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Contents lists available at ScienceDirect

Process Safety and Environmental Protection

journal homepage: www.elsevier.com/locate/psep

An experimental study for H2 S and CO2 removal

via caustic scrubbing system

Ersin Üresin a,∗,1 , Halil İbrahim Saraç b , Alper Sarıoğlan a , Şiringül Ay a ,

Fehmi Akgün a
a TÜBİTAK Marmara Research Center Energy Institute, P.O. Box 21, 41470 Gebze, Kocaeli, Turkey
b Kocaeli University, Mechanical Engineering Department, Kocaeli, Turkey

a b s t r a c t

In this study, removal of hydrogen sulfide (H2 S) and carbon dioxide (CO2 ) from simulated syngas has been studied
on one column scrubbing system. Gas flow rate as a measure of gas residence time and superficial gas velocity, gas
composition, inlet H2 S load, flow modes (countercurrent and cocurrent) and packing geometry were the parameters
in the design and/or operation of an acid gas scrubber system. Better H2 S scrubbing efficiencies have been obtained
in countercurrent flow mode than that of cocurrent flow mode. When accordingly designed, static mixer with its
superior performance on H2 S removal overweighed to structured packings. The coexistence of CO2 and H2 S has been
shown to increase the sodium hydroxide (NaOH) consumption along the scrubber column thereby decreasing the
H2 S removal efficiency at higher H2 S loads. The gas residence time as changing with the gas velocity was found to
be more dominant on acid gas removal efficiency than the effect of superficial gas velocity within the experimented
range. A gas residence times of equal or above 3 s were seemed to be closer to the optimum point.
© 2014 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Keywords: Gas clean up; Packed bed gas scrubbers; Hydrogen sulfide removal; CO2 removal; NaOH; Static mixer

1. Introduction reaction rate of pollutant in the liquid. In physical scrub-

bing, the pollutants in basic nature can be passivated by
Particulate, ammonia (NH3 ) and hydrogen sulfide (H2 S) com- the acidic solutions and vica-versa. Currently, the processes
prise the main impurities of synthetic raw gas produced by of choice in the commercial integrated gasification com-
coal gasification. Removal of these contaminants is an essen- bined cycle (IGCC) facilities for the removal of acid gases are
tial step in coal and biomass gasification process to avoid its both the chemical solvent acid gas removal processes based
detrimental effects on materials and environment. Hydrogen on aqueous methyldiethanolamine (MDEA) and the physi-
sulfide and ammonia can cause corrosion in pipelines and cal solvent-based Selexol process which uses mixtures of
thus limit plant lifetime. These are also a well-known cata- dimethyl ethers and polyethylene glycol (Couvert et al., 2008;
lyst poisoner. Therefore, utilization of gasification products Turpin et al., 2008; Ohtsuka et al., 2009; Wang et al., 2004;
either as a fuel for gas turbines, gas engines or fuel cells or as Wallin and Olausson, 1993).
a syngas for Fischer–Tropsch fuel, ammonia or methanol pro- Alkaline hypochlorite, hydrogen peroxide or caustic solu-
ductions requires an effective gas clean-up technology (Chen tions are economicaly alternative solvents to be used in
et al., 2001; Moussavi et al., 2008; Panza and Belgiorno, 2010). physical solvent-based processes and show good results for
For the abatement of H2 S and NH3 , packed towers are decades. Sodium hydroxide solution is a very effective, but
widely used for chemical and physical scrubbing. The choice of non-regenerable absorbent for CO2 and H2 S. Therefore the use
the solution is critical in determining dissolution or chemical of caustic is usually limited to the removal of trace amounts of

∗
Corresponding author. Tel.: +90 262 677 27 80; fax: +90 262 641 23 09.
E-mail address: ersin.uresin@tubitak.gov.tr (E. Üresin).
1
Present address.
http://dx.doi.org/10.1016/j.psep.2014.06.013
0957-5820/© 2014 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

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these impurities. For the disposal of the spent caustic, differ- Ballaguet et al., 2003) there were only a sufficient number of
ent considerations are applied such as simple neutralization comparison studies differentiating the performances of both
or its use in pulp and paper mills after some certain qual- the static mixer and the structured packing for the acid gas
ity control analysis (Couvert et al., 2006; Miltner et al., 2012; removal. Static mixers have been known with their excellent
Mamrosh et al., 2008; Bontozoglou and Karabelas, 1991). gas–liquid contact due to a high turbulence rate inside and
For the improvement of scrubbing efficiencies, design of their potential on well mixed gas distribution giving high mass
the scrubber system is as important as the choice of the sol- transfer rates (Couvert et al., 2008; Sanchez et al., 2008). Con-
vent. Multiple gas sorption columns packed with structured sequently, the objective of this study is to design a static mixer
materials are used in order to increase the active surface area being able to generate high interfacial areas and improved
and residence time for an efficient gas–liquid interaction. High mass transfer rates for acid gas alkali washing towers and
efficiencies of commercial structured packing materials for compare the results with those of commercial packings. In
H2 S removal with an alkaline washing solution was attributed order to elucidate the advantages of static mixers over struc-
to a high contact area existing between the gas and the liquid tured packings, the removal of H2 S has been studied on one
phases. The major drawback in the use of structured packing column scrubbing system on both of the designed static mixer
is their excessive price per volume unit. Static mixers, if prop- and commercial structured packing. The effect of gas compo-
erly designed, can be acceptable in terms of investment costs sition has been investigated by using H2 S in nitrogen and H2 S
and have higher resistance to pluggings. Nevertheless, high in simulated refinery gas mixtures. For these two different gas
mass transfer performances cannot be reached by static mix- atmospheres, inlet H2 S concentration was increased in step-
ers as structured packing materials can be. Hence, the design wise. The gas flow rate as a measure of gas residence time was
of a static mixer has crucial importance in generating high changed to monitor the effect of superficial gas velocity and
interfacial areas and improving mass transfer rates (Couvert gas residence time. The scrubber has been operated in both
et al., 2008; Mamrosh et al., 2008; Godini and Mowla, 2008). countercurrent and cocurrent modes.
Basic design parameters of the structured packing columns
are hydrodynamic flow characteristics and packing surface
area as determined by the packing material geometry, res- 2. Materials and methods
idence time, liquid to gas ratio, pH and reactivity of the
solution. To avoid high investment and operation costs, the 2.1. Experimental apparatus
scrubber system should be designed by taking into consid-
eration of these parameters (Bhave et al., 2008; Biard et al., Fig. 1 illustrates the experimental set-up used in this study.
2010). The hydrogen sulfide (H2 S), carbon dioxide (CO2 ), methane
Although design studies and commercial applications on (CH4 ) and nitrogen (N2 ) inlet concentrations were adjusted by
structured packings were found in the literature extensively mass flow controllers (3) at the outlet of standard gas cylin-
(Miltner et al., 2012; Godini and Mowla, 2008; Bhave et al., 2008; ders respectively, and mixed with a manifold (4) for preparing
Aliabad and Mirzaei, 2009; Dang et al., 1998; Lu et al., 2006; simulated refinery gas mixtures before entering to scrubber

Fig. 1 – Scheme of the experimental set-up.

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column. There were two different scrubber columns (8) used

Table 1 – Main characteristics of the static mixer.
for the experiments in this study. The first one was equipped
Operating parameters Case 1
with packing materials. The internal and external diameters of
the packed column were 20.10 mm and 25.4 mm, respectively. Internal diameter (mm) 30
The column was constructed from 316 grade stainless steel Element thickness (mm) 0.5
and had a total height of 85 cm. The total packed bed height Total length of static mixer (mm) 290
Number of internal elements 33
and volume of column were 64 cm and 0.2 L, respectively. In
the second column static mixer was located. The second col-
umn was made of 316 grade stainless steel and had a inner
Table 2 – Geometric characteristics of packing material
diameter of 30.15 mm, a external diameter of 33.7 mm and a and static mixer used in the present study.
total height of 45 cm. The total static mixer height was 29 cm.
Packing material Static mixer
A 30 L tank (5) allowing to store the scrubbing liquid was
placed downstream the column. The liquid phase was dis- Internal diameter (mm) 20 30
persed by means of a spray nozzle located at the top of the both Packed bed height (mm) 640 290
Void fraction, ␧ 0.86 0.90
columns, whereas the gas phase was sparged at the bottom
of the column in countercurrent experiments. The concentra-
tion of NaOH in the scrubbing solution was controlled by a pH
are attached to the opposite sides of the static mixer wall in
meter (6). The flowmeter (2) used for measuring liquid flow
step-wise manner (Fig. 2). Table 1 lists the main characteristics
rates was made from stainless steel to reduce the corrosion
of the static mixer.
problem. The spent scrubber liquid-gas mixture was stored in
The liquid stream passes into the throat sections of the
a waste tank (10) and drained by a valve which was mounted
static mixer, where the high gas velocity and the associated
at the bottom of the tank. A water trap (11) was placed in the
low pressure region causes atomization of the liquid into small
column outlet to remove entrained liquid droplets from the
droplets to occur. Also, when liquid is introduced at the throat
gas stream.
the high turbulence zone is created. Small droplets formed
by atomization join together by hydrostatic force to form
2.2. Experimental procedure droplets cloud which would move as a single system and have
a much larger effective diameter. So, these atomized liquid
The experiments were carried out at 20 ◦ C. H2 S, CO2 , CH4 and droplets improve the gas–liquid interaction and increase the
N2 gases were injected from gas cylinders and the volumetric surface area tremendously which allows enhanced absorption
mixed gas flow rate QG , controlled with mass flow controllers, of desired components of interest. Nevertheless, the contact
ranged from 0.18 to 0.30 m3 /h. Packing material and static surface area increase gradually at the upper and the lowest
mixer have a diameter of 20 mm and 30 mm respectively. region of the static mixer due to its designed shape. The geo-
In the experiments, commercial metal sheet structured metric characteristics of the commercial packing and static
pack was used to generate a packing bed in the column. This mixer used are shown comparatively in Table 2.
kind of commercial structured pack has been manufactured The scrubbing liquid solution was stored fed to the column
with series of channels. The channels are consist of corrugated by spraying the solution with the nozzle at a constant rate
stainless steel sheets which are parallel with each other and of 2.5 L/h. During the experiments the pH value of the liquid
located vertically. Corrugated sheets are arranged in a criss- solution was measured continuously and the caustic (NaOH
crossing relationship to create flow channels for the vapor aqueous solution) was added if it is necessary for adjusting
shape. The intersections of the corrugated sheets create mix- the pH as 11. The operating parameters are shown in Table 3.
ing points for the liquid and vapor phases. Designed each By-pass line valves were mounted to appropriate locations
static mixer was used in the experiments have slightly ven- on the systems and the scrubber was operated in countercur-
turi shape, an internal diameter of 30 mm, length of 96.5 mm rent and cocurrent modes. At the first stage of experiments,
and 11 mixing baffles. The baffles were located equidistant direction was countercurrent with mixed gas entering from
from each other in the vertical direction and consecutive ones the bottom of the column and flowing upward through the
column. Cocurrent direction was studied in the second stage
of experiments where mixed gas enters from the top of the
packed bed as with the same direction of the sprayed liquid.
Dry outlet gas stream is fed to a gas chromatography. Gas
analysis system consists of two gas chromatographs. Sulfide
containing gases are analyzed with a gas chromatography
instrument equipped with a flame photometric (FPD) and a
pulsed flame photometric detector (PFPD). Permanent gases
Fig. 2 – Schematic representation of the static mixer. (H2 , CO, CO2 , CH4 , N2 ) are detected by a gas chromatography

Table 3 – Operating parameters of the system for each experiment.

Operating parameters Case 1 Case 2 Case 3
3
Gas flow rate (m /h) 0.18 0.24 0.30
Liquid flow rate (L/h) 2.50 2.50 2.50
Liquid/gas ratio (L/m3 ) 8.30 10.40 13.80
NaOH concentration (g/L) 0.25 0.25 0.25
Operating temperature (K) 293 293 293
Operating absolute pressure (Pa) ≈105 Pa ≈105 Pa ≈105 Pa

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with two thermal conductivity detectors (TCD). The outlet gas 100

was sent to both of these two instruments and so H2 S, CO2 ,

CH4 and N2 concentrations were measured simultaneously.

H2S removal efficiency, %

80

3. Results and discussion

60

Absorption experiments have been realized in two different

gas compositions. The first set of experiments, the simulated
40
gas composed of H2 S in balance nitrogen was used. The level of
H2 S has been adjusted by using a secondary nitrogen diluent
gas. Thereby, four different inlet conditions for H2 S concen- 20
tration in nitrogen have been adjusted as namely 250 ppmv,
500 ppmv, 750 ppmv and 1000 ppmv in balance nitrogen. In
0
the second set of experiments, the effect of CO2 , which is in 200 400 600 800 1000
competition with H2 S to react with NaOH, was investigated. Inlet H2S concentration, ppmv

To do this, a simulated gas composed of 25% CO2 , 25% CH4 countercurrent; mixture countercurrent; N2 cocurrent; mixt ure cocurrent; N2
and balance nitrogen was prepared. A separate H2 S in balance
Fig. 3 – H2 S removal efficiency (%) in N2 atmosphere and
nitrogen stream was used to adjust H2 S levels to 250 ppmv,
CO2 , CH4 and N2 mixture in cocurrent and countercurrent
500 ppmv, 750 ppmv and 1000 ppmv, respectively. Each of the
modes on commercial packing.
reactant gas streams were scrubbed with a caustic solution,
prepared by NaOH. At every set of experiments, pH of the
caustic solution was maintained as 11. Countercurrent and in the pH all along the reactor, possibly due to the presence of
cocurrent modes of operation were tested as well. CO2 in excess concentration.
In the scrubbing processes, sodium hyroxide (NaOH) is The superficial gas velocity and residence time play impor-
known commercially as caustic solution and NaOH reacts tant roles in scrubbing processes. To determine the effects
with H2 S dissolved in aqueous solution. Hydrogen sulfide and of superficial gas velocity and residence time, three variable
caustic reaction is in the water phase, thus hydrogen sul- flow rates (0.18, 0.24, 0.30 m3 /h) were used for both packed
fide is diffused from organic phase to the interface and then bed column and static mixer column during our experiments.
entered to the water phase. Sodium sulfide (Na2 S) and sodium As the gas flow rate increases, the superficial gas velocity
hydrosulfide (NaHS) are reaction products of the reaction as increases through the column which has a constant diame-
specified by the Eqs. (1) and (2). Sodium sulfide has partial mis- ter. By the way, with the increase in the superficial gas velocity,
cibility in water. To maintain removal quality, controlling the the residence time decreased. So, three variable superficial gas
pH of the spent NaOH solution is required otherwise NaHS can velocity and residence time values were obtained for each two
occur as predominant sulfide species. So, if caustic is added, columns of different diameters. These also provided to com-
H2 S is removed, and if the pH of NaOH decreases, it becomes pare performances of static mixer column and packed column
acidic and H2 S is produced. The following equations describe in terms of superficial gas velocity.
the reaction mechanism of H2 S and caustic solution: In order to investigate the influence of gas residence time
on the H2 S removal, the gas residence times were changed
in between 2.4 s and 4 s. In the experimented range, it was
NaOH + H2 S → NaHS + H2 O (1)
shown in Fig. 4 that the H2 S removal efficiency decreased
with decreasing the gas residence times. This is reasonable
2NaOH + H2 S → Na2 S + 2H2 O (2)
since one would expect a decrease in H2 S removal effi-
ciency by limiting the contact time. On the other hand, as
Also, the assessment of system efficiency had to take into claimed by Turpin et al. the degree of H2 S removal might
account NaOH parasitical consumption due to carbon dioxide be increased with the gas velocity, since an increase in the
(CO2 ) absorption. Carbon dioxide in gas streams complicates superficial gas velocity would bring an increase in the vol-
using NaOH solution for H2 S scrubbing, because CO2 is readily umetric mass transfer coefficient. According to them, when
scrubbed into NaOH solution as well (Eq. (3)). Consequently, the superficial gas velocity increases, the gas prevents the
the presence of CO2 concentration increases the consumption droplets from falling inside the column and the droplets
of NaOH solution, thus decreases the H2 S removal. residence time in the column increases. So, the exchange
area available for the mass transfer gets bigger. It may
2NaOH + CO2 → Na2 CO3 + H2 O (3) be proposed here that the residence time in the column
might be more effective on the H2 S removal efficiency than
The results of caustic scrubbing have been seen in Fig. 3. It is the effect of volumetric mass transfer coefficient in the
apparent that near 100 percent of H2 S capture was succeeded experimented range. In other words, all superficial gas veloc-
in the case of nitrogen atmosphere, whatever of the inlet H2 S ities in the experiments were high enough providing less
level was and without depending on the flow mode. On the variations of the mass transfer coefficients (Turpin et al.,
other hand, the level of H2 S removal affected in a negative 2008).
way when a competitive acid gas presented for both of the flow To investigate the effect of the geometry of structured pack-
modes. In spite of the better H2 S scrubbing efficiencies have ing material, a static mixer has been designed, manufactured
been obtained in countercurrent flow mode, the efficiency val- and used in the experiments. The properties of commercial
ues were decreased with increasing the inlet H2 S levels. The structured packing and in house static mixer have been given
decrease in H2 S removal efficiencies with increasing the inlet in Table 1. The diameter of the static mixer and the commer-
H2 S concentration can be explained by an important decrease cial packing were 30 mm and 20 mm, respectively. To maintain

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100

90 CO2 removal at
H2S 250 ppmv inlet H2S

80 CO2 removal at

H2S-CO2 removal efficiencies, %

500 ppmv inlet H2S
CO2 removal at
70
750 ppmv inlet H2S
CO2 removal at
60
1000 ppmv inlet H2S
H2S removal at
50
250 ppmv inlet H2S
H2S removal at
40 500 ppmv inlet H2S
H2S removal at
30 750 ppmv inlet H2S
H2S removal at
CO2
20 1000 ppmv inlet H2S

10

0
2.5 3 3.5 4 4.5

Gas residence time, sec

Fig. 4 – H2 S removal efficiency (%) in CO2 , CH4 and N2 mixture with countercurrent modes on commercial packing.

the same volume of the packing column, the height of the the band between the H2 S removal efficiency plots were
static mixer has been adjusted accordingly. Hence, while the broadened showing remarkable performance improvements
superficial gas velocities were changed for each point of exper- with the static mixer. Relatively stable H2 S removal per-
iment, the gas residence times were constant for the same formances were obtained with the static mixer for all the
experimental conditions of two different absorber units (com- experimented gas residence times.
mercial packing materials and static mixer) geometries. To investigate the origin of the H2 S removal performances
As seen in Fig. 5, better H2 S removal efficiencies have been with the use of static mixer, the results were re-evaluated
obtained with the static mixer than the commercial struc- according to the changes with superficial gas velocities (Fig. 7).
tured packing. Although the H2 S removal efficiencies were High cross-sectional area of static mixer located column pre-
affected more at lower gas residence time of ∼2 s for commer- sented lower superficial gas velocities when the volume of the
cial structured packing, no remarkable change was observed packing column and the gas flow rate were kept constant for
with the static mixer (Fig. 5). At every experimented gas resi- each of the absorber units for every gas residence time points.
dence time, the quite stable results have been obtained with Hence while the gas residence time was changing, the super-
the use of static mixer. Solely, at the lowest inlet H2 S concen- ficial gas velocities also changed. As seen in Fig. 7, the H2 S
tration of 250 ppmv and high residence times of 3 and 4 s, the removal performances were changed with the superficial gas
H2 S removal performances of both packings were merged. velocities as well. The less the superficial gas velocity was,
Fig. 6 shows the results for the higher inlet H2 S loads the more the H2 S removal performance was meaning that
of 500, 750 and 1000 ppmv. At the higher inlet H2 S loads,

100
100

90 90
H2S removal efficiency, %

H2S removal efficiency, %

80 80

70
70
500 ppmv;
commercial packing
60 750 ppmv;
60 commercial packing
1000 ppmv;
commercial packing
50 500 ppmv;
static mixer
250 ppmv 50
750 ppmv;
static mixer
40 1000 ppmv;
2 2.5 3 3.5 4 static mixer
40
Gas residence time, sec 2.5 3 3.5 4
static mixer commercial pack ing Gas residence time, sec

Fig. 5 – H2 S removal efficiency (%) in CO2 , CH4 and N2 Fig. 6 – H2 S removal efficiency (%) in CO2 , CH4 and N2
mixture with countercurrent modes on commercial packing mixture with countercurrent modes on commercial packing
and static mixer at 250 ppmv inlet H2 S. and static mixer at 500, 750 and 1000 ppmv inlet H2 S.

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100 100

90 CO2 removal at
90 250 ppmv inlet H2S
80
CO2 removal at

H2S-CO2 removal efficiencies, %

H2S removal efficiency, %

500 ppmv inlet H2S

70
80 CO2 removal at
750 ppmv inlet H2S
60
CO2 removal at
70 1000 ppmv inlet H2S
50
H2S removal at
40 250 ppmv inlet H2S
60 H2S removal at
30 500 ppmv inlet H2S
H2S removal at
50 20 750 ppmv inlet H2S
static mixer commercial packing H2S removal at
10
1000 ppmv inlet H2S
40
0 0.05 0.1 0.15 0.2 0.25 0.3 0
2.5 3 3.5 4 4.5
Superficial gas velocity, m/sec Gas residence time, sec
250 ppmv 500 ppmv 750 ppmv 1000 ppmv

Fig. 9 – H2 S removal efficiency (%) in CO2 , CH4 and N2

Fig. 7 – H2 S removal efficiency (%) versus superficial gas mixture with countercurrent modes on static mixer.
velocity (m/s) in CO2 , CH4 and N2 mixture with
countercurrent modes on commercial packing and static
mixer.
4. Conclusions
40
The key parameters to design a packed bed scrubber unit were
35 the gas residence time, superficial gas velocity, flow mode and
packing geometry. The better H2 S scrubbing efficiencies have
30 been obtained in the countercurrent flow mode. It was shown
CO2 removal efficiency, %

that the lower the superficial gas velocity was, the higher
25
the removal efficiency for both acid gases, namely H2 S and
CO2 . The effect of superficial gas velocities was interpreted
20
that the gas residence time as changing with the gas veloc-
15 ity was more effective on acid gas removal efficiency than
its effect on liquid droplets residence time within the exper-
10 imented range. On the other hand, although both of the acid
gas removal efficiencies were decreased with decreasing the
5
static mixer comm ercial packing gas residence time, the degree of decrease for CO2 , due to its
relatively weak reactivity with NaOH, was more noticeable in
0
0 0.05 0.1 0.15 0.2 0.25 0.3 relation to H2 S. Coexistence of CO2 and H2 S has been shown
Superficial gas velocity, m/sec to affect the design of the scrubber. The presence of CO2 leads
at 250 ppmv inlet H2S at 500 ppmv inlet H2S at 750 ppmv inlet H2S at 1000 ppmv inlet H2S to increase in NaOH consumption along the scrubber column
thereby decreasing the H2 S removal efficiency. This effect was
Fig. 8 – CO2 removal efficiency (%) versus superficial gas more remarkable at higher H2 S loads. In order to find the
velocity (m/s) in CO2 , CH4 and N2 mixture with best design values, gas residence time should be optimized
countercurrent modes on commercial packing and static regarding the lowest CO2 removal at the highest H2 S removal.
mixer at 250, 500, 750 and 1000 ppmv inlet H2 S. The results showed that a gas residence time of 3 s and more
seemed to be close to the optimum point. The static mixer
might be preferable over the structured packings not only due
the superficial gas velocity is a very important parameter in
to its cost effective nature and resistance to plugging but also
determining the overall scrubbing performance.
its superior performance in H2 S removal when accordingly
The same effect was also examined for the CO2 removal via
designed.
caustic scrubbing. Fig. 8 presents the results of CO2 removal
efficiencies with the superficial gas velocities. A change in the
CO2 removal efficiency with the superficial gas velocity was Acknowledgement
observed individually for each of the packing geometry. For
each of the packed material, the CO2 removal efficiencies were We greatly acknowledge The Scientific and Technological
increased with the superficial gas velocity. This might mean Research Council of Turkey (TÜBİTAK) for supporting of “Fuel
that the CO2 removal efficiency was seen to depend on the Production from Biomass and Coal Blends” project (Contract
packing material geometry as well, besides its dependency code: 108G043) in which this study was carried out.
on the superficial gas velocity. Fig. 9 gives the change of H2 S
and CO2 removal efficiencies with the gas residence time for References
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Please cite this article in press as: Üresin, E., et al., An experimental study for H2 S and CO2 removal via caustic scrubbing system. Process Safety
and Environmental Protection (2014), http://dx.doi.org/10.1016/j.psep.2014.06.013