Desulfurization of Syngas in a
Transport Reactor
a a a b
Raghubir P. Gupta, Brian S. Turk, Jeffrey W. Portzer, and Daniel C. Cicero
a
Research Triangle Institute, P.O. Box 12194, Research Triangle Park, NC 27709-2194
b
U.S. Department of Energy, National Energy Technology Laboratory, Morgantown, WV 26507-0880
During gasification, sulfur present in carbonaceous
materials is converted into reduced sulfur species, such as
H S and COS. These sulfur species ar e conventionally
2
removed from syngas by catalytic hydrolysis of COS into H S, 2
followed by scrubbing of H S with liquid-phase amine sys-
2 power industry. Their advantages include high ther-
tems. Amine-based processes are subject to equipment corr o-
sion, foaming, amine-solution degradation, and evapora-
tion, and re q u i re extensive wastewater treatment. As a
result, this sulfur removal technology is complex, capital-
intensive, and expensive. Furthermore, this conventional
technology requires the syngas be cooled to nearly ambient
temperatures, thus wasting valuable energy.
New emerging technologies for sulfur removal from syn-
gas use regenerable sorbents, primarily based on ZnO.
Recent advances in sorbent technology allow sulfur species
to be removed from syngas over a wide temperature range
(260° to 760° C), making it an attractive alternative for a
wide variety of applications, including power generation,
chemical production, and fuel cells. This sorbent technology
has advanced to the point that syngas desulfurization can
be carried out in both fixed- and fluidized-bed re a c t o r s ,
depending upon process design needs. Additional applica-
tions of this technology in desulfurization of natural gas
and removal of sulfur species from a syngas generated from
gasification of black liquor were investigated.
INTRODUCTION
Syngas is a fundamental ingredient for producing
electric power, value-added chemicals (e.g., acetic
acid, formaldehyde), transportation fuels (e.g., Fischer
Tropsch [FT] diesel), hydrogen, fertilizers and other
gaseous and liquid hydrocarbons. Syngas is loosely
defined as a gas stream containing CO and H , but it 2 solution degradation and evaporation, and re q u i re
may contain other components, such as CO , H O, N , 2 2 2
C H , H S, and COS, depending upon the feedstock
4 2
source and method of generation. Most syngas is pro-
duced by natural gas reforming and by gasification of
Environmental Progress (Vol.20, No.3)
carbonaceous fuel, such as coal, petroleum coke, and
biomass. Integrated-gasification-combined cycle
(IGCC) systems, which utilize syngas produced from
gasification of carbonaceous feedstocks to generate
power in a gas turbine, are penetrating the electric
mal efficiency, environmental superiority over con-
ventional coal-fired, combustion-based power plants,
[1] and lower fuel costs, particularly, in light of recent
increases in natural gas prices.
However, syngas produced by gasification of car-
bonaceous feedstocks contain significant amounts of
reduced sulfur species—predominantly H S and COS;
2
minor amounts of CS and organic sulfur compounds
2
may also be present, depending upon the gasification
conditions. The amount of total sulfur in syngas pro-
duced from gasification can vary between 100 and
30,000 ppmv, depending upon the sulfur content of the
feedstock and design and operating conditions of the
gasifier (e.g., air-blown vs. O -blown, fixed-bed vs.
2
entrained-bed). Removing these sulfur species from
syngas is essential to minimize corrosion of downstream
equipment (such as gas turbines and fuel cell elec-
trodes) and poisoning of catalysts (e.g., FT catalyst), and
to meet SO emission requirements. The environmental
2
superiority of IGCC systems stem in part from their abil-
ity to effectively remove reduced sulfur species.
Currently, amine systems are the standard commer-
cial sulfur removal technology, but they are not trou-
ble free and have significant operating costs. They
operate in liquid phase at essentially ambient condi-
tions. This process means the syngas must be cooled
to nearly ambient temperatures, wasting valuable
energy. These amine-based processes are also subject
to process equipment corrosion, foaming, and amine-
extensive wastewater treatment. As a result, this sulfur
removal technology is complex, capital-intensive, and
operationally expensive. In addition, amine systems
cannot remove COS from the syngas, so a separate
October 2001 187
reactor vessel is needed to catalytically hydrolyze COS
into H S prior to absorption by the amine solution. To
2
alleviate some of the problems associated with amine
systems, research on new processes to remove sulfur
at high-temperature conditions was initiated.
Hot-gas desulfurization was originally conceived
for—and development was aimed at—maintaining the
syngas at an elevated temperature. The goal was to
achieve as high a cycle efficiency as possible in IGCC
power plants. Unfortunately, development of this hot-
gas desulfurization technology was not suff i c i e n t l y
advanced to be considered a viable technology for the
IGCC clean coal demonstration plants. As a result, the
commercial standard, amine-based “cold” gas desulfur-
ization technologies were used in these plants. Howev-
e r, several hot-gas, sorbent-based desulfurization
processes were included for slipstream testing at these
plants.
Additional developments and slipstream testing have
helped refine the economics of sorbent-based desulfur-
ization technology. It is now believed that a sorbent-
based process can be competitive with a conventional
amine-based process, on economics alone (indepen-
dent of the goal of overall cycle efficiency), when the
syngas is available at moderate to high temperatures.
These sorbent-based desulfurization processes use
a regenerable metal oxide (MeO), where Me is a suit-
able metal, and are carried out in a two-reactor system
consisting of a desulfurizer and a regenerator:
MeO + H2S = MeS + H2O
(Removal of H2S in a desulfurizer)
MeS + O2 = MeO + SO2
(Regeneration of sulfided sorbent in a regenerator)
The main criteria for a metal oxide in this process
are as follows: 1) it should selectively react with both
H S and COS at desired temperatures and pressures; 2)
2 granulation method to produce suitable sorbents for
t h e rmodynamics should be favorable to reduce the
sulfur level to a desired value; 3) it should be stable in
reducing and oxidizing conditions; and 4) it should be
easily regenerable under oxidizing conditions without
formation of undesirable side products, such as metal
sulfates.
In a recent review article, Cicero, et. al. [1] report
the development and commercial status of various
sorbents being developed worldwide. The vast major-
ity of the sulfur sorbents are ZnO-based because of
their favorable thermodynamics, good kinetics for
desulfurization and regeneration, and good stability
under reducing and oxidizing conditions. In addition
to the chemistry of desulfurization/regeneration reac-
tions, reactor design is critical due to the cyclic nature
of the process, necessitating a two-reactor system.
Reactor designs investigated, as reported by Cicero, et.
al., include fixed-bed, moving-bed, conventional flu-
idized-bed (bubbling bed) and fast fluidized-bed
(transport reactor) [1]. Currently, sorbent development
work is focused on two reactor designs: fixed-beds
and transport reactors. This paper presents the status
of technology development for transport reactors.
188 October 2001
FEATURES OF A TRANSPORT REACTOR SYSTEM
Transport reactors, which are essentially fast flu-
idized-bed reactors, offer several advantages over
fixed- or moving-bed reactors, including excellent
gas-solid contact, rapid kinetics, ability to handle par-
ticles in syngas, and ability to control temperature
during highly exothermic reactions. Additional advan-
tages of transport reactors include smaller sorbent
inventory because of higher gas velocities and short
residence time, and sorbents with low stoichiometric
sulfur capacity (unlike fixed-beds [2]). However, the
sorbent must be highly reactive and attrition-resistant
for a transport reactor to work successfully. Research
Triangle Institute (RTI) researchers have been devel-
oping sorbents for transport reactor applications for
the past 12 years. This work has focused on obtaining
the right combination of chemical activity and attrition
resistance. RTI researchers have made several break-
throughs, as demonstrated by the patents on various
aspects of this technology listed in Table 1.
Sierra Pacific Power Company’s (SPPCo’s) Piñon
Pine IGCC Clean Coal Technology Demonstration
plant, located in Reno, Nevada, uses a transport reac-
tor system for desulfurization of the syngas produced
in the fluidized-bed gasifier. This transport re a c t o r-
based desulfurization system was developed by Kel-
logg, Brown & Root, Inc. (KBR). In this system, both
desulfurization and regeneration are carried out in a
transport mode, with a provision for sorbent transfer
between the two reactors. It should be noted that this
transport desulfurization system is used as a polishing
bed to reduce the 400 to 600 ppmv of H S in the syn-
2
gas down to < 20 ppmv. The fluidized-bed gasifier
used at the Piñon Pine IGCC plant employs limestone
for in situ bulk sulfur capture [1].
SORBENT DEVELOPMENT FOR A TRANSPORT REACTOR
Originally, RTI re s e a rchers attempted to use a
transport reactors. This effort led to the develop-
ment of the ZT-4 sorbent that exhibited excellent
p e rf o rmance for bubbling fluidized-bed systems
(see Table 1, Item 1) [3]. However, attrition pro b-
lems occurred when tested under transport re a c t o r
conditions [4]. To correct the attrition problems, RTI
attempted developing spray-dried sorbent formula-
tions with CMP, Inc., and Intercat Development,
Inc., as discussed in Cicero , et. al. [1]. These
research efforts led to development of a zinc titanate
formulation, designated as EX-S03 by RTI and Inter-
cat [5]. As a prequalification requirement for testing
at the Piñon Pine plant, a 1,000 lb batch of this
material was produced in a commercial-scale spray
dryer to demonstrate scale-up of the manufacturing
process.
RTI successfully conducted bench-scale tests using
their high-temperature, high-pressure (HTHP) sorbent
test facility described by Gupta, et. al. [6] with the EX-
S03 sorbent (from the 1,000 lb batch) to determine its
long-term chemical reactivity and mechanical strength.
Following successful bench-scale tests at RTI, the EX-
S03 sorbent was tested at KBR’s transport reactor test
Environmental Progress (Vol.20, No.3)
Table 1. RTI patents in syngas desulfurization.

No. Patent No. Issue Date Title

1 US 5,254,516 10/19/93 Fluidizable zinc titanate materials with high chemical

reactivity and attrition resistance
2 US 5,366,717 11/22/94 Method for producing elemental sulfur from sulfur-
containing gases
3 US 5,714,431 02/03/98 Zinc titanate sorbents
4 US 5,798,088 08/25/98 Method for producing elemental sulfur from sulfur-
containing gases
5 US 5,914,288 06/22/99 Metal sulfide initiators for metal oxide sorbent
regeneration
6 US 5,928,980 07/27/99 Attrition-resistant catalysts and sorbents based on
a
heavy metal-poisoned FCC catalysts
7 US 5,972,835 10/26/99 Fluidizable particulate materials and methods of
making same
8 09/282, 608 Allowed Metal sulfide initiators for metal oxide sorbent
regeneration
9 60/075, 680 Pending (04/03/00) Attrition-resistant zinc titanate-containing reduced
sulfur sorbents
a
FCC = fluid catalytic cracking.
Table 2. Bench-scale test conditions simulating the Piñon Pine IGCC plant.

Condition Sulfidation Regeneration

Pressure (psig) 262 262
Temperature (° C) 538 538
Residence Time (s) 2.1 6.3
Gas Composition (vol %)
CO 25.0
CO 2
5.0
H 2
15.0
H S (ppmv)
2
1000
HO 2
5.0
N 2
50.0 79.0
O 2
21.0

unit (TRTU) to determine its suitability for use at the function of sulfur loading for this sorbent at a temper-
Piñon Pine plant. The TRTU at KBR is a pilot-plant pro- ature of 538° C. As can be seen, the sorbent met the
totype of a commercial transport reactor system for hot- H S leak as well as sulfur loading targets. Multicycle
2

gas desulfurization. The sorbent exhibited excellent
reactivity and attrition resistance characteristics. Cicero,
et. al. describe further details of these test results [1].
Based on these verification bench-scale and TRTU
testing results, SPPCo ordered a 50,000 lb batch of the
EX-S03 sorbent from Intercat. The sorbent was loaded
into the external desulfurizer at the Piñon Pine plant and
was successfully circulated under nitrogen at 150° C
without attrition problems. Currently, the sorbent is
loaded in the desulfurizer and is awaiting full evaluation
(including sulfur removal efficiency, regenerability, and
attrition under reaction conditions) upon startup of the
Piñon Pine IGCC plant. Integrated operation of the
Piñon Pine IGCC plant is planned for the future.
The sorbent was tested for its chemical reactivity
and regenerability in RTI’s HTHP bench-scale test
facility under test conditions simulating typical Piñon
Pine plant operating conditions. The actual test condi-
tions used during bench-scale testing at RTI are
shown in Table 2. Figure 1 shows a typical bre a k-
t h rough curve plotted with H S concentration as a
2
testing of this sorbent indicated continuous perf o r-
mance improvement over extending testing.
There was an additional challenge to using the EX-
SO3 sorbent at the Piñon Pine IGCC plant: because of
equipment design limitations, the neat air regenera-
tion had to be initiated at or below 538° C. RT I
researchers discovered and patented a suitable com-
position for a “light-off additive” (see Table 1, Items 5
and 8) [7]. After initial feasibility tests, RTI developed
this additive as a commercial material. Intercat pro-
duced a batch of this material, designated as LOA-1,
for the Piñon Pine plant. Figure 2 shows regeneration
t e m p e r a t u re profiles for the EX-S03 material mixed
with 5 wt % of the LOA-1 additive. Three of these
temperature profiles come from thermocouples locat-
ed within the sorbent bed at 2.54, 7.62, and 12.7 cm
(1, 3, and 5 in.) from the distributing frit at the gas
inlet. The temperature labeled “reac” in Figure 2 is
from a thermocouple located in the gas inlet stream
just below the distributing frit. This regeneration test
was conducted with neat air in a bubbling fluidized

Environmental Progress (Vol.20, No.3) October 2001 189

Figure 1. A typical breakthrough curve for the commercial sorbent supplied to SPPCo.

Figure 2. Regeneration temperature profiles for the commercial sorbent mixed with the LOA-1 in RTI’s HTHP
bench-scale unit.

190 October 2001 Environmental Progress (Vol.20, No.3)

Figure 3. Oxidation of coke breeze and sulfided sorbent in a TGA.
bed. As can be seen, sorbent regeneration was initiat-
ed at 427° C. The maximum temperature achieved
was about 760° C. These data clearly indicate that the
sorbent, with the help of the LOA-1 additive, should
easily regenerate at 538° C with neat air at the Piñon
Pine IGCC plant.
In addition to testing the sorbent for its sulfur
removal activity and regenerability, the effect of char
fines that may be present in syngas was investigated.
The syngas entering the transport reactor hot-gas desul-
furization system can potentially contain a significant
amount of char fines due to the poor efficiency of
cyclones, and process upsets during start-up. If oxygen
is selectively consumed by char over zinc sulfide in the
regenerator, it would lead to incomplete sorbent regen-
eration and would present serious temperature control
problems. A series of experiments were conducted in
RTI’s HTHP bench-scale reactor with the sorbent con-
taining 3 to 5 wt % coke breeze (a simulant for char
fines) to study the selectivity of the oxidation reaction in
the regenerator (carbon vs. zinc sulfide). During these
tests, sulfur burned preferentially over carbon. In fact,
oxidation of the carbon did not become significant until
almost all the sulfur was consumed. At this time, the
sorbent bed temperature was between 732° and 760° C.
These results were further confirmed by oxidation
experiments in a thermogravimetric analyzer (TGA) as
shown in Figure 3. In these experiments, samples of
coke breeze and sulfided sorbent were exposed to 2%
O in N at 538° C, and weight loss was recorded as a
2 2
function of time.
The attrition index (AI) of the EX-SO3 sorbent (sup-
plied to SPPCo) as defined in Cicero, et. al. [1] was 1.4
Environmental Progress (Vol.20, No.3)
compared to 4.0 for its previous version initially tested
in RTI’s bench-scale test facility. Note that as the AI
value drops, the material becomes harder, or more attri-
tion-resistant. The AI value of commercial fluid catalytic
cracking (FCC) catalysts is below 5, which is an industry
standard for all new products to be used in transport
reactors. This 1.4 AI value, measured at RTI using a
modified ASTM Test Method D-5757-95, was indepen-
dently confirmed by KBR.
In addition to testing this sorbent under simulated
conditions at RTI, it was also used at the U.S. Depart-
ment of Energy/National Energy Technology Labora-
tory (DOE/NETL) facilities in Morgantown, West Vir-
ginia, with real coal gas. Its performance was consis-
tent with that observed in previous testing, as
described in Gupta, et. al. [6]. The trace contaminants
present in real coal gas, particularly the heavy metals
and chlorides, did not affect sorbent perf o rm a n c e ,
and were not sequestered on the sorbent.
Desulfurization of Syngas Produced from Black Liquor
Gasification
Another important application for this sorbent tech-
nology is desulfurization of syngas produced fro m
gasification of black liquor produced by the paper
and pulp industry. RTI conducted a series of tests with
a simulated syngas re p resentative of a composition
from a gasifier fed with black liquor. The approximate
composition of this syngas was 49.7 vol % H O, 14.4
2
vol % CO , 5.1 vol % CO, 28 vol % H , and 28,000
2 2
ppmv H S. This test was run at 493° C in a fluidized-
2
bed mode. The sorbent was able to consistently
reduce the sulfur content of syngas from 28,000 ppmv
October 2001 191
Figure 4. Reactor effluent during a desulfurization test of syngas generated from black liquor.

Figure 5. Breakthrough profiles during several sulfidations of low-quality natural gas.

192 October 2001 Environmental Progress (Vol.20, No.3)

Figure 6. Temperature profiles during regeneration of low-quality natural gas.

to < 5 ppmv, as shown in Figure 4. The sulfur capacity
of the sorbent at breakthrough was approximately 7 wt
%. The sulfided sorbent was subsequently regenerated
using neat air (21 vol % O in N ) at 600° C. The sorbent
2 2
and achieved a sulfur loading of about 30 wt % sulfur.
The breakthrough profiles for these sulfidations appear
in Figure 5. At sulfidation temperatures of 427° C, the
reactor effluent concentration of COS, SO , and CS was
2 2

was then subjected to a second cycle of desulfurization ≥ 100 ppmv. These poor sulfidation results at 427° C
and regeneration testing to evaluate its cyclic perfor- prompted termination of this test.
mance. The desulfurization activity of the sorbent in the The only observed effect of oxygen content and
second cycle was similar to that observed in the first, as space velocity of the regeneration gas was the sorbent
well as what had been observed previously with the bed temperature. Increasing the oxygen content
Kellogg, Rust, and Westinghouse (KRW) syngas [6]. resulted in an increased sorbent bed temperature .
Effluent SO concentrations for both regenerations were
2 Because increasing the oxygen increases the exother-
between 12 and 14 vol %. This is approximately the sto- mic regeneration reaction kinetics, this would be
ichiometric amount produced during regeneration of expected. Increasing the space velocity, which forces
the sulfided sorbent, indicating minimal deactivation by more mass through the reactor and carries away the
side reactions. During both regenerations, the length of energy from the exothermic reaction, results in lower
the regeneration and amount of SO released were simi-
2 temperatures in the sorbent bed and better control of
lar, suggesting stable cyclic operation of the sorbent the temperature rise during regeneration. All these
between desulfurization and regeneration is possible. features can be seen in Figures 6 and 7. The tempera-
ture profiles in Figure 6 were collected with the same
Desulfurization of Low-Quality Natural Gas thermocouple placement described for Figure 2. An
Removal of sulfur (particularly H S and COS) from
2 important factor to observe in Figure 7 is that the
low-quality natural gas was investigated with one of changes in oxygen content and space velocity do not
the preliminary formulations that led to the develop- seem to affect the ability to regenerate the sorbent.
ment of the EX-S03 sorbent. For this test, low-quality Thus, sulfur removal from low-quality natural gas
natural gas was simulated with a mixture of 58 vol % should be possible with the EX-S03 sorbent at sulfida-
methane, 29 vol % N , 10 vol % CO and 3 vol % H S.
2 2 2 tion temperatures > 427° C and with a suff i c i e n t l y
The parameters varied during the test, including sulfi- high space velocity of neat air.
dation temperature, regeneration space velocity, and In addition to the ability of the zinc titanate sor-
oxygen content of the regeneration gas. At sulfidation bents (like EX-SO3) to remove H S from syngas, these
2

temperatures > 427° C, the sorbent reduced the sulfur sorbents were also tested for removal of COS fro m
content of the reactor effluent to less than 20 ppmv syngas. As mentioned previously, the commerc i a l

Environmental Progress (Vol.20, No.3) October 2001 193

Figure 7. Effluent concentration profiles during regeneration of low-quality natural gas.

amine systems used for sulfur removal are not very lated syngas mixtures, and bench-scale field testing
e ffective at removing COS. COS needs to be using actual coal gas at DOE/NETL’s facilities at Mor-
hydrolyzed in a separate reactor according to the fol- gantown, West Virginia, showed that a single, fixed-
lowing reaction: COS + H O = CO + H S. However,
2 2 2 bed catalytic reactor could achieve the high sulfur
with zinc titanate sorbents, it was confirmed that ZnO conversion rates desired [11, 12]. In a commerc i a l
in the sorbent reacts with the COS according to the embodiment of the DSRP, the tail gas would likely be
following reaction: ZnO + COS = ZnS + CO . The 2 recirculated to the syngas desulfurization reactor, thus
Gibbs free energy for this reaction at 300° C is -24.9 eliminating a potential emissions stream.
kcal/mol, indicating this reaction is thermodynamical- Development of the DSRP has expanded to handle
ly very favorable. Therefore, no separate COS removal the higher SO concentrations that will result fro m
2

system is required with these sorbents.
Treatment of Regeneration Tail Gas
The regeneration of sulfided sorbent produces a
gas stream containing SO in N that cannot be dis-
2 2
c h a rged. Various concepts have been proposed to
deal with this stream, such as production of sulfuric
acid or conversion to sulfate (gypsum). Conversion to
elemental sulfur appears to be a preferable alternative
because the sulfur thus obtained is a potential byprod-
uct with industrial value, or at least is in the lowest-
volume form, and is sufficiently inert so that it may be
readily disposed.
RTI researchers have developed and patented the
Direct Sulfur Recovery Process (DSRP) to catalytically
convert the SO in the regeneration off-gas to elemen-
2 High-temperature removal of reduced sulfur species
tal sulfur using a small slipstream of the syngas (see
Table 1, Items 2 and 4) [8, 9]. Initial development
work [10] in the early 1990s suggested that a two-step
process would be required to achieve high sulfur con-
version rates (98+%). Subsequent testing using simu-
neat air transport reactor sorbent regeneration [13]. A
skid-mounted, pilot-scale, fluidized-bed reactor DSRP
unit is currently in place at DOE’s Power System
Development Facility (PSDF) in Wilsonville, Alabama,
for long-term slipstream testing using actual coal gas.
Combining RTI’s sorbent and DSRP technologies
offers an attractive option for removing reduced sulfur
species from syngas to very low concentrations in a
wide range of temperature and pressure conditions.
These sulfur species can be eventually recovered as
high-purity elemental sulfur that can be safely stored
or used in variety of industrial applications.
CONCLUSIONS AND FUTURE TRENDS
from syngas produced by gasification of carbonaceous
feedstocks has progressed to initial demonstrations at
large-scale facilities. The definition of an IGCC facility is
changing to that of a multiple-product slate producer. It
is expected not only to provide electric power via com-

194 October 2001 Environmental Progress (Vol.20, No.3)

bustion turbines, but also be a syngas source for chemi-
cals or fuels production, to generate electric power by
way of fuel cell technology, and even be a source of
hydrogen for integration into hydrogenation processes in
refineries. Efforts are underway to develop next genera-
tion sulfur cleanup processes to bring sulfur levels down
to parts-per-billion (ppb) levels. With the incre a s e d
emphasis on control of greenhouse gas emissions, sepa-
ration and capture of CO has also become a priority. RTI
2 the 15th Annual International Pittsburgh Coal
and its project partners are working on a process consist-
ing of a polymer membrane and a ZnO-coated monolith
to remove CO and reduce sulfur levels of syngas to ppb
2 tors for Metal Oxide Sorbent Regeneration,” U.S.
levels. Details of this process are described in a recent
paper by Gupta, et. al. [14]. Fundamental properties of
the polymer membrane materials that permit this novel
separation are reported in Merkel, et. al. [15].
It has been projected that sorbent-based sulfur
removal at elevated temperatures (above the dew point
of syngas) can offer a significant cost advantage over
conventional amine-based systems. However, the long-
term performance and reliability of these high-tempera-
ture syngas desulfurization systems must be demonstrat-
ed before these systems can penetrate the IGCC market.
ACKNOWLEDGMENTS
The work reported in this paper has been done with
the sponsorship of DOE/NETL. The authors wish to
express appreciation for the contribution of Gunnar
Henningsen of KBR, Dr. Albert Vierheilig of Intercat,
and Suresh Jain of DOE/NETL. Assistance from Ti m
Merkel of RTI in preparing this paper is gratefully
acknowledged.
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