER
                               WASH WATER  RECEIVER
                               FINAL  WASH  WATER FILTER RECEIVER

                               PRIMARY REACTOR
                               SECONDARY REACTOR
                               THICKENER
                               GUNITE LINING FOR R-3
            OXYGEN COMPRESSOR
            VACUUM PUMP
VENDOR/FOB
  POINT

MODERN/Cal.

MODERN/Cal.
MODERN/Cal.
   ND
FIBER-DYNE/Cal.
MODERN/Cal.
FIBER-DYNE/Cal.
FIBER-DYNE/Cal.
FIBER-DYBE/Cal.

FIBER-DYNE/Cal.
FIBER-DYNE/Cal.
FIBER-DYNE/Cal.

FIBER-DYNE/Cal.
MODERN/Cal.
MODERN/Cal.
MODERN/Cal.

WYSSMONT/Cal.
MODERN/Cal.
FIBER-DYNE/Cal.
MODERN/Cal.
MODERN/Cal.
MODERN/Cal.
MODERN/Cal.
FIBER-DYNE/Cal.
FIBER-DYNE/Cal.
MODERN/Cal.

MODERN/Cal.

MODERN/Cal.
AMETEK/I11.
AMETEK/I11.
AMETEK/I11.
AMETEK/I11.
AMETEK/I11.

HOWARD/Cal.
HOWARD/Cal.
 SOUTH LAND/Colo.
 SOUTHLAND/COlo.
                                             NASH/Conn.
                                             AMETEK/I11.
                                             AMETEK/I11.
                                             AMETEK/I11.
                                                                                               DELIVERY     EQUIPMENT
                                                                                                 WEEKS    CLASSIFICATION
52

52
52
ND
10
52
10
10
10

10
10
10

10
52
52
52

28
52
10
52
52
52
52
10
10
52

52

52
26
26
26
26
26

65
65
19
19
                        34
                        26
                        26
                        26
                                                                                                             Tanks
                                                                                                             Vessels
                                                                              Reactors
                                                                                                           Compressors
        REMARKS

Estimated $1000 added for
  extra connections
Estimated

Estimated
                                                                                               Increased by  $200 over bid
                                                                                                 for  extra support
                                                                                               Furnished with  S-2 on skid
                                                                                                  11       n    S-2   »
                                                                                                  "       "    S-3   "
                                                                                                          "    S-3   "
                                                                                                  ii       »    s-4   "
                                                                                               Estimate for field application
                                                                                                 of gunite
                           Furnished  with  S-2 on  skid
                                      n    s_3   ,,
                                          S-4   "
                                                                        COMPLETE  EQUIPMENT  LIST  (CONT'D)

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EQUIPMENT
NUMBER
E-l
E-2
E-3
E-4
E-S
E-6
E-7
E-8
E-9
M-1A/C
M-2A/J
M-3
M-4
M-5
M-6
M-7
M-8
M-9
M-10
M-ll
M-12
H-13
S-l
S-2
S-3
S-4
S-S
S-6
S-6a
S-7
S-8
S-9
S-10
S-ll
SP-1
SP-2
SP-3
SP-4
SP-5
SP-6
SP-7
SP-8
SP-9
SP-10A/C
SP-11
SP-1 2
SP-13
SP-14
C-l

SERVICE
BAROMETRIC CONDENSER
it ti
11 11
COAL COOLER
SOLVENT STRIPPER CONDENSER
AZEOTROPE STILL CONDENSER
SOLVENT STILL CONDENSER
DELETED
SOLVENT COOLER
SLURRY SURGE TANK MIXERS
REACTOR MIXERS
MAKE-UP TANK MIXER
It II tl
DELETED
WASH WATER TANK MIXER
FINAL WASH WATER TANK MIXER
AZEOTROPE STILL MIXER
WASH WATER CONTACTOR MIXER
HYDROCLONE SURGE TANK MIXER
II 11 M M
SECONDARY REACTOR MIXER
M it M
DELETED
LEACH LIQUOR FILTER
WASH WATER FILTER
FINAL WASH WATER FILTER
FIRST SOLVENT CENTRIFUGE
FINAL SOLVENT CENTRIFUGE
CONTROL BOARD FOR S-6
SULFUR FILTER
11 ii
CYCLONE COLLECTOR
SPINNER SEPARATOR
DUST COLLECTOR
SCRUBBER MIST ELIMINATOR
SLURRY HYCROCLONE
EVAPORATOR CRYSTALLIZER
SOLVENT STRIPPER
VAPOR ADSORBER
ROTARY FEEDER
ROTARY FEEDER
II tt
BASKET STRAINER
STATIC MIXERS
ROTARY VALVE
H n
ir M
ii M
SOLVENT STILL
All costs based on vendor quotes unless otherwise noted under "Remarks"
 No data.
VENDOR/FOB
POINT
AMETEK/IH.
AMETEK/I11.
AMETEK/I11.
WYSSMONT/N.J.
WYSSMONT/N.J.
BROWN/Ohio
BROWN/Ohio
ARMSTRONG/Penn.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LIGHTNING/N.Y.
LICHTNING/N.Y.
,
AMETEK/I11.
AMETEK/I11.
AMETEK/I11.
BAKER/Mich .
DORR-OLIVE R/Penn.
DORR-OLIVE R/Penn.
SPARKLE R/Tex.
SPARKLER/Tex.
EMPIRE/MO.
EMPIRE/MO.
E4PIRE/MO.
MODERN/Cal.
KREBS/Cal .
GOSLIN/Ala.
WYSSMONT/N.J.
MODERN/Cal .
WYSSMONT/N.J.
SPROUT-WALDREN/ Penn .
SPROUT-WALDREN/Penn .
BAILEY/N.D.
RAMCO/Cal .
EMPIRE/MO.
EMPIRE/MO.
EMPIRE/MO.
EMPIRE/MO.
HOWARD/Cal.
DELIVERY
WEEKS
26
26
26
28
28
13
12
16
15
15
15
IS
15
15
IS
IS
15
15
15
15
^
26
26
26
32
30
30
25
25
26
26
26
52
8
16
28
52
28
24
24
11
10
26
26
26
26
52
EQUIPMENT
CLASSIFICATION
Exchangers
11
11
11
ii
11
ii
M
Mixers
11
11
11
n
i
ii
11
ii
n
11
ii
Filters
It
26
n
ii
<":
11
II
II
tl
If
II
Miscellaneous
"
»
"
n
n
11
»
ti
M
11

"
"
If
                                                                                                        REMARKS


                                                                                                  Furnished with S-2 on skid
                                                                                                      ii      n  s_j   n
                                                                                                      "      "  S-4   "
                                                                                                      n      n  Sp_4  „
                                                                                                      "      "  SP-4  "
                                                                                                  3 mixers
                                                                                                  10 mixers
                                                                                                  Includes P-8,9,V-2,3,K-2,E-1
                                                                                                  Includes P-11.12.V-4,5,K-3.E-2
                                                                                                  Includes P-14,V-6.K-4,E-3
                                                                                                  Estimated
                                                                                                  Included in A-3
                                                                                                  Included with SP-4
                                                                                                  3 mixers
                                                                                                  Included with A-3
                                           COMPLETE  EQUIPMENT  LIST  (CONT'D)

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APPENDIX     E
CRITICAL PATH DIAGRAM
         141

-------
                               APPENDIX  E
                          CRITICAL  PATH  DIAGRAM
A critical path diagram indicating  the  time  phase  sequence  of pilot plant
construction activities is  presented  on the  following  page.   The  critical
path, indicated by the dark lines,  requires  87 weeks.   Of the 87  weeks,
there is one pacing item,  namely  the  delivery of the long lead time equip-
ment.  This time requirement (65  weeks) is dictated by the  quoted delivery
schedule for reactors  R-l  and R-2.  Were the procurement  activitites
associated with these  two  items of  equipment started prior  to the initi-
ation of the presented critical path, a maximum of up  to  13 weeks of
scheduled time could be saved.  The resultant construction  schedule would
then require 74 weeks.
                                  142

-------
CO
                       CRITICAL PATH SCHEDULE FOR PILOT PLANT CONSTRUCTION

-------

-------
                                                                                                                                                                                                                       TIMES SHOWN MtC IN WEKS
CJ1
                                                                                                                                                                                                                                                CMTICAL
                                                                                                                                                                                                                                                PATH
                                                                                                                                                                                                                                                t7 WEEKS
                                                                                                                                                                                                                                                OVBtAU
                                                                                                                                                                                                                                                LAKEO TIME

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    APPENDIX     F
REACTOR TEST UNIT FLOW DIAGRAM
               147

-------
4*
00

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to
                                                                                                                                                                                     TRW (MEYERS) COAL DESULPURIZATION
                                                                                                                                                                                            TEST REACTOR
                                                                                                                                                                                          PROCESS FLOW D.I A SRAM

-------
  APPENDIX      6
REACTOR TEST UNIT PLOT PLAN
     AND CONFIGURATION
             151

-------
(J1
ro
                                                     TEST REACTOR  PLOT PLAN

-------
en
CO
                                            ARTIST'S RENDITION  -  REACTOR TEST UNIT

-------
      APPENDIX    H
REACTOR TEST UNIT EQUIPMENT LIST
               155

-------
en
EQUIPMENT
 NUMBER

  A-2
  A-3

  A-5
  A-6

  T-l
  T-2
  T-3
  T-4
  T-5
  T-6
  T-7
  T-8
  M-l
  M-2
  M-3
  M-4
  thru
  M-l 3
  M-l 4
  El

  P-l
  P-2
  P-3
  thru
  P-6
  P-7
     SERVICE             VENDOR

BIN DISCHARGER           CARMAN
WEIGH BELT FEEDER        K-TRON

PORTABLE CONVEYOR
COARSE COAL BIN
DISCHARGER

FINE COAL STORAGE TK.
MIX TANK
COOLING WATER DRUM
FLASH TANK
LEACH SOLUTION SURGE TK.
LEACH SOLUTION SURGE TK.
WASTE DISPOSAL TANK
WATER STORAGE TANK

MIX TANK MIXER           LIGHTNIN
             ESTV'HP

                3/4
                1/3

BUCKEL ELEVATOR  1
TOTE            3/4


C.E. HOWARD
C,E. HOWARD
FIBER-DYNE
FIBER-DYNE
FIBER-DYNE
FIBER-DYNE
FIBER-DYNE
FIBER-DYNE

                1/3
                PRIMARY  REACTOR MIXER    LIGHTNIN
                SECONDARY  REACTOR MIXER

                COARSE  COAL HEAT EXCH.

                SLURRY  FEED PUMP
                REACTOR RECIRCULATION
                PUMPS
                SECONDARY REACTOR DISC
                PUMP
                         LIGHTNIN

                         BROWN

                         HILLS-McCANNA
                         LABOUR
                         LABOUR


                         HILLS-McCANNA
                                         3/4
                 3
                 1
                 1
                                                                   DELIVERY
                                                                    WEEKS

                                                                     10-12
                                                                     10--12

                                                                     10-12
                                                                     10-12


                                                                     12
                                                                     12
                                                                     12-14
                                                                     12-14
                                                                     12-14
                                                                     12-14
10


10


10

10

16-18
28-30
28-30


16-18
                REMARKS
         Includes Sample Valve,
         and  Flex. Connection
QUANTITY

    1
    10


     1
     1
     1
     1
     4
                                            REACTOR TEST UNIT EQUIPMENT LIST

-------
in
      EQUIPMENT
       NUMBER       SERVICE

        P-8      WASH PUMP
        P-9 _     FILTRATE  PUMP
        P-10      WASH WATER PUMP
        P-ll      LEACH SOLUTION CIRC.
                 PUMP
        P-12      LEACH SOLUTION FEED
                 PUMP
        P-13      FILTER WASTE PUMP
        P-14     WASTE DISPOSAL PUMP
        P-15     WATER TRANSFER PUMP
        K-l       VACUUM PUMP
        R-l       PRIMARY REACTOR
                 GENERATOR
        R-2       SECONDARY REACTOR
        R-3       COARSE COAL REACTOR
                 WASHER
        V-l       KNOCK-OUT DRUM.
        V-2       FILTRATE RECEIVER
        V-3       WASH WATER RECEIVER

        B-l       BLOWER

        B-2       COARSE COAL BLOWER

VENDOR
EASTERN


AMETEC
AMETEC
DEAN
SUNDYNE
EASTERN


WESTCO PUMP
EASTERN


AMETEC
C.E. HOWARD
C.E. HOWARD
C.E, HOWARD
C.E. HOWARD
AMETEC
AMETEC

EST. HP
1/2
115/220
10
2
2
15
5
1/2
1 1 5/220
10
10
1/2
115/220
10
30






DELIVERY
WEEKS
4-6




30
28-30
4-6


16-18
4-6



15
16
16
12



REMARKS
316 S.S. (Purchase Spare)


W/Filter Package
W/ Filter package


316 S.S.






W/Filter Package




W/Filter Package
W/Filter Package

QUANTITY
2


-
-
1
1
1


1
1


-
1
1
1
1

^
SHARPE HEATING  1/3
& VENT        110/230
SHARPE HEATING  1/3
& VENT        110/230
                                        REACTOR TEST UNIT EQUIPMENT  LIST  (CONT'D)

-------
     EQUIPMENT
      NUMBER       SERVICE

     SP-1       ROTARY FEEDER
     SP-2       SCRUBBER & MIST
                ELIMINATOR

     S-l        VACUUM FILTER

     NA         CRANE (FOR COARSE &
                FINE COAL]

     NA         TILT MECHANISM FOR
                FEED BIN FINE COAL
     NA         TILT MECHANISM FOR
                FEED BIN COARSE COAL
   VENDOR

SPROUT WALDRON
C.E, HOWARD
AMETEC

TOTE


TOTE



TOTE
 EST. HP

 1/2



35-40

 10
DELIVERY
 WEEKS

   12
   15
1st Quarter
  of 1976
    12
    12
              REMARKS
             0.175  CF/RE
Including vibrator
need 25 CFM of air
for unloading.

Including vibrator
need 25 CFM of air
for unloading.
                          QUANTITY
                              1
                              1
en
oo
                                       REACTOR TEST UNIT EQUIPMENT LIST (CONT'D)

-------
	 ' 	 	 	 	 — 	 	
TECHNICAL REPORT DATA
1 REPOR — ~ 	 • 	 (Please read Instructions on the reverse before comp
EPA-600/2-77-080
4. I 1 1 Lt AND SUBTITLE 	
Pilot Plant Design for Chemical Desulfurization
of Coal
L. J. Van Nice and M. J. Santy
9. PERFORMING ORGANIZATION NAME AND ADDRESS
TRW Systems Group
One Space Park
Redondo Beach, California 90278
f
12. SPONSORING AGENCY NAME AND ADDRESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
letingj 	
3. RECIPIENT'S ACCESSION- NO. I
5. REPORT DATE
April 1977
6. PERFORMING ORGANIZATION CODE I
8. PERFORMING ORGANIZATION REPORT NO
10. PROGRAM ELEMENT NO. I
1AB013; ROAP 21ADD-097
11. CONTRACT/GRANT NO.
68-02-1335
13. TYPE OF REPORT AND PERIOD COVERED 1
Final; 6/73-3/77
14. SPONSORING AGENCY CODE
EPA/600/13
is. SUPPLEMENTARY NOTES T£RL-RTP project officer L. Lorenzi is no longer with EPA: for I
details contact L.D.Tamny, Mail Drop 61, 919/549-8411 Ext 2851.
16. ABSTRACT The repOrt gives results of a program for design and operational planning
of facilities for testing the Meyers Process for chemical removal of pyritic sulfur
„ __. ,. vii 11 • ijtijji* «.i i
from coal.  Two options were evaluated: a complete pilot plant test of the process at
a 0. 5-ton per hour scale; and scale-up and testing of only the most critical portion of
the process, the reactor and regenerator section (reactor testing unit).   The report
includes: a summary of background process data; a discussion of the pilot plant design;
pilot plant start-up and operational test plans; and the preliminary design,  start-up,
and test approach for the reactor testing unit.  It also includes: process flow diagrams
for the complete pilot plant; pilot plant mass balance computer program; pilot plant
plot plans and a sketch of the facility; complete pilot plant equipment list; critical path
schedule for construction of the pilot plant; preliminary process flow diagrams for the
reactor testing unit approach; preliminary reactor test unit plot plans and a sketch of
the facility; and reactor test unit equipment list.
17. KEY WORDS AND DOCUMENT ANALYSIS j
a. DESCRIPTORS
Air Pollution
Coal
Coal Preparation
Desulfurization
Pilot Plants
Design
13. DISTRIBUTION STATEMtrn I
Unlimited
b.lDENTIFIERS/OPEN ENDED TERMS
Air Pollution Control
Stationary Sources
Pyritic Sulfur
Chemical Processes
Meyers Process
19. SECURITY CLASS (This Report)
Unclassified
20. SECURITY CLASS (This page)
Unclassified
c. cos AT I Field/Group ]
13B 1
21D
081
07A,07D
21. NO. OF PAGES
159 I
22. PRICE
EPA Form 2220-1 (9-73)
159

-------