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
16
-------
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
-------
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
-------
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
-------
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
20
-------
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.
21
-------
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).
22
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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
-------
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.
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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
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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
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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)
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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.
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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.
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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.
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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.
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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
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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]
-------
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.
65
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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
-------
• 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
68
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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.
-------
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
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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
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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
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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
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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.
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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".
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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
-------
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.
89
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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
90
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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
-------
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.
-------
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
93
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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)
94
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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
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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
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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
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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
-------
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
-------
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
-------
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
-------
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)
-------
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)
-------
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
-------
APPENDIX F
REACTOR TEST UNIT FLOW DIAGRAM
147
-------
4*
00
-------
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
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