Research Article 1

Xiaoxu Wang
Theoretical and Experimental Studies on
Jia Gao
Jianshu Zhang Acetylene Absorption in a
Xiaopeng Zhang
Polytetrafluoroethylene Hollow-Fiber
Ruili Guo
Membrane Contactor
Key Laboratory for Green
Processing of Chemical
Engineering of Xinjiang
The separation of acetylene from a gas mixture was investigated using a polytetra-
Bingtuan, School of Chemistry fluoroethylene hollow-fiber membrane contactor and 1-methyl-2-pyrrolidinone
and Chemical Engineering, as absorbent. The effects of the gas velocity, the liquid velocity, the feed gas con-
Shihezi University, Shihezi, centration, and the module length on the acetylene mass transfer were investi-
Xinjiang, China. gated. The results showed that the acetylene mass transfer flux increased with in-
creasing liquid velocity, gas velocity, and feed gas concentration, but decreased
with increasing membrane module length. A mathematical model was used to
predict the wetting extent of the membrane and the mass transfer resistance in
the acetylene mass transfer process. The wetting extent of the membrane was
found to increase with increasing liquid velocity and to be effectively restrained
with increasing gas velocity. The liquid phase resistance and the wetted-mem-
brane phase resistance controlled the acetylene mass transfer in the acetylene
absorption process. The acetylene absorption efficiency was maintained at 90 %
for 114 h of the C2H2 membrane absorptionthermal desorption cycle process.

Keywords: Acetylene absorption, Hollow-fiber membrane contactor, Membrane wetting,

1-Methyl-2-pyrrolidinone, Polytetrafluoroethylene
Received: May 31, 2014; revised: September 23, 2014; accepted: November 27, 2014
DOI: 10.1002/ceat.201400338

1 Introduction no unloading at low flow rates, and operation at low pressure

Acetylene is a basic organic raw material used in various fields,
which can be produced by the calcium carbide process, the
hydrocarbon cracking process, and by plasma pyrolysis of coal.
The content of acetylene in the pyrolysis gas produced by the
hydrocarbon cracking process and by plasma pyrolysis of coal
is 530 %. The separation and enrichment of acetylene is highly
necessary. Acetylene has been primarily separated in gas sepa-
ration processes by adsorption and absorption methods. The
tower solvent absorption method is mainly applied in the in-
dustry. However, this method has many drawbacks, such as
flooding, entrainment, channeling, large-scale equipment, etc.
[1]. In contrast, a gas-liquid hollow-fiber membrane contactor
allows two phases to come into direct contact with each other
for mass transfer, without dispersion of one phase into the oth-
er [2]. This device offers several advantages, including a high
interfacial area per unit volume, no flooding at high flow rates,
Correspondence: Prof. Ruili Guo (grli@shzu.edu.cn), Key Laboratory
for Green Processing of Chemical Engineering of Xinjiang Bingtuan,
School of Chemistry and Chemical Engineering, Shihezi University,
Shihezi, Xinjiang 832003, China.
[3, 4], thus showing good prospects for gas absorption.
Hollow-fiber membrane contactors have been used to sepa-
rate CO2, SO2, H2S, benzene, and propylene from flue gas, nat-
ural gas, and gas mixtures. For example, Rahbari-Sisakht et al.
[5] investigated CO2 stripping in polyvinylidenefluoride
(PVDF) hollow-fiber membrane contactors using diethanol-
amine as absorbent. The results displayed that a CO2 stripping
efficiency of 82 % could be reached. Albo et al. [6] and Albo
and Irabien [7] studied CO2 absorption in a polypropylene hol-
low-fiber membrane contactor using the ionic liquid, 1-ethyl-
3-methylimidazolium ethylsulfate, as the absorption liquid.
The results showed that around 2835 % of the carbon dioxide
can be recovered. Park et al. [8] performed experimental stud-
ies on the removal of SO2 using a 2 M NaOH solution as ab-
sorbent in PVDF hollow-fiber membrane contactors. The SO2
removal efficiency could reach 85 %. Membrane gas absorption
provides an efficient way for acid gas separation. In addition,
gas molecules can diffuse through membrane pores to the other
side of the membrane at low pressure, which is suitable for the
safe operation of acetylene. Therefore, membrane gas absorp-
tion is a promising technology for the separation of acetylene
from pyrolysis gas mixtures.
At present, many mathematical models have been developed
for the analysis of mass transfer in membrane gas absorption
processes, such as the two-dimensional mathematical model

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2 Research Article

[9, 10], the three-dimensional mathematical model [11], the , and k are individ-
overall mass transfer coefficient, kg, kM, kM L
rate-based model [12], the plug flow model and Happels regu- ual mass transfer coefficients of the gas side, the dry mem-
lar free-surface model [1315], and the resistance-in-series brane, the wetted membrane, and the liquid side, respectively.
model [16, 17]. The resistance-in-series model is widely used to T is the temperature, R is the gas constant, and H represents
research changes in the extent of membrane wetting and resist- Henrys constant. Eq. (2) can also be expressed in terms of re-
ance in membrane gas mass transfer processes. sistance, as shown in Eq. (3)
In the industry, 1-methyl-2-pyrrolidinone (NMP) is widely
used as a solvent for the absorption of acetylene. NMP is also a RT RG RM RM RL (3)
good solvent for most polymer membrane materials, such as , and R are the total resistance, the gas
where RT, RG, RM, RM L
polypropylene, polyethylene, PVDF, polysulfone, etc. However,
phase resistance, the dry-membrane phase resistance, the wet-
polytetrafluoroethylene (PTFE) material shows a remarkable
ted-membrane phase resistance, and the liquid phase resist-
chemical resistance and is insoluble in all known solvents. In
ance, respectively.
this work, acetylene was separated from a gas mixture by a
PTFE membrane contactor using NMP as absorbent. The
effects of the liquid velocity, the gas velocity, the feed gas con-
2.2 Individual Mass Transfer Coefficients
centration, and the module length on the acetylene absorption
efficiency and the mass transfer flux were investigated by a
The mass transfer coefficient for the gas flow in the lumen side
one-way absorption process. A mathematical model correlating
can usually be described by Leveques correlation [19]:
the resistance-in-series equation is proposed to investigate
  0:33
membrane wetting and the mass transfer resistance of PTFE kg di di
hollow-fiber membranes for acetylene absorption. Additionally, Sh 1:62 ReSc (4)
Di:G L
an absorptionthermal desorption cycle process was performed
to detect the acetylene absorption performance and the solvent where Sh, Re, and Sc are the Sherwood number, the Reynolds
resistance of the PTFE membrane. number, and the Schmidt number, respectively. L is the effec-
tive length of the membrane. Di,G is the diffusivity of acetylene
in the gas phase.
2 Theory The mass transfer coefficient for the liquid flow in the shell
side is calculated by the following equation [20]:
2.1 Mass Transfer in the Membrane Contactor  
k d d
Sh L h 5:851  j h Re0:6 Sc0:33 (5)
The change of heat in the acetylene absorption process was Di;L L
minimal and could be neglected. Thus, the process was re-
garded as an isothermal operation. Meanwhile, there is no acet- where dh and j are hydrodynamic radius and the packing frac-
ylene-NMP chemical reaction. The resistance-in-series model tion of the module, respectively. Di,L is the diffusivity of acety-
was used to describe the mass transfer of the gas-liquid contac- lene in the liquid phase. In the non-wetted mode, the mem-
tor system. Mass transfer between the gas and the liquid brane mass transfer coefficient kM is predicted using the
through the hollow-fiber membrane contactor occurs in three following equation:
parts: the gas film, the membrane, and the liquid film [18]. In 1 td
the partial wetting operation mode, the mass transfer flux Ji1) non-wetted (6)
kM Di;M eM
of the acetylene component is given in Eq. (1). The overall mass
transfer coefficient shown in Eq. (2) is a function of the mass In the membrane-wetting mode, the membrane mass trans-
transfer coefficients in the gas, membrane, and liquid. fer coefficient can be expressed using the following equation:
kG k 1 htdwetted
J p  pi;m M pi;m  pi;int (7)
RT i;g RT
kM Di;L eM

kM k
C  Ci;m L Ci;m  Ci;L (1) where eM is the membrane porosity, dnon-wetted and dwetted are
H i;int H
the thicknesses of the non-wetted and wetted parts of the
1 RT RT H H membrane pores, respectively, t is the tortuosity, and Di,M is
(2) the effective diffusion coefficient of the gas in the pores, which
KG kG kM kM kL
is calculated by the combination of the molecular and Knudsen
where pi,g, pi,m, and pi,int are the acetylene partial pressures in diffusivities in the following equation:
the bulk gas phase, the gas-membrane interface, and the gas- 1 1 1
liquid interface, respectively; Ci,int, Ci,m, and Ci,L are the acety- a (8)
Di;M Di;g DK
lene concentrations at the gas-liquid interface, the liquid-mem-
brane interface, and the liquid bulk, respectively. KG is the where DK is the Knudsen diffusion coefficient.

1) List of symbols at the end of the paper.

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 Research Article 3

3 Experimental Table 1. Specifications of the hollow-fiber membrane module.

3.1 Materials and Methods of Analysis Parameter Value

Module outer diameter, Do 0.014 m

The NMP used in the experiments was purchased from Tianjin
Guangfu Science and Technology Development Co., Ltd., and Module inside diameter, Di 0.01 m
the purity was 99 %. The solubility of acetylene in NMP was Fiber outside diameter, do 2.3 103 m
2.8 g mL1 by bubble absorption under the conditions of 20 C
and 0.1 MPa. The hydrophobic porous PTFE hollow-fiber Fiber inside diameter, di 8 104 m
membrane used in the experiments was provided by Zhejiang Effective fiber length, L 0.01, 0.02, 0.03, 0.04 m
DD Water Industry Co., Ltd. (Zhejiang, China). Tab. 1 shows
Fiber wall thickness, d 7.5 104 m
the characteristics of the membrane.
The gas concentrations of acetylene in the feed and outlet Number of fibers, n 7
gases were measured by a thermal conductivity detector gas 4
Outer membrane area, A 10 5.06, 10.1, 15.17, 20.2 m2
chromatograph (GC-2014C; Shimadzu), and the liquid concen-
trations of acetylene were determined by a hydrogen flame ion- Average pore size, dp 0.22 mm
ization detector gas chromatograph.
Fiber porosity, e 52 %

Packing density 37.03 %

3.2 Experimental Unit and Procedures

According to the solubility in NMP and the composition of the

pyrolysis gas, in the membrane absorption process, carbon
monoxide, hydrogen, and acetylene were mixed to simulate the
pyrolysis gas.
Fig. 1 is a schematic representation of the experimental setup
for acetylene absorption. In the hollow-fiber membrane con-
tactor, the gas stream flows through the inside of the hollow fi-
bers and the absorption liquid flows countercurrently through
the shell side considering the higher absorption liquid pressure,
which results in easy wetting of the membrane pores. Each gas
stream was mixed in the mixer by turning each valve of the
chromatograph to the desired velocity, and was then fed into
the hollow fiber membrane lumen side. The treated gas stream
was released at the other end of the module. Adjusting the
pressure control valve resulted in an increase in the gas phase
pressure to about 0.001 MPa higher than that of the liquid
phase. The rich absorbent entered the solution tank 1 in a non-

Figure 1. Scheme of the experimental setup for acetylene absorption.

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4 Research Article

liquid-circulated manner. When the process was

operated in the liquid-circulated mode, the rich ab-
sorbent entered the stripper through a heater ex-
changer and was hot-regenerated. The temperature
of the heater exchanger was controlled at about
173 C by an oil bath. In order to ensure that the
acetylene was fully regenerated from the rich ab-
sorbent, the stripper was heated to 173 C by an
electric heating tape. The regenerated acetylene
could reach a purity of 99 %. The regenerative ab-
sorbent was cooled through a water cooler and was
then once again introduced into the shell side of
the membrane contactor. The operation continued
for about 1 h to allow the system to reach a stable
state. Stable-state conditions were indicated by a
constant acetylene concentration of the treated gas.

3.3 Treatment of Experimental Data Figure 2. Effect of the liquid velocity on the acetylene mass transfer flux and the
absorption efficiency.
In the present paper, the acetylene mass transfer
flux JC2 H2 and the absorption efficiency hC H were used to indi- The C2H2 mass transfer was analyzed by the mathematical
2 2
cate the process efficiency, which can be experimentally calcu- model at various liquid velocities (Fig. 3). The results show that
lated from the following equations: the mass transfer resistance of the C2H2 membrane absorption
process was mainly composed of the liquid phase resistance
and the wetted-membrane phase resistance. The percentage of
QG:in CG:in  QG:out CG:out 273 60 1000 the liquid phase resistance decreased from 80.95 to 43.9 % with
JC2 H2 (9)
22:4TA the liquid velocity increasing from 0.00361 to 0.0167 m s1,
which led to a decreased total mass transfer resistance. However,
QG:in CG:in  QG:out CG:out the membrane wetting extent increased from 33 to 43 % with in-
hC H 100% (10) creasing liquid velocity, resulting in an increase in the wetted-
2 2 QG:in CG:in
membrane phase resistance from 17.82 to 53.44 %. When the liq-
uid velocity increased from 0.0135 to 0.0167 m s1, the wetted-
CG.in and CG.out are the acetylene concentrations of the feed membrane resistance was higher than the liquid phase resistance.
gas and the treated gas, respectively. QG.in and QG.out are the The increased wetted-membrane resistance led to a slight de-
gas velocities of the feed gas and the treated gas, respectively. T crease in the total resistance. Thus, the C2H2 mass transfer flux
is the operation temperature and A is the mass transfer area. increased only 0.293 times with the liquid velocity increasing
from 0.00361 to 0.0167 m s1 because of the wetted membrane.

4 Results and Discussion

4.1 Effect of the Liquid Velocity on the
Acetylene Mass Transfer

Fig. 2 shows the effect of the liquid velocity on the

acetylene mass transfer flux and the absorption
efficiency at a membrane module effective length of
30 cm, a C2H2 content of 8 % in the feed, and a gas
velocity at 0.4739 m s1. When the liquid velocity
was increased from 0.00361 to 0.0167 m s1, the
acetylene mass transfer increased slightly and the
acetylene absorption efficiency increased from
65.17 to 92.79 %. A high liquid velocity decreased
the thickness of the liquid membrane side boun-
dary layer. In addition, a good correlation can be
seen between the experimental and the simulated
profiles for the acetylene mass transfer flux and the
absorption efficiency. The maximum deviation was Figure 3. Membrane wetting extent and mass transfer resistance at various liq-
less than 10 %. uid velocities.

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 Research Article
4.2 Effect of the Gas Velocity on the Acetylene
Mass Transfer
Fig. 4 shows the effects of the gas velocity on the acetylene mass
transfer flux and the absorption efficiency at a membrane mod-
ule effective length of 30 cm, a C2H2 content of 8 % in the feed,
and a liquid velocity at 0.01679 m s1. The acetylene mass trans-
fer flux increased significantly from 0.577 to 2.424 mol m2h1
when the gas velocity was increased from 0.237 to 1.4217 m s1.
The increase in gas velocity increased the acetylene concentra-
tion and accelerated the renewal of acetylene at the gas-liquid in-
terface. However, the higher gas velocity decreased the residence
time of the gas in the membrane, which resulted in a decline of
the acetylene absorption efficiency from 95.48 to 58.52 %.
The C2H2 mass transfer was analyzed by the mathematical
model at various gas velocities (Fig. 5). The results also showed
Figure 4. Effect of the gas velocity on the acetylene mass transfer flux and the
absorption efficiency.
Figure 5. Membrane wetting extent and mass transfer resistance at various gas
velocities.
Chem. Eng. Technol. 2015, 38, No. 00, 19 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
5
that the mass transfer resistance of the absorption process was
mainly controlled by the liquid phase resistance and the wet-
ted-membrane phase resistance. The increase in the gas veloc-
ities had no effect on the liquid phase resistance and had a
minimal influence on the gas phase resistance. However, mem-
brane wetting was effectively restrained by increasing the gas
velocities because the wetting extent of the membrane de-
creased from 45 to 42.5 %.
4.4 Effect of the Feed Gas Concentration on the
Acetylene Mass Transfer
Fig. 6 shows the effects of the feed gas concentration on the
acetylene mass transfer flux and the absorption efficiency at a
membrane module effective length of 30 cm, a liquid velocity
of 0.0167 m s1, and a gas velocity of 0.4739 m s1.
The acetylene mass transfer flux increased with in-
creasing feed gas concentration. The increase in the
feed acetylene concentration enhanced the driving
force of the system. The acetylene absorption effi-
ciency increased with increasing feed gas concen-
tration from 7 to 9 % and then slightly dropped with
further increasing the feed gas concentration to
10 %. The C2H2 absorption was balanced in the gas-
liquid interface when the feed gas concentration was
increased from 7 to 9 %. Thus, additional acetylene
could not be absorbed when the acetylene concentra-
tion in the feed gas increased from 9 to 10 %.
4.5 Effect of the Module Length on the
Acetylene Mass Transfer
The effects of the membrane module effective
length on the acetylene mass transfer flux and the
absorption efficiency were investigated at 8 % C2H2
concentration in the feed, a liquid velocity of
0.0167 m s1, and a gas velocity of 0.4739 m s1. As
shown in Fig. 7, the acetylene mass transfer flux de-
creased with increasing module length. The wetting
extent of the membrane increased from 28.1 to
66 % with the membrane module length increasing
from 10 to 40 cm (Fig. 8). The wetted membrane
resistance and the total membrane resistance in-
creased with increasing module length.
In addition, Fig. 7 shows that the acetylene ab-
sorption efficiency increased when the module
length increased from 10 to 30 cm and slightly
dropped when the module length increased to
40 cm. The mass transfer area and residence time
effectively increased with increasing module length,
while the total mass transfer coefficient declined
with increasing module length due to the increase
in the wetted-membrane resistance (the fixed ratio
of the outer membrane area to the lumen volume is
1437). Therefore, the mass transfer flux of acety-
lene declined noticeably when the membrane mod-
ule effective length increased from 30 to 40 cm.
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6 Research Article
Figure 6. Effect of the feed gas concentration on the acetylene mass transfer
flux and the absorption efficiency.
Figure 7. Effect of the module length on the acetylene mass transfer flux and
the absorption efficiency.
Figure 8. Effect of the membrane module effective length on membrane wet-
ting and the mass transfer resistance.
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4.6 C2H2 AbsorptionThermal
Desorption Cycle Process in the PTFE
Hollow-Fiber Membrane Contactor
The membrane absorptionthermal desorption
cycle process was investigated using NMP as ab-
sorbent at a membrane module effective length of
30 cm, 8 % C2H2 concentration in the feed, a liquid
velocity of 0.0167 m s1, and a gas velocity of
0.4739 m s1. The system was continuously oper-
ated for 114 h. Fig. 9 presents the acetylene absorp-
tion efficiency as a function of the operation time.
The acetylene absorption efficiency remained at
99 % within the first 8 h. After this, the absorption
efficiency slightly declined and remained at more
than 90 % in the last 106 h. This decrease was at-
tributed to the increased wetting extent of the
membrane and the increased C2H2 concentration
in the feed. The rich absorbent was heated to
173 C for C2H2 desorption. The content of C2H2
in the regenerated gas reached 99 %, which met the
production requirements of the downstream prod-
ucts. The C2H2 concentration in the regenerative
absorbent was 2.04 106 g mL1.
A comparison between the operation of gas
absorption column and membrane gas absorption
processes for the separation of acetylene is shown
in Tab. 2. The results show that the membrane gas
absorption process, as compared to the column
absorption process for the separation of C2H2,
presents a lower absorption efficiency of C2H2.
However, membrane gas absorption is operated at
room temperature and near atmospheric pressure.
Therefore, membrane gas absorption is a potential
technology for the separation of acetylene from
pyrolysis gas mixtures. Further research will be
focused on the decrease of membrane wetting and
the enhancement of mass transfer on the liquid
side.
5 Conclusions
The PTFE hollow-fiber membrane absorption
thermal desorption process was used to separate
and purify acetylene from simulated plasma pyrol-
ysis gas streams using NMP as absorbent. The re-
sults were as follows:
The C2H2 one-way absorption efficiency reached
was as high as 95.48 %. The C2H2 absorption
thermal desorption cycle process revealed that the
absorption efficiency was higher than 90 % during
114 h and the C2H2 concentration of the regener-
ated gas was 99 %. The C2H2 concentration of the
regenerative absorbent was 2.04 106 g mL1.
A mathematical model correlating the resis-
tance-in-series equation was used to analyze the
C2H2 mass transfer. The results showed that the
liquid phase resistance and the wetted-mem-
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 Research Article 7

Symbols used
A [m2] total outer surface area of the
hollow fibers
Ci,int [mol m3] acetylene concentration at the
gas-liquid interface
Ci,L [mol m3] acetylene concentration in the
liquid bulk
Ci,m [mol m3] acetylene concentration at the
liquid-membrane interface
Di,G [m2s1] gas diffusion coefficient
Di,L [m2s1] liquid diffusion coefficient
Di,M [m2s1] membrane diffusion coefficient
DK [m2s1] Knudsen diffusion coefficient of
acetylene in the membrane
phase
dh [m] hydrodynamic radius
Figure 9. Long-term performance of the membrane contactor. H [m3kPa kmol1] Henrys constant
J [mol m2h1] mass transfer flux
KG [kmol m2s1kPa1] overall mass transfer coefficient
brane phase resistance constituted the main mass transfer
kg [m s1] gas phase mass transfer
resistance. The increased liquid velocity decreases the liquid
coefficient
phase resistance but increases wetting of the membrane and
kL [m s1] liquid mass transfer coefficient
the wetted-membrane phase resistance. The increased gas
kM [m s1] membrane mass transfer
velocity had little influence on the C2H2 mass transfer resis-
coefficient
tance. Nonetheless, the wetting extent of the membrane
L [m] length of a hollow fiber
could be restrained by increasing the gas velocity.
pi,g [kPa] acetylene partial pressure at the
The wetted-membrane resistance was as high as 53.44 % of
bulk gas phase
the total mass transfer resistance due to the wetted mem-
pi,int [kPa] acetylene partial pressure at the
brane. Therefore, developing a membrane material with low
gas-liquid interface
wetting extent for NMP is significantly valuable for acetylene
pi,m [kPa] acetylene partial pressure at the
membrane absorption and purification processes.
gas-membrane interface
QG.in [mL min1] feed gas velocity
QG.out [mL min1] outlet gas velocity
Acknowledgment R [m3kPa kmol1K1] gas constant
Re [] Reynolds number
Sc [] Schmidt number
The authors gratefully acknowledge the financial support from
Sh [] Sherwood number
the Xinjiang Production and Construction Corps of Industrial
T [K] temperature
Science and Technology Projects of China (no. 2010GG13), the
National Technology Research and Development Program of
China (no. 2012AA03A611), and the Program for Changjiang
Greek symbols
Scholars and Innovative Research Teams in University (no.
IRT1161). dnon-wetted [m] thickness of the dry membrane
dwetted [m] thickness of the wetted
The authors have declared no conflict of interest. membrane
eM [] surface porosity

Table 2. Comparison between the column gas absorption and membrane gas absorption processes for the separation of acetylene
(DMF = dimethylformamide).

Method Acetylene concentration Absorption Operation Operation C2H2 absorption Reference

in the feed [vol %] solvent pressure [MPa] temperature [C] efficiency [%]

Column gas absorption 1 DMFa) 1.0 35 99.9 [21]

12 DMF 2.6 12.2 99.1 [22]

10 DMF 0.8 50 95 [23]

Membrane gas absorption 8 NMP 0.1 2025 9095 This study

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8 Research Article

j [] packing fraction of the
membrane contactor
hC H [] removal efficiency
2 2
t [] tortuosity of the membrane pore
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 Research Article
Research Article: Acetylene is primarily
separated in gas separation processes
by adsorption and absorption methods.
Membrane absorption technology was
applied to purify acetylene gas from
simulated pyrolysis gas. A mathematical
model correlating the resistance-in-
series equation was used to predict
changes in the wetted membrane
resistance and the mass transfer
resistance during the acetylene mass
transfer process.
Chem. Eng. Technol. 2015, 38, No. 00, 19
9
Theoretical and Experimental Studies
on Acetylene Absorption in a
Polytetrafluoroethylene Hollow-Fiber
Membrane Contactor
X. Wang, J. Gao, J. Zhang, X. Zhang,
R. Guo*
Chem. Eng. Technol. 2015, 38 (),
XXX K XXX
DOI: 10.1002/ceat.201400338
2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.cet-journal.com