Fuel 82 (2003) 2153–2159

www.fuelfirst.com

Reduction of CO2 emissions by a membrane contacting processq

M. Mavroudi, S.P. Kaldis, G.P. Sakellaropoulos*
Chemical Process Engineering Research Institute, Aristotle University of Thessaloniki, P.O. Box 1520, Thessaloniki 54006, Greece
Received 6 November 2002; revised 30 April 2003; accepted 8 May 2003; available online 12 June 2003

Abstract
A membrane-based gas– liquid contacting process was evaluated in this work for CO2 removal from flue gases. The absorption of CO2
from a CO2 – N2 mixture was investigated using a commercial hollow fiber membrane contactor and water or diethanolamine as absorbing
solvents. Significant CO2 removal (up to 75%) was achieved even with the use of pure water as absorbent. By using aqueous amine solutions
and chemical absorption, mass transfer improved, and CO2 removal was nearly complete (, 99%). A mathematical model was developed to
simulate the process and it was validated with experimental data. Results show that membrane contactors are significantly more efficient and
compact than conventional absorption towers for acid gas removal.
q 2003 Elsevier Ltd. All rights reserved.
Keywords: Membrane contactor; CO2 removal; Modeling

1. Introduction by combining conventional techniques. In a membrane

Although carbon dioxide is only one of the many
greenhouse gases and certainly a non-toxic one, it
contributes significantly to the greenhouse effect by
anthropogenic sources [1]. Without major policy or
technology changes, future concentrations of CO2 will
continue to increase, mainly as a result of fossil fuel uses in
transport, heating and power generation [2]. Given this high
degree of dependence on fossil fuels and the difficulties in
their large scale replacement by alternative options, such as
nuclear and renewables, it is important to devise techniques
which would reduce greenhouse gas emissions arising from
the use of fossil fuels. Conventional capture technologies
based on a variety of physical and chemical processes
including absorption, adsorption, cryogenics and mem-
branes, involve problems that adversely affect the energy
efficiency and the economics of power stations [3 – 5].
Efficient and flexible technologies, capable to remove
greenhouse gases are needed, operating over a wide range of
concentration levels and a wide range of volumetric flow
rates. To meet these needs hybrid processes are introduced
* Corresponding author. Tel.: þ 30-2310-996271; fax: þ 30-2310-
996168.
E-mail address: sakel@vergina.eng.auth.gr (G.P. Sakellaropoulos).
q
Published first on the web via Fuelfirst.com—http://www.fuelfirst.com
0016-2361/03/$ - see front matter q 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/S0016-2361(03)00154-6
contactor, separation of a pollutant through the membrane is
completely integrated with the absorption operation in order
to exploit the benefits of both technologies. The membrane
offers a flexible, modular, energy efficient device with a
high specific surface area. The absorption process can offer
a high selectivity and a high driving force for transport even
at low concentrations. The membrane-based gas absorption
technique operates efficiently and it can be adapted easily to
the specific demands of an individual plant.
These advantages paved the way for the application of
membrane contacting technology in the recovery/removal
of acid gases from flue gases, natural gas and various
industrial process gas streams as reviewed by Ho and Sirkar
[6] and Gabelman and Hwang [7]. Membrane-based
absorption may be applied to most systems treated by
conventional gas absorption technology.
The absorption of a variety of gases in an acidic or
alkaline medium using a membrane hollow fiber module
was studied initially by Cussler and his coworkers [8 – 10].
Since then, several investigators have studied membrane-
based absorption of acid gases [11 – 19], mostly in lab-made
and bench scale membrane contactors. The TNO Institute
research group [20,21] worked on a larger scale, using a
patented membrane module. A membrane gas absorption
pilot plant with a capacity of 100 N m3/h was also built and
it was tested for two six-month seasons. Over 95% SO2
2154 M. Mavroudi et al. / Fuel 82 (2003) 2153–2159

recovery was obtained and no problems with dust, particle

condensation, or other flue gas components (e.g. NOx, CO2,
HCl) were encountered.
In the present work the performance of a commercially
available membrane contactor is assessed for carbon
dioxide removal from a power plant flue gas. The
commercial Liqui-Cel Extra Flow membrane module
(Hoechst Celanese Corp., Charlotte, NC, USA) was used
to obtain reliable data and to predict separation performance
for process scale-up. Absorption experiments were carried Fig. 1. Mass transfer regions and dominant resistances in a membrane
out using a simulated typical power plant flue gas as feed contactor.
gas, and water or aqueous diethanolamine (DEA) solutions,
as absorbents. The influence of tube side and shell side
dynamics were studied and a mathematical model was used a resistance-in-series model
to predict mass transfer coefficients. Experimental results 1 Hi Hi 1
were compared with those of conventional technologies and ¼ þ þ ð1Þ
Koverall ki;gas ki;membrane Eki;liquid
discussed in terms of future developments of the membrane
contacting process for acid gas capture. where ki;gas is the gas side mass transfer coefficient (cm/s),
ki;membrane is the membrane mass transfer coefficient (cm/s),
1.1. Theory ki;liquid is the liquid phase mass transfer coefficient (cm/s), Hi
is the dimensionless Henry’s constant, and E is an
Membrane gas absorption is based on a gas – liquid enhancement factor due to the chemical reaction.
contact across a hydrophobic microporous membrane. The overall liquid phase mass transfer coefficient,
This membrane forms a permeable barrier between the Koverall ; is calculated by Eq. (2):
liquid and the gas phase, which permits mass transfer Ql cout
il
between the two phases without dispersing one phase Koverall ¼ ð2Þ
Am ðDCÞlm
into the other. The gas preferentially fills the hydro-
phobic membrane pores and meets the liquid at the where Ql is the liquid flow rate (cm3/s), cout
il is the liquid
opposite side of the membrane. The liquid phase pressure phase outlet concentration of CO2 (mol/cm3) and ðDCÞlm is
should be slightly higher than that of the gas phase to the logarithmic mean driving force based on liquid phase
prevent dispersion of gas bubbles into the liquid. As long concentrations:
as the excess aqueous solution pressure is less than the ðcinp out outp
il "2 cil Þ 2 ðcil# Þ
breakthrough pressure of the membrane [22] the solution ðDCÞlm ¼ ð3Þ
does not penetrate the pores and the gas/liquid interface ðcinp out
il 2 cil Þ
ln outp
is immobilized at the pore mouth of the membrane on cil
the solution side.
The cinp outp
il and cil are hypothetical liquid phase concen-
Operation of gas – liquid membrane contactors differs
trations in equilibrium with the corresponding gas phase
from that of other membrane processes, such as filtration,
CO2 concentrations, cig ; expressed by Henry’s law as:
since there is no convective flow through the pores, but only
diffusive transport of certain components. This is the main
cpil ¼ Hi cig ð4Þ
reason that membrane contactors are less sensitive to
fouling than conventional membranes. As the membrane
is non-selective, the chemistry of the separation is the same 2. Model development
as for conventional equipment. The choice of a suitable
combination of absorption liquid, membrane characteristics A mathematical model was developed using the
and operation mode determines the selectivity of the resistance-in-series concept, combining process conditions,
process. membrane properties and module geometric characteristics.
Mass transfer is determined by the consecutive steps in the The following assumptions are made: (a) single component
three phases shown schematically in Fig. 1, i.e. diffusion of (CO2) absorption from a CO2 –N2 gas mixture flowing
gaseous component i from the bulk gas to the membrane wall, through the fiber lumen into an aqueous solution flowing in
diffusion through the pores of the membrane to the the shell side, as described schematically in Fig. 2; (b)
membrane – liquid interface, and dissolution into the liquid steady state and isothermal operation; (c) Newtonian fluids
absorbent, followed by liquid phase diffusion/chemical with constant physical properties; (d) fully developed
reaction. Hence, the overall liquid phase mass laminar flow in the lumen; (e) negligible radial convection
transfer resistance, 1=Koverall (s/cm), can be expressed by and axial diffusion; and (f) applicability of Henry’s law.
 M. Mavroudi et al. / Fuel 82 (2003) 2153–2159 2155

Fig. 2. Flow configuration through a typical hollow fiber.

With these assumptions, the CO2 concentration profile in is considered, the effective mass transfer coefficient is
the lumen can be estimated from the differential mass balance reduced by a factor, which denotes the fraction of the pores
   wetted by the liquid phase, x; according to:
›Cig 1 › ›Cig
uz ¼ Dig r ð5Þ 1 ð1 2 xÞtlm xtlm
›z r ›r ›r ¼ þ ð11Þ
ki;membrane Dig 1 Dil 1
where Dig is the diffusion coefficient in the lumen fluid
(cm2/s), considered here independent of concentration and In pure water, absorption of CO2 is accompanied by the
derived from Chapman –Enskog theory [23], and uz the gas following reaction:
velocity inside the lumen (cm/s). This velocity profile is þ
given by CO2 þ 2H2 O $ HCO2
3 þ H3 O
"  2 # Because the value of equilibrium constant of the reaction is
r
uz ¼ u 1 2 ð6Þ very small, the formation of bicarbonate is very small [12].
ri
Therefore, CO2 is absorbed physically.
where u is the maximum velocity inside the fiber lumen (cm/ For absorption in an aqueous DEA solution, chemical
s) and ri the inner fiber radius (cm). reaction should be considered. The zwitterions-mechanism
The initial condition for CO2 in the lumen is specified as [25] was adopted for this theoretical study:
k1 =k21
in
Cig ¼ Cig ; for z ¼ 0 and all r ð7Þ CO2 þ R2 NH $ R2 NHþ COO2
in k2
where Cig is the inlet concentration of CO2 in the gas R2 NHþ COO2 þ R2 NH ! R2 NCOO2 þ R2 NHþ
2
phase (mol/cm3).
In the radial direction, symmetry is assumed at the axis of The mechanism consists of two steps, the formation of the
the cylindrical fiber: zwitterions followed by the removal of a proton by the amine.
The physicochemical properties, such as diffusivities of
›Cig CO2 in gas phase and in aqueous solutions, and solubilities
¼ 0; for r ¼ 0 and all z ð8Þ
›r were obtained from the literature [23,25,26]. In the case of
At the gas –liquid interface, the conservation of mass with chemical reaction, the enhancement factor E in Eq. (10), was
respect to CO2 is expressed as evaluated from the classical solution of gas absorption
accompanied by a chemical reaction [27].
›Cig
Dig ¼ 2Kext ðCig 2 ms Cil Þ; for r ¼ ri and all z ð9Þ The set of partial differential Eqs. (5) –(11) was solved
›r using the method of lines. A finite difference scheme in
where ms is the distribution coefficient between gas and dimensionless r direction was applied to convert the set of
liquid phase and Kext the external (membrane wall and shell partial differential equations into a system of ordinary
side) mass transfer coefficient (cm/s), calculated by Eq. (10): differential equations (ODE). The latter gives an ODE initial
1 Hi 1 value problem, which was solved by the explicit ‘hybrid’
¼ þ ð10Þ method [28].
Kext ki;membrane Eki;liquid
The shell side mass transfer coefficient, ki;liquid ; is calculated
by an engineering correlation developed for this type of cross 3. Experimental
flow membrane contactors [24]. The membrane mass
transfer coefficient, ki;membrane depends on the diffusivity of A gas mixture containing 15% CO2 – 85% N2 (procured
absorbed gas in the gas-filled, Dig ; or liquid-filled pores, Dil ; and certified by Air Liquid Hellas S.A.G.I.) was selected as
and the thickness lm ; porosity 1; and tortuosity t of the feed gas. This mixture simulates a typical composition
the membrane wall. When partial wetting of the membrane (in major components) of flue gases from a coal combustion
2156 M. Mavroudi et al. / Fuel 82 (2003) 2153–2159
Table 1
Specifications for the hollow fiber membrane module
Effective membrane area (cm2) 14,000
Effective area/volume (cm21) 29.3
Fiber diameter inside/outside (cm) 0.024/0.030
Effective fiber length (cm) 15.24
Fiber porosity (%) 40
Fiber pore size (mm) 0.03
Number of fibers 10,000
power plant. Pure water and aqueous solutions of DEA
(0.5 –2 M) were chosen as absorption liquids. Water used
through out the study was reverse osmosis grade and in
contact with ambient air in order to be saturated with N2.
Therefore, no transfer of N2 was involved in this study.
A Liqui-Cel Extra Flow membrane contactor (Hoechst
Celanese Corp., Charlotte, NC, USA) was used, 8 cm
dia. £ 28 cm long (2.5 in. £ 8 in.). Detailed design and
configuration features of this type of cross flow membrane
module have been presented in the literature [29].
Specifications of the hollow fiber membrane module are
given in Table 1.
4Fig. 3 is a schematic representation of the experimental
set-up. The feed gas was introduced directly from a gas
cylinder to the fiber lumen of the module at a pressure
between 1 and 1.5 atm and the liquid flowed through the shell
side at a pressure of 0.2 up to 0.5 atm higher than that of the
gas. The feed gas flow was controlled and measured with a
precision rotameter. Pressure gauges at the contactor inlet
and outlet indicated the gas pressure, while a back pressure
regulator was installed in the exit gas line in order to maintain
the desired pressure, if necessary. A check valve was used
before the contactor inlet to prevent accidental injection of
liquid into the feed gas line. The liquid absorbent was
pumped from the liquid storage tank. The instrumentation in
the liquid line for the control and measurement of flow and
pressure was similar to that in the gas line. The composition
of the gas streams was monitored by sampling a slip stream
from the feed or exit line and diverting it into a Perkin– Elmer
Fig. 3. Schematic representation of the membrane module contactor unit.
8500 gas chromatograph with a thermal conductivity
detector. Before sending the gas sample to the chromato-
graph, liquid droplets and moisture were removed by a glass
liquid trap and a moisture trap.
The module was kept in an isothermal condition, using a
temperature control water bath and experiments were
carried out at 23 ^ 0.5 8C. Gas flow rates were varied
from 50 to 240 N cm3/s and the liquid flow rates from 10 to
160 cm3/s. All data were obtained at steady state, after
30 min of operating time, which allowed for system
stabilization. Steady state was indicated by a constant CO2
concentration in the exiting gas stream. Three samples were
taken under the same operating conditions and the average
value was calculated.
4. Results and discussion
Carbon dioxide absorption experiments in pure water
were conducted initially to evaluate the performance of the
hollow fiber membrane contactor. The dependence of CO2
gas outlet concentration, expressed in a dimensionless form
ig =cig Þ; on the gas and absorbent flow rates is shown in
ðcout in
Fig. 4. The amount of CO2 in the gas outlet decreases as the
liquid flow rate increases. Obviously, an increase in the
liquid flow rate results in a lower liquid phase mass transfer
resistance and, hence, in a more efficient gas removal. This
effect is more pronounced when the gas flow rate is low. For
higher gas flow rates, an equivalent gas removal can be
achieved if a higher volume module is used providing more
gas –liquid contact area. The membrane contacting process
shows an excellent performance in terms of mass transfer.
The depletion of CO2 ððcin out in
ig 2 cig Þ=cig Þ was as high as 75%,
for gas and liquid flow rates equal to 50 N cm3/s and
160 cm3/s, respectively.
Theoretical estimations obtained from the numerical
solution of Eqs. (5) – (11) are plotted in the same diagram.
Model estimates of outlet CO2 concentration calculated for
 M. Mavroudi et al. / Fuel 82 (2003) 2153–2159
Fig. 4. Membrane-based CO2 absorption in water.
a completely hydrophobic membrane, i.e. for non-wetted
pores, are lower than those experimentally measured,
especially for high gas and liquid flow rates. An additional
mass transfer resistance may be considered as a probable
reason of this deviation. The lumen side and the shell side
resistances to mass transfer become negligible for high gas
and liquid flow rates, respectively, and the membrane
resistance seems to dominate the process. Considering, non-
wetted membrane pores, the membrane resistance, and
consequently the overall resistance to mass transfer, is
underestimated and the model predicts higher CO2 removal.
Trace impurities and long term operation of the membrane
are presumed to modify the surface hydrophobicity and,
thus, to allow some penetration of liquid into the pores,
thereby decreasing the membrane mass transfer coefficient
[16,30,31]. The theoretical predictions of CO2 depletion
were recalculated taking into account some possible
penetration of the liquid into the membrane pores. The
membrane mass transfer coefficient was calculated from
Eq. (11) assuming partially wetted membrane pores. The
fraction of wetted pores, x; was adjusted to fit the
experimental data and ranged from 2.5 to 8%, increasing
with liquid flow rate. Although the fraction of wetted pores
Fig. 5. Effect of chemical reaction on membrane-based CO2 absorption.
Feed gas: 100 N cm3/s. Simulation: partially wetted mode (solid curves).
2157
is small, the membrane resistance to mass transfer increases
significantly. Simulation results for partially wetted mode
are plotted as solid curves in the same diagram.
In the presence of DEA as absorbent, absorption is
facilitated by chemical reaction. Fig. 5 shows the overall
liquid phase mass transfer coefficient, Koverall ; as a function of
liquid flow rate. In this case, mass transfer increases
appreciably even for low DEA concentrations. By increasing
DEA concentration in the liquid phase from 0 to 2 M, the
mass transfer of CO2 increases because of an increase in the
reaction rate. At low liquid flow rates, the solution becomes
saturated with CO2, and the mass transfer rate decreases. At
high liquid flow rates, the absorbent does not become
saturated with CO2, and the gas absorption rate increases.
Theoretical estimations assuming partially wetted pores are
also plotted in Fig. 5 and seem to be in good agreement with
the experimental results. The membrane mass transfer
coefficient was calculated from Eq. (11), assuming that a
fraction of membrane pores, x; was liquid filled. The
adjustable values of x ranged from 1.5 to 7%, similar to
those estimated for the CO2 – water system.
The separation performance of the hollow fiber mem-
brane contactor, expressed as percentage of CO2 removal, is
given in Fig. 6 versus liquid flow rate for a constant gas flow
rate of 100 N cm3/s. Compared to water, performance
improves considerably, reaching up to 99% CO2 removal,
by using aqueous DEA solutions as absorbent under the
same experimental conditions. Theoretical predictions for
partially wetted pores, plotted in the same diagram, are in
good agreement with the experimental results. The
adjustable values of x were similar to those used in Fig. 5.
The use of a chemical aqueous solution instead of water
enhances mass transfer of CO2 and, therefore, the scrubbing
capacity of the liquid absorbent improves. Consequently,
for an equivalent gas removal the required absorbent flow
rate decreases and it can be achieved in a smaller contactor.
Against these considerable advantages, the main disadvan-
tage is the cost of chemical solvents. Since organic amines
Fig. 6. Removal of CO2 in various absorbents. Feed gas: 100 N cm3/s.
Simulation: partially wetted mode (solid curves).
2158 M. Mavroudi et al. / Fuel 82 (2003) 2153–2159
can be regenerated, their use is generally more economic
than other liquid absorbents, which are discarded after use.
This indicates that DEA is suitable as an absorbent for CO2
removal in a membrane contacting process. However,
comparison of theoretical and experimental results for all
gas/liquid systems studied indicate that the membrane is
operated somewhere between the limits of gas-filled and
liquid-filled pores. The penetration of the liquid into
the pores, as explained by the necking phenomenon,
depends on the gas – liquid system and on the characteristics
of the fiber used. In order to prevent this wetting, research
efforts should focus on new membrane materials having a
high degree of hydrophobicity [16,32], and/or on new liquid
absorbents with improved surface tension properties [31].
In order to evaluate the membrane-based technology
efficiency, the absorption performance of the hollow fiber
membrane contactor needs to be compared with that of a
conventional packed absorber. For this, the classical
measure of absorption technology efficiency was used, i.e.
the height of a transfer unit (HTU) required for CO2
absorption in an absorbent (here pure water and DEA). In
Fig. 7, the required HTUs for physical and chemical
absorption of CO2 under the same operating conditions are
plotted as a function of superficial velocity for the case of
the tested membrane contactor and for packed contactors
Fig. 7. HTU for a membrane contactor and for packed towers for CO2
absorption in (a) water and (b) DEA.
with Raschig rings of diameter dr ¼ 25 and 50 mm. The
height of transfer unit based on liquid phase, HTUL, was
plotted in Fig. 7(a) for the case of CO2 absorption in water,
while the height of transfer unit based on gas phase, HTUG,
demanded for a gas phase controlled process, was plotted in
Fig. 7(b) for the case of CO2 absorption in DEA. The values
of HTU for packed contactors were calculated with the use
of empirical correlations [33]. The HTUs for membrane
technology were based on the experimental results pre-
sented in this work.
Under the same operating conditions, the experimentally
obtained HTU values for the membrane contactor were
significantly lower than those of a conventional packed
contactor, for CO2 absorption both in water and in DEA.
This leads to lower specific area requirements and, hence, to
a reduction in absorber investment costs compared to
packed towers. Thus, a significantly higher amount of CO2
removal can be achieved with a relatively small module and
low flow velocities. Another benefit of using membrane
technology instead of conventional absorption equipment is
that membrane operation can be scaled-up linearly, so that
an increase in capacity is achieved simply by adding
membrane modules.
5. Conclusions
Gas – liquid contactors based on hollow fiber membranes
can be used to reduce acid gas emissions such as CO2 from
flue gases. The present experimental results with a
simulated flue gas mixture (CO2, N2) show that high levels
of CO2 removal (, 99%) can be accomplished with
chemical solution absorbents. Physical absorbents like
water can also be used albeit not with such high levels of
CO2 absorption. To simulate the behavior of gas –liquid
membrane contactors, a mathematical model was devel-
oped. The model takes into account mass transfer at the gas,
liquid and membrane interfaces, chemical reaction and
possible membrane wetting. Comparison of model esti-
mations with experimental results indicates partial wetting
of the membrane, resulting to significant membrane
resistance to mass transfer. Compared to conventional
technologies, hollow fiber membrane modules offer high
specific surface area and, therefore, the calculated HTU
values for similar operating conditions are significantly
smaller. This should lead to more compact, efficient and
easily scaled-up absorption units.
Acknowledgements
The authors wish to thank the European Coal and Steel
Community for support of this work. Maria Mavroudi
wishes to thank the State Scholarship’s Foundation for
economical support of her PhD research, which includes
part of this work.
 M. Mavroudi et al. / Fuel 82 (2003) 2153–2159
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