United States
Environmental Protection
Agency
Air and Energy Engineering
Research Laboratory
Research Triangle Park NC 27711
Research and Development
EPA/600/S7-87/020 Apr. 1988
Project Summary
Influence of Coal  Mineral
Matter  on the  Effectiveness  of
Dry Sorbent  Injection for 862
Control
D. M. Slaughter, W. J. Thomson, T. W. Peterson, S. L. Chen, W. R. Seeker,
and D. W. Pershing
  This report summarizes the results of
a detailed examination of the interac-
tions between calcium based sorbents
and chemical species which could
either enhance or detract from the
sorbents' ability to  capture SO2 in
pulverized coal flames.  Previous,
limited experimental studies had indi-
cated that sorbent performance would
be influenced by various inorganic
compounds, particularly those occur-
ring in coal mineral matter.
  This Project Summary  was devel-
oped by EPA's Air and Energy Engi-
neering 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),

Program Objectives
  The overall program objectives were to:
(1) determine the influence of mineral
ash constituents on the sulfur capture
performance of calcium based sorbents,
(2) define the chemical compounds
which can enhance the ability of the
calcium based sorbents to capture SO2
and identify the mechanism(s) of promo-
tion, (3) establish the influence of mineral
ash on the  effectiveness of sorbent
promoters, and (4) optimize the process
for adding promoter  materials to the
sorbents.
Program Scope
  A combined experimental and theoret-
ical approach was used in this study.
Programs examined the  physical and
chemical changes of a wide variety of
sorbents with carefully selected chem-
ical additives under different composition
environments and over the  range of
time/temperature histories. Experimen-
tal testing was  conducted in furnace
facilities ranging from laboratory to small
pilot scale with both natural gas and coal
as the primary fuel. Thermal histories
ranging from near isothermal to highly
quenched conditions were considered.
Fundamental mechanistic information
on the interactions between the pro-
moters and calcium based sorbents were
obtained from a  dynamic x-ray diffrac-
tometer (DXRD)  and from extensive
investigation of solid samples extracted
from the combustion furnaces. Chemical
and elemental  analysis techniques
included electron microscopy (scanning
and transmission), energy dispersion
spectroscopy, and x-ray diffractometry.
DXRD  was used  to trace the formation
of chemcial species and the destruction
of solid, promoted and  unpromoted,
calcium compounds as a function of time
and temperature. Microscopy and spec-
troscopy techniques were used to char-
acterize the physical  morphology and
elemental spatial  distribution of the
promoter, calcium sorbent, and chemical

-------
constituents of the mineral ash. X-ray
analysis was used to quantify chemical
species present. Equilibrium calculations
based on free energy minimization were
used to characterize the probable gas and
solid phase species. The MAEROS com-
puter  program was used to involve the
multicomponent  population balance
equations governing the coagulation,
fragmentation,  condensation,  and
nucleation of  the ash and  promoter
aerosols system.

Coal/Sorbent Interactions
  Under certain limited conditions, coal
mineral matter can influence the effec-
tiveness  of calcitic sorbents.  If  the
mineral matter and sorbent are in direct
intimate contact  (particularly  by simul-
taneous pulverization) prior to injection
and  if they are injected through  the
burner into the temperature regions of
a boiler, sorbent performance may be
reduced.  The  controlling mechanism
appears to involve the formation of low
melting eutectics:  the calcium  reacts
chemically with  various alumina  and
silica  components  of the  ash  and
becomes  unavailable  for subsequent
sulfation.  Because  of  this interaction
(and because of  the deleterious effects
of the flame zone on the sorbent itself)
burner injection  cannot  be  recom-
mended.  If, however, the sorbent  is
injected separately from the pulverized
coal (either with the secondary air or
downstream) then essentially no sorbent
deactivation due to  mineral  matter
occurs.  Modelling calculations indicate
that particle/particle collision frequen-
cies are simply not adequate to deacti-
vate a significant number of the sorbent
particles.  Figure  1 shows data obtained
in the 293 kW boiler simulator  furnace
(BSF) with both  limestone (i.e., Vicron)
and hydrated (i.e., Longview) sorbents
injected with the fuel and downstream.
A wide range of normal and cleaned coals
were tested in this sequence, and the
results  compare  favorably with the data
taken firing natural gas. No evidence of
ash deactivation was observed with any
coal. Therefore, the performance of the
current limestone injection multistage
burner  (LIMB) concept (separate down-
stream sorbent injection) should not be
significantly degraded by mineral ash
effects.

Promoter/Sorbent Interactions
  A major series of promoter  screening
tests  indicated that chromium  series
transition elements and alkali metals can
                 Vicron

        W/Fuel       Downstream
      Longview

W/Fuel      Downstream
  60
 §50
 §30
 o
  10
                         American
                         Boiler (AB)
                         Profile

                        O Natural Gas
                        • Indiana #3
                        m Illinois
                        A Kentucky
                        * Lower Kittannir
                        • Lower
                          Kittanning
                          Clean Coal
                          (1-35)
        123      123      123      12
         Ca/S          Ca/S           Ca/S           Ca/S
Figure 1.    effect of fuel type on SOi capture with Vicron and Longview.
effectively increase the ability of calcium
based sorbents to capture SO2. Figure 2
summarizes data obtained in the bench
scale Control  Temperature Tower (CTT)
furnace with  limestone  and indicates
that all of the alkali metals significantly
enhance the measured SO2 capture. The
primary enhancement mechanism is not
chemical catalysis of  the SOz to SO3
reaction  step; rather, these materials
react chemically with the CaO to produce
local physical changes in the sorbent
which enhance  sorbent capture.  In
particular,  both  the  chromium series
elements and the alkali metals appear
to induce particle fragmentation, crea-
tion  of large  cracks, and  pore enlarge-
ment, all of which increase  the acces-
sibility  of the  interior  calcium and
decrease the  rate of site loss by pore
mouth plugging. In addition, the pro-
moters often produce low  melting eutec-
tics with the CaO, and this liquid phase
may enhance the local transport of the
SOz  to the unreacted CaO. In  addition
to affecting the sorbent morphology, the
alkali metal promoters also directly react
with SO2 to  produce  sulfate products;
they effectively function as sorbents
themselves. The chromium compounds
do not exhibit this behavior.

Coal/Promoter Interactions
  Unfortunately, the  effectiveness  of
promoted sorbents for SOz control may
be significantly less in actual, coal fired
systems than  in SOz doped, natural gas
tests due to the presence of coal mineral
matter, in particular the submicron ash
aerosol.  Figure  3 summarizes a wide
series of tests conducted to evaluate the
 influence of coal mineral matter constit-
 uents on the promotion of limestone and
 hydrated  sorbents by both NaHC03 and
 Cr2O3. These data indicate that under all
 conditions tested both the sodium and
 the chromium produced  significant
 increases in sorbent utilization in the ash
 free  experiments (natural  gas  firing).
 However, with all of the sodium promo-
 tion cases and with the chromium cases
 where the sorbent was added within the
 burner zone,  the promotion effect was
 greatly reduced with coal firing.  Only
 when the sorbent  was added down-
 stream and the promoter was Cr203, was
 the beneficial effect retained  in the
 presence of  coal firing.  With sodium
 promotion external contact between the
 promoted sorbent and the  coal is not
 required; separate injection still leads to
 deactivation. EDS analysis confirmed the
 presence of sodium on the mineral ash
 as well as the sorbent, suggesting that
 the controlling mechanism  is vaporiza-
 tion and  uniform sodium condensation.
 Condensation modeling calculations
 indicated that more than  90% of the
 added sodium could condense on the
 submicron ash aerosol  if the sorbent
 particles are large  and the internal
 surface  area is  not readily avialable.
 X-ray diffractograms indicated that the
 condensed  sodium reacted with the
 refractory oxides in the coal ash to form
 sodium  silicates,  thereby effectively
 reducing  the sodium available for direct
 reaction with SOZ. Thus, the effective-
 ness of sodium promotion is reduced in
 coal  fired systems simply  because the
 promoter itself condenses on the submi-
 cron ash  aerosol and the amount avail-
 able  for  enhancement  of  the  calcium

-------
     70
     60
     50
     40
  I
  O 30
     20
     10
                                                    Control
                                                    Temperature
                                                    Tower
             Natural Gas
             1500 K Injection


            £±  Vfcron + LiiCOt


            D  Vicron + NaHCO3


            Q  Vicron + K2CO3


            Q  Vicron
are almost  certainly environmentally
unacceptable.  Figure 4 illustrates data
obtained with a chromium-promoted
pressure-hydrated  calcitic sorbent and
indicates that capture levels in excess of
70% were achieved at a  Ca/S  ratio of
2.0. Unfortunately, to date it has not been
possible to identify an environmentally
acceptable promoter capable of inducing
the morphological changes produced by
chromium with a sufficiently low vola-
tility to avoid  vaporization and  subse-
quent scavenging by the ash aerosol.
                        Ca/S
Figure 2.   Summary of SOz capture with alkali metals.
sorbents is greatly reduced. The coal ash
has less influence on chromium promo-
tion  because  chromium  is  a  far  less
volatile promoter. EDS analysis indicated
that the chromium was primarily asso-
ciated with the calcium; little chromium
was found with the ash,  particularly in
the downstream injection cases.

Application Considerations
  Parametric process studies indicated
that the chemical  form of  the  sodium
promoter is not significant. Particle size
can influence promotion;  large particles
may not be completely  vaporized  and
dispersed in the residence time available.
Because of the vapor phase transport of
the alkali  metals,  they need  not  be
injected with the  sorbent  particles to
provide effective promotion (in the
absence of an ash aerosol).
  Various, externally  generated pro-
moted sorbents  were  produced and
evaluated  in  an attempt to avoid the
deleterious effects of the ash aerosol.
However, even hydration in the presence
of sodium did not overcome this problem;
at normal LIMB injection temperatures
the sodium still tends to vaporize initially
anda large fraction ultimately condenses
on the submicron aerosol. Conversely,
chromium promotion can be optimized to
produce extremely high capture  levels,
although chromium promoted sorbents

-------
            Sorbent + NaHCO3

         Burner        Downstream
     Sorbent + Cr2O3

Burner        Downstream
60
50

c
?40
!
330
s

-------
   80
   70
   60
   SO
 $ 40

 I
   30
   20
   JO
                                 I
                                  I.Ox 10'Btu/hr (290 kW)

                                  2200~230O°Ff120O-
                                  1260°C) Injection

                                 Q EER-PH* (Illinois Coal)

                                 £ EER-PH + Cr2Os (Indiana Coal)
                                      Ca/Cr = IS

                                  Boiler Simulator Furnace
                                             /'{Energy and Environmental
                                               Research Corporation
                                               Pressure Hydrate
Figure 4.
   1        2        3
      Ca/S (molar ratio)

Chromium-promoted, catcitic pressure hydrate.
   D. Slaughter, W. Thomson, T. Peterson, S. Chen, W. Seeker, and D. Pershing
    are with Energy and Environmental Research Corporation, Irvine, CA 92718-
    2798.
   David A. Kirchgessner is the EPA Project Officer (see below).
   The  complete report, entitled  "Influence  of Coal Mineral  Matter on  the
    Effectiveness of Dry Sorbent Injection for SO2 Control," (Order No. PB  88-
    178 587/AS; Cost: $25.95. 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:
           Air and Energy Engineering Research Laboratory
           U.S. Environmental Protection Agency
           Research Triangle Park, NC 27711
                                                                               . GOVERNMENT PRINTINGOfHCfe  1983/548-153/67094

-------
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
Official Business
Penalty for Private Use $300

EPA/600/S7-87/020
            0000329   PS

            IS  3 EJIVIR PROTECTION AGENCY
            REGION %  LIBRARY
            230 $  DEARBORN  STREET
            CHICAGO             IL   60604

-------