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Figure I , to avoid clutter, is provision for cooling both reactor/crystallizers with cooling
water so that the solvent is sub-saturated in sulfur a t all other points in t h e system.)
T h e underflow f r o m the SO2-rich reactor carries the sulfur a n d water formed in t h e
r e a c t i o n b e t w e e n H2S a n d S 0 2 . T h e f l o w of t h i s s t r e a m is sized t o k e e p t h e water
content of the solvent f r o m exceeding 5% and is directly proportional to the rate of H2S
removal - - the flow will typically be about 10% of the total flow of solvent through the
p r i m a r y absorber. S u f f i c i e n t H2S-rich solvent, from the primary absorber, is added to
the stream to leave a small excess of H2S a f t e r all of the residual SO2 has reacted. This
stream is then flashed to atmospheric pressure in the settler/surge tank,
T h e sulfur made in t h e process forms a slurry i n the underflow from the surge tank.
The sulfur is recovered a n d washed in a centrifuge. In most cases about one-third of the
s u l f u r will be burned in the furnace to make the SO2 needed i n the process. T h e energy
recovered i n t h e waste-heat boiler will usually supply a n d perhaps exceed t h e energy
required by the process.
T h e overflow streams from the surge tank a n d the centrifuge a r e combined a n d sent
to t h e solvent stripper. Boiling most of the water out of the solvent provides a stripping
vapor t h a t also removes unreacted H2S a n d co-absorbed gases such a s C 0 2 f r o m the
solvent. Most of t h e solvent leaving the solvent stripper is used in t h e SO2 scrubber
where i t absorbs the SO2 from the combustion gas leaving the furnace. T h e SO2 content
of this solvent is nil, a n d hence the SO2 content of the stack gas leaving the scrubber can
readily be reduced t o t h e part-per-million level. The remainder of the solvent from the
stripper is sent to the primary absorber, where i t prevents loss of SO2 in the treated gas.
Figure 2 shows a process configuration suitable f o r removing a n d recovering one or
more components (in a d d i t i o n to the H2S) from t h e gas being treated, such a s removing
C 0 2 from a synthesis gas ahead of a s h i f t reactor in a process f o r producing hydrogen.
T h e operation of this process is identical to t h a t described above in many respects. It
differs as follows:
At the bottom of t h e primary absorber is a short section in which much of the H2
and CO are stripped f r o m the solvent. T h e stripping gas is obtained by a partial flash of
t h e solvent i m m e d i a t e l y downstream of t h e p r i m a r y absorber. Most of t h e H2S-rich
solvent stream leaving t h e flash drum, together with a controlled flow of SO2 solution,
e n t e r s a n S 0 2 - r i c h reactor. T h e pressure of t h e SO2-rich solvent stream is reduced in
stages (only t w o a r e s h o w n ) to a b o u t one atmosphere. T h e o f f - g a s f r o m each stage is
recompressed t o the pressure desired f o r the C 0 2 product a n d i s contacted w i t h neat
solvent to remove traces of S 0 2 , then washed with water to recover solvent vapor. For
the case shown, in w h i c h a high degree of C 0 2 removal is not required, clarified H2Sf r e e solvent f r o m t h e atmospheric f l a s h can be pumped d i r e c t l y back to t h e primary
absorber.
301
'
~~
Table 1:
Metal
Carbon Steel
304 Stainless
316 Stainless
SOz:
@ 100C
@ 12OoC
0.6
1.7
1.5
4.8
0.7
1.3
H2S: @ 15OoC
0.05
0.02
0.01
302
The crystallizer consists of a well-stirred 2-liter vessel. Hot saturated feed enters at
the top, and the vessel walls a r e cooled. Cold effluent exits a t the bottom of the vessel as
a sulfur/solvent slurry. A sample of the effluent slurry i s collected when the system is
at steady-state and t h e size distribution of the sulfur crystals is determined. analysis.
G a s Absorption with Chemical Reaction
Tray efficiency d a t a a r e needed f o r two process situations. In one, H2S a t very low
concentration is being absorbed by a chemically reactive solution of S 0 2 . In t h e other,
gaseous SO2 i n the low parts-per-million concentration range is absorbed by lean process
solvent. Both a r e of interest because one wishes to e f f e c t very stringent sulfur removal
with the UCBSRP. T h e equipment consists of a single seive tray (or section of packed
column) placed in a test section through which gas a n d liquid streams pass. Murphree
t r a y efficiencies a r e determined from the mass balances and previously obtained solubili t y data.
Work Required for Proof-of-Concept
The crystallizer is being modified to incorporate crystal size classification to retain
smaller c r y s t a l s a n d p r o d u c e a p r o d u c t of l a r g e r size. S u l f u r will be produced by
chemical reaction. Data obtained for absorption of H2S enhanced by the presence of SO2
in t h e solvent will b e used to develop a model t h a t incorporates the reaction kinetics
work done previously.
A c o m p u t e r model t h a t s i m u l a t e s a l l of t h e u n i t o p e r a t i o n s i n t h e process is
operational and facillitates process synthesis f o r specific applications. It will be used to
evaluate a n d f u r t h e r refine the process configurations shown in Figures I and 2 for the
purification of hydrogen derived from gasified coal.
Acknowledgement
This work was supported by the Assistant Secretary for Fossil Energy, Office of Coal
Utilization, Division of S u r f a c e Coal Gasification, of the US. Department of Energy
under contract DE-AC03-76SF00098.
303
References
Demyanovich, R.J. a n d Lynn, S. 1987. Vapor-Liquid E q u i l i b r i a of S u l f u r Dioxide in
Polar Organic Solvents. I&EC Research 26 548.
Lynn,
s., Neumann,
304
TREITED GAS
Pigure 2
Co-Absorption Process.
305