United States
Environmental Protection
Agency
Industrial Environmental Research
Laboratory
Research Triangle Park NC 2771
Research and Development
EPA-600/S7-81-141b Dec. 1981
Project Summary
Evaluation of  the  Limestone
Dual Alkali  Prototype
System  at  Plant  Scholz:
Final  Report

J. A. Valencia, J. F. Peirson, Jr., and G. J. Ramans
  The limestone dual alkali process,
 developed by Thyssen-CEA Environ-
 mental Systems, Inc. (until late 1980
 under Combustion Equipment Asso-
 ciates, Inc. ownership) and Arthur D.
 Little, Inc., was tested at an existing
 20 MW prototype facility at Gulf
 Power Company's Scholz  Steam
 Plant. The intent of the project was to
 evaluate the technical feasibility of the
 process at a prototype scale  and to
 develop sufficient technical informa-
 tion leading to the implementation of
 the process at a full commercial scale.
  Due to budgetary considerations,
 the testing period was reduced from 6
 to 2 months. The report gives results
 obtained  during the  2 months of
 testing—February and March 1981.
 Excellent SO2 removal efficiencies in
 excess of 95 percent were achieved;
 limestone utilizations were also high,
 over 97 percent. The solids properties
 ranged from excellent  to poor. The
 generation of poor solids was the most
 significant process problem. The
 solids content in the filter cake was
 typically 35-45  percent, which was
 below the anticipated 55 percent. The
 soda ash consumption of 0.29 moles
 of Na2CO3/mole of SO2 removed far
 exceeded  the design consumption of
 0.04 moles of Na2CO3/mole of SO2.
 Much of this consumption was due to
 leaks  and other liquor  losses in the
 system. The mechanical performance
of the equipment, recommissioned
after 3 years of inactivity, was poor
and contributed to the above prob-
lems.
  Although the technology appears to
be technically feasible, further testing
is necessary before a conclusive
evaluation is made; some refinement
of the process is still needed.
  This Project Summary was devel-
oped by EPA's Industrial Environ-
mental Research Laboratory. Research
Triangle Park, NC, to announce key
findings of the research project that is
fully documented in a separate report
of the same title (see Project Report
ordering information at back).

Introduction
  The purpose of this test program was
to evaluate the performance, at a
prototype scale, of the limestone dual
alkali process  developed by Thyssen-
CEA Environmental Systems, Inc.(TESI)
(initially Combustion Equipment Asso-
ciates, Inc. (CEA)) and Arthur D. Little,
Inc. (ADL). The overall intent of this
project, however, was not only to
demonstrate the technical feasibility of
the process at a prototype level but to
supply technical  and cost information
related to the implementation of the
process at a full commercial scale.
  The test program was conducted at an
existing dual alkali facility at Gulf Power
Company's (GPC) Scholz Steam Plant

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near Sneads,  FL The 20  MW lime-
based dual alkali system was modified
for operation with limestone. Following
its conversion, the system underwent
an evaluation of its performance with
regard to:
  • S02 removal capabilities.
  • Raw materials and energy require-
    ments.
  • Quality of waste material generated.
  • Reliability and ease of operation of
    the system.
  Originally, the formal testing period of
the system was to last 6 months;  this
period was, however, reduced  to 2
months due to  budgetary  considera-
tions.
  Parallel to this EPA  program,  the
Electric Power Research Institute(EPRI)
sponsored a program to study  and
evaluate the landfill  disposal of the
waste cake generated by the limestone
dual alkali system.

The Scholz Prototype System

Limestone Dual Alkali
Technology
  The limestone dual alkali technology
is based on the absorption of S02 in an
alkaline sodium  solution, followed by
regeneration of the absorbing  solution
by  reaction  with a  second alkali,
calcium. These  reactions generate
insoluble calcium-sulfur salts which are
discharged from the system as a moist
cake.
  S02 is absorbed by contacting flue gas
with a sodium sulfite/bisulfite solution.
The sulfite reacts with the SO2 producing
additional bisulfite according to the
following overall  reaction:

  SOi + SO2 + H2O - 2  HSOa

  During absorption,  and to  a lesser
extent throughout the remainder of the
process, some sulfite is oxidized to
sulfate:

  SOI + 1 /2 O2 -SOJ

  The level of oxidation during absorp-
tion  is  generally a  function of  the
scrubber configuration, oxygen content
of the  flue  gas, and  the  scrubber
operating temperature.  At excess oxygen
concentrations normally encountered
in utility power  plant operations, the
level of oxidation is expected to be 5-10
percent of the SO2 removed (for medium
and high sulfur coal applications).
  The  spent scrubbing solution is
reacted with  limestone  to regenerate
the absorbent. The reaction precipitates
mixed calcium sulfite and sulfate solids,
resulting in a slurry containing up to 5
wt. percent insoluble solids.  The re-
generation  process involves basically
the following overall reactions:

   2 HSOa + CaCOa — SOa + CaS03
     •1/2H2Om/2H20
2 HSOS + Na:>SO4 + CaCOs - 2 SO3 +• CaS04
     •1/2H2Oi + 1/2H20
  Following regeneration, the insoluble
calcium-sulfur salts are separated from
the regenerated liquor. After settling in
a  thickener,  the insoluble  salts are
vacuum-filtered before being discharged
as a moist cake. The clarified liquor from
the thickener is returned to the scrubber,
closing the process liquor loop.
  The filter cake is washed to recover
most of the soluble sodium salts in the
mother liquor. A small portion of the
sodium salts, however, remains oc-
cluded in the cake  and is lost. Thus,
some sodium carbonate must be added
to the system to make up  for these
sodium  losses.  Typically, the Na2COa
makeup should  amount to less than 5
mole percent of the SO2 removed.
  The amount of limestone added to the
system for absorbent regeneration  is
reduced  slightly due to  the  soda ash
makeup.  Under  normal conditions, the
limestone feed  stoichiometry will  be
slightly less than 1.0 mole of CaCO3/
mole of S02 removed.

Description of the Scholz
System
  The dual alkali system took flue gas
from the  Scholz Steam Plant Unit No. 1 ,
a 40 MW nominal capacity (47 MW peak
capacity) Babcock and Wilcox pulver-
ized-coal-fired power boiler. The flue
gas from the boiler passed through a
high  efficiency,  sectionalized electro-
static precipitator (ESP) designed to
remove  up to  99.5  percent of the
paniculate  matter.  Part  of  the gas
discharged from the ESP was directed to
the limestone dual alkali system, which
was designed to handle flue  gas flow
rate equivalent to a 20 MW boiler load.
The remaining gas was sent directly to
the stack.
  The limestone dual alkali system  at
Scholz was a  modification of a lime dual
alkali system previously installed and
operated during 1975 and 1976 for a
test program sponsored by  Southern
Company and jointly funded with EPA.
The modified dual alkali system con-
sisted of four  sections:  absorption,
regeneration, waste solids dewaterini
and  raw materials storage  and fee
preparation. A process flow diagram fc
the dual alkali system  for  Scholz  i
shown in Figure 1.
  The absorption system consisted of
venturi scrubber, followed by an absorp
tion tower. An SOz injection system wa
provided to increase, when necessan,
the SO2 concentration in the flue ga
entering the dual alkali system by 2O
ppm or more.
  The variable throat, plumb-bob typ
venturi scrubber  was  designed fo
particulate removal and/or S02 ab
sorption. Typically, a dual alkali systerr
taking flue gas from  a particulat
removal device (e.g.,  ESP) would no
require a venturi scrubber. Such beini
the case at Scholz, the system in fact dii
not require the venturi scrubber. Rathe
than remove it, the venturi scrubbe
was used primarily for quenching an<
saturating the flue gas;  these opera
tions, which also contribute to the SO;
removal, would normally be performec
in the absorption tower. A booster far
directed the S02-rich flue gas exitinc
the ESP into the  scrubber, where i
contacted scrubbing liquor flowing at ar
L/G of 15-20 gal./IO*5 acf.* The liquo:
was collected  at  the bottom of the
scrubber in an internal recycle tank.  ^
  After  being quenched  and saturatec
with water, the partially desulfurizec
gas entered the bottom of the absorption
tower. Gas passed upward through twc
trays and then through a de-entrainmenl
separator. A spray under the bottom tray
was used to wet the  underside of the
tray. The de-entrainme'nt separator was
operated dry, without mist eliminator
wash water. The  scrubbing solution,
which  was fed to  the top tray of the
absorber at an L/G of 2-3 gal./106 acf,
flowed countercurrent 'to the  gas
through the tray system. This counter-
flow permitted high SO2 transfer from
gas  to  liquid  phase. The liquor was
collected at the bottom of the absorber
in the  internal recycle tank, which
served as the supply for the liquor spray
under the bottom tray.
  A  bleed  from the  absorber liquor
recycle  line was sent forward to the
scrubber recirculation loop where it was
used to quench the  gas and  provide
additional SO? removal. A bleed stream
of spent liquor was  drawn from the
scrubber recycle  line and  fed  to the
absorbent regeneration system.
 (*) To convert from British to metric units: multiplv
 gal by 3.79 to yield liters, and multiply cf (ft3; 6y
 0 028 to yield m3.

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                                       SO2/OZ
                                       Outlet
                                       Probe
         «Cleaned
         I   Gas
SOa
Injection
 Water
Normal Flow
Alternate Flow	
 uigure  1.    Limestone dual alkali system at Scholz - process flow diagram.
   The regeneration system consisted of
 five separate reactors in series with a
 total design holdup time of approximately
 100 minutes. It was designed to provide
 the capability of operation  in various
 configurations. The bleed from the
 scrubber system was piped such that it
 could be fed either to the first or second
 stage  reactor. Similarly, the limestone
 silo feed chute could feed dry limestone
 to either of these two tanks. Thus, the
 modified reactor system was capable of
 being  operated  as  either four or five
 reactor tanks in series with dry  lime-
 stone  feed, or as four reactor  tanks in
 series with  slurried limestone  feed
 prepared in  the first stage  reactor.
 Furthermore, the three intermediate
 reactors had  overflows at two  levels to
 provide the  flexibility of varying the
 holdup time. Due to the shortened
 testing period, however, the regenera-
 tion system was operated in only one
 mode: five reactors  in series with dry
 limestone feed to the first reactor. The
 first four reactors operated on overflow
 (high overflow for the three intermediate
 reactors), while the last reactor was on
level control so that the effluent could
be pumped to the thickener.
  Clear liquor overflow from the thick-
ener was collected in the thickener hold
tank which acted as surge capacity for
the absorbent liquor feed to the scrubber
system.  Process makeup water was
added  to this tank to  make up for the
total water loss due to evaporation in
the system and moisture in the cake:
  The  thickened  slurry was  fed to  a
rotary  drum vacuum filter. A series of
wash sections were used  to wash the
filter cake in order to  recover valuable
process  liquor. Solids from the filter
cake were discharged to a weigh belt
conveyor for transport to the waste
processing system. The mixed filtrate
and wash liquor from the filter were
returned to the thickener.
  Two raw materials were required for
operation of the system—limestone for
absorbent regeneration and soda ash to
make up for losses of sodium salts in the
waste  filter  cake. Finely ground lime-
stone was received, stored, and fed to
the system in  a  dry form.  Dense soda
ash was used for the makeup soda ash
solution, which was normally prepared
using clarified liquor from the thickener
hold tank; occasionally, river water was
used for preparing this solution but only
when the additional water input did not
upset the system volume balance. The
makeup soda ash solution was fed back
to the thickener hold tank to be mixed
with the regenerated scrubbing solution
and pumped forward to the absorber.
  The  waste  processing  system  was
installed  and operated as part of  a
separate test program funded by EPRI. It
is briefly discussed here to indicate its
relation to overall plant operation.
  The  moist waste  cake discharged
from the vacuum filter was mixed in a
pug mill with fly ash and lime. Fly ash
was added at approximately one part of
ash per part of dry solids in the cake.
Lime was added at a rate of 3-5  wt.
percent of the dry solids contained in the
mix of  cake  and fly ash. The  mix
discharged by the pug mill was trucked
to a landfill test area. Mixed material not
meeting  specifications or untreated
filter cake—when the waste processing
system was unavailable or inoperative—

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were  disposed  of in a separate "off-
spec" disposal area.

Operating History
  System design  and test program
planning began in  September 1978,
immediately  after EPA awarded the
contract for the project. Recommission-
ing and conversion of the  existing
system to a limestone dual alkali system
began in March 1979 and was completed
by March 1980.
  Process operations were  initiated in
August 1980. In the interim, the system
was operated mechanically to prevent
mechanical deterioration of the equip-
ment. This delay was caused by equip-
ment delivery problems encountered in
the installation of the EPRI waste
disposal system.  As  the expenses
associated with the mechanical opera-
tion continued  to accumulate, it was
decided to start up the system in August
even though the EPRI system was not
yet completely installed. Formal testing
of the dual alkali system did not start
until February 1980 when the S02 and
Oz  monitors were finally placed in
operation. During this period—August
20, 1980, to  the end of January—the
system was operated for about 57 days
and was down  for about 107 days. Of
the downtime in this initial startup and
break-in testing period, 43 percent was
attributable to mechanical problems
(e.g.,  leak in the thickener tank), 20
percent  to process problems (e.g.,
generation of solids with poor  settling
characteristics), 26 percent  to the time
needed  to  resolve CEA's bankruptcy-
related issues*, 7 percent  to a lack of
raw materials (due to reluctant suppliers
in light of the bankruptcy declaration),
and 4 percent to miscellaneous causes
(e.g., boiler outage).
  System tests began on February 2,
1981, and  extended until  March 28,
1981. During this  period,  the  system
was operated for 925 hours (38.5 days)
or 71.4  percent of the time,  and  it
recorded one completely uninterrupted
period of operation of  431  hours (18
days).
 •On October 20, 1980, CEA filed a petition for
 financial reorganization pursuant to Chapter 11 of
 the U S. Bankruptcy Code Thyssen-CEA Environ-
 mental Systems, Inc. (TESI) bought the CEA Air
 Pollution  Division  and  administered this  EPA
 contract starting in early December 1980, assuming
 financial responsibilities retroactive to October 21,
 1980. The  EPA contract for this  project  was
 formally assigned to TESI in April 1981  CEA is
 referenced  in this report to maintain historic
 integrity
  Outages during the test period were
due primarily to mechanical problems
(filter repairs) which accounted for 63
percent of the downtime, and to process
problems (resuspension of solids left in
thickener while  repairing  the filter)
which accounted  for 30 percent of the
downtime.

System Performance
  Given the  limited tests performed,
due to the reduction of testing from 6 to
2  months,  a final and conclusive
evaluation of the technology, leading to
its full-scale commercialization, cannot
be made at  this time. Nevertheless, a
number of very encouraging qualities of
this technology have  been  clearly
identified. Problem areas that will
require further refinement have been
identified as well.

S(?2  Removal
  The SO2  removal capability was
excellent. During  the tests, the system
averaged an S02  removal efficiency of
95.8 percent. S02 removal efficiencies
were  easily controlled by simply ad-
justing the pH  of the scrubber bleed
liquor. SOz removal efficiencies greater
than  90 percent were  obtained by
maintaining  a scrubber bleed  pH of at
least 5.5. Outlet SOa concentrations of
less  than  100  ppm were obtained  at
scrubber bleed pH's higher than 5.7;
concentrations less than 50 ppm were
obtained at a  pH  of 6.0.  Inlet  S02
concentrations  during this period
ranged from  1460  to 3240 ppm and
averaged slightly over 2000 ppm.

Limestone Utilization
  Limestone utilization  by  the dual
alkali system was very good. During the
test period,  utilizations in the reactor
train effluent were 85-95 percent of the
available CaCOa in the raw limestone.
As the reaction with limestone continued
in the dewatering system, the final
system utilizations, determined from
chemical analyses  of the filter cake,
were  93-100 percent, averaging 97.5
percent.

Oxidation and Suit ate
Precipitation
  About 18 percent of the S02 removed
by the scrubbing solution was oxidized
to sulfate as it  passed through the
system. As  anticipated,  most of this
oxidation, as much as 90 percent, took
place in the absorber/ scrubber section.
The  capabilities of the system to co-
precipitate calcium sulfate along with
calcium sulfite  were adequate  to
remove the sulfate formed. The soluble
sulfate concentration in  the system
achieved a  steady level about  1  M.
Although liquor losses (due  to leaks,
spills, and purges to maintain the liquor
volume balance in the system) con-
tributed to the removal of sulfate from
the system, the sulfate concentration in
a tight closed-loop operation  is not
expected to rise above 1.2 M, which
appears to be  within  the sulfate co-
precipitating capabilities of the system.
Waste Solids
  The  generation of solids with good
settling characteristics was the most
significant  process  limitation encoun-
tered at Scholz. It essentially accounted
for all  of the process-related outages.
Throughout December and February,
solids with  excellent settling character-
istics were  generated. In contrast, poor
solids were generated in January. The
good settling solids were agglomerates,
roughly spherical in shape; whereas,
the  poor  solids were  fine, needle-
shaped solids. These fine solids, when-
ever carried  over  in the thickener
overflow in noticeable amounts (>1000
ppm),  promoted the formation  in  the
reactors of more fine and  difficult-to-
settle solids. While on some occasions,
the formation  of these fine solids was
stopped by process changes, in others it
simply continued to  deteriorate, forcing
interruptions  in system  operation.
Although some mechanical problems
intensified the difficulties in the settling
of solids, the fundamental physical and
chemical reasons for  the formation of
poor settling solids  are  not clearly
understood,  and therefore require
further investigation.
  The  solids appeared,  in  general, to
have good  dewatering characteristics;
nevertheless, the typical solids content
in the  cake was 35-45 wt. percent, far
below  the  anticipated 55 wt. percent.
Severe mechanical  problems with  the
filter and associated pumps and piping
were the  major factors in  this short-
coming. Closely  associated with this
problem were the high sodium losses in
the waste filter cake.
  It  appears  that both of these prob-
lems—low  solids content of the cake
and high  sodium losses—are  not
inherent to the limestone  dual alkali
technology, but were  rather caused by
the mechanical condition of the equip-
ment used.
                                                                                                                   4

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Soda Ash Consumption
  Soda ash consumption was excessive,
amounting  to  about 0.29 mole of
Na2C03/mole of SO2 removed,  far
above the design value of 0.04 mole of
NaaSOs/mole of SOz  removed. Soda
ash is fed to the system to make up for
'normal  sodium  losses in the liquor
entrained in the  filter cake. At Scholz,
however,  not only were the sodium
losses high in the filter cake, but much
sodium  was lost through leaks, spills,
and liquor purges needed to maintain
the liquor volume balance in the system.
(Large amounts of seal  water were
needed  to keep  worn  out  pumps in
operation which, coupled with heavy
rains, were very  taxing on the  limited
surge capacity available.)
  Again, this excessive soda ash con-
sumption problem does not appear to be
inherent to  the  limestone dual alkali
technology.

Power Consumption
  Power consumption ranged from 2.5
percent  (0.53 MW)—at flue gas rates
equivalent to a boiler load of 21 MW—to
5.3 percent (0.42 MW)—at an equivalent
load of 8 MW. In a typical limestone dual
alkali  application, where flue  gas is
taken from an ESP and the use  of a
venturi  is not  required, one  would
expect the power consumption to be
much lower—more like 1 -1.5 percent of
the power generated at full boiler load.

Process Operability
  Process operability, unlike equipment
or mechanical operability, refers to: the
ease with which the  system can be
operated and controlled, the ability of
the system to adequately respond to
varying conditions, and the ability of the
system  to tolerate  upsets in process
chemistry due to mechanical problems
or operator oversight.
  In general, process  operability  was
good after the first 2 or 3 days of stable
operation. It was during these initial
days, following any  restart  of  the
system,  that problems with process
operability were encountered. All of
these related to the generation of solids
with poor settling characteristics.
  Once  the  system reached a stable
operation, such as during December or
February, process operability was very
good.  The system was able  to easily
accommodate variations in  inlet  S02
concentrations of as much as 500 ppm,
by simply adjusting the feed forward
rate  of  regenerated  solution  to  the
absorber/scrubber to maintain  a con-
stant bleed pH. Variations in boiler load
and thus in the amount of gas processed
were accommodated  in  the same
fashion.
  Upsets to process chemistry were
also handled well by the system. These
upsets included the carryover of fly ash
in the flue gas due to a  malfunction in
the ESPs,  the gross overfeeding  of
limestone due to operator oversight,
and occasional limestone and soda ash
outages lasting from 1 to 5 hours.

Mechanical Performance
  The mechanical performance of the
equipment  and its associated  instru-
mentation represented a major source
of problems at Scholz:  43 percent  of
system downtime during the start-up
and  break-in and  59  percent  of the
downtime during testing were due  to
mechanical problems.  Not only  was
system availability affected by these
mechanical problems, but also system
operating conditions were affected. An
example of these limitations was the
inability of undersized thickener under-
flow pumps to handle slurry with more
than  15 wt. percent  solids,  which
required  the dilution  of  the  20-25
percent thickener underflow  slurry.
Although some of the problems were
caused by the limited capacity of an
existing piece of equipment, most of the
mechanical problems were due  to
equipment failures. The age  of the
equipment and its condition, even after
recommissioning,  were, undoubtedly,
primary causes of these failures.

Conclusions
  System performance, summarized
above, leads  to the following conclu-
sions:
  • The limestone dual alkali process
    appears to be technically feasible.
  • Further  testing is required  to
    reinforce the above conclusion and
    to develop sufficient process in-
    formation needed for full-scale
    commercialization.
  It is also recommended that laboratory
or small pilot plant tests, to better
understand  the generation of solids
with good settling characteristics, be
performed prior to any further prototype
scale testing.

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J. Valencia andJ. Peirson are with Arthur D. Little, Inc.. Acorn Park, Cambridge,
  MA 02140; G, Ramans is with Thyssen-CEA Environmental Systems, Inc..
  555 Madison Avenue, New York,  NY 10022.
Norman Kaplan is the EPA Project  Officer (see belowj.
The complete report, entitled "Evaluation of the Limestone Dual Alkali Prototype
  System at Plant Scholz: Final Report," (Order No. PB 82-110 685; Cost: $12.00.
  subject to change) will be available only from:
        National Technical Information Service
        5285 Port Royal Road
        Springfield, VA 22161
        Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
        Industrial Environmental Research Laboratory
        U.S. Environmental Protection Agency
        Research Triangle Park, NC 27711
                                                                           U.S. GOVERNMENT PRINTING OFFICE-.1981--559-092/3362

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