Pervaporative separation of bioethanol produced from the

fermentation of waste newspaper

Ly Thi Phi Trinh
a
, Eun Jin Cho
b
, Young Ju Lee
c
, Hyeun-Jong Bae
b
, Hong-Joo Lee
a,
*
a
Department of Bioenergy Science and Technology, Chonnam National University, Gwangju 500-757, Republic of Korea
b
Department of Bioenergy Science and Technology, Bio-energy Research Institute, Chonnam National University, Gwangju 500-757, Republic of Korea
c
Gwangu Center, Korea Basic Science Institute, Gwangju 500-757, Republic of Korea
1. Introduction
Bioethanol is one of the most important renewable biofuels
since it has the potential to reduce negative environmental
impacts such as air pollution and greenhouse gas emission [14].
Conventionally, bioethanol is produced from the fermentation of
sucrose-containing feedstocks such as corn and sugar cane. The
techniques are mature and the yield of bioethanol from starch is
high. However, the use of starchy feedstocks increases the risk of
causing global food storage. Therefore, interest on the use of
lignocellulosic biomass, which is abundant, and most importantly,
renewable natural source, has increased as an alternative to the
conventional biomass for bioethanol production. It includes weed,
grass, saw dust, municipal solid waste, woody biomass, paper mill
waste, and waste paper [5,6]. Waste paper consists of a
considerable share of municipal and industrial waste. However,
the recycling rate of waste paper is low and the recycled waste
paper has a low grade paper product because of shorted ber
length. Still, waste paper is considered as one of the prospective
and renewable biomass materials to produce bioethanol because
of the high fraction of cellulose [7,8].
Currently, distillation has been used for the separation and
purication of the produced bioethanol, but it has some
disadvantages due to high energy requirements and low efciency
at low ethanol concentrations. Pervaporation is one of the most
promising approaches for the recovery of alcohols produced from
fermentation [911]. In the pervaporation process, one of the
components is preferentially removed from the mixture due to its
higher afnity and diffusivity in the membrane when a membrane
is in contact with a liquid mixture [1214].
It is known that the pervaporative separation performance,
such as the separation factor and ethanol ux, depends on the
selective interaction with a specic component of the feed mixture
and on the properties of membrane materials. Among polymeric
membranes in the pervaporation process, silicone rubber based
polydimethylsiloxane (PDMS) membrane is most used since
silicone-containing polymers exhibit good organophilicity for
separation of aqueous organic solutons [15].
In general, membrane process performance is strongly inu-
enced by process conditions such as ethanol concentration in feed
and operating temperature. In addition, membrane fouling is one
of the most important considerations, which takes place due to the
organic deposition on the membrane surface [16]. Fermentation
broth, containing inorganic salts, sugars, microbial cells and other
chemical inhibitors as well as produced ethanol, would affect the
pervaporation performance [17,18].
In the present study, the pervaporative separation of bioethanol
was carried out in the fermentation broth after anaerobic
fermentation of glucose and waste newspaper. In the preliminary
study, synthetic solutions of ethanol/water mixture with a wide
Journal of Industrial and Engineering Chemistry 19 (2013) 19101915
A R T I C L E I N F O
Article history:
Received 4 December 2012
Accepted 26 February 2013
Available online 6 March 2013
Keywords:
Bioethanol
Fermentation
PDMS membrane
Pervaporation
Separation
A B S T R A C T
In this study, a hydrophobic polymeric polydimethylsiloxane (PDMS) membrane was used for the
pervaporative separation of bioethanol produced fromfermentation of lignocellulosic biomass (waste
newspaper) and glucose. As a preliminary study, the pervaporation permeation performance showed
strong dependence on feed concentration and temperature. The pervaporation of bioethanol
produced by the fermentation of waste newspaper by Saccharomyces cerevisiae decreased process
performance. However, the process performance was restored reversibly by water cleaning. The
pervaporative separation of bioethanol from the fermentation of waste newspaper was carried out
without any signicant decreasing process performance in the study.
2013 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights
reserved.
* Corresponding author. Tel.: +82 62 530 2040; fax: +82 62 530 2047.
E-mail addresses: hjlee68@jnu.ac.kr, hjleehan@daum.net (H.-J. Lee).
Contents lists available at SciVerse ScienceDirect
Journal of Industrial and Engineering Chemistry
j our n al h o mepag e: w ww. el sevi er . co m / l ocat e/ j i ec
1226-086X/$ see front matter 2013 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jiec.2013.02.036
concentration range (0.510.0%) were used to determine perva-
poration operating conditions and investigate the inuence of
temperature and feed concentration. In addition, the permeation
performance change was observed in the pervaporative separation
experiments in series of experiments of bioethanol produced by
the fermentation of waste newspaper.
2. Experimental methods
2.1. Bioethanol production
In this study, bioethanol was produced in the fermentation of
waste newspaper. Waste newspaper was dried at ambient
temperature to equilibrium moisture content and then cut into
approximately 2 cm length and stored for fermentation. And 100 g
(dry weight) of waste paper was soaked in water for 1 day at room
temperature. Waste newspaper samples were ground for size
reduction (particle size: 251422 mm) in a Willy mill tted with
stainless steel blades.
For inoculum, a spore suspension of Saccharomyces cerevisiae
KCTC 7906 was cultured on yeast extract, peptone, and biomass at
30 8C. Three hundred milliliter of the actively growing culture was
added to the fermenter and kept under anaerobic condition. The
fermenter containing 3 L of medium was autoclaved at 121 8C for
1517 min and then cooled down to 35 8C. Fermentation was
carried out in a fermenter, FMT-05 (Fermentec, Korea), using
medium containing 5 g/L yeast extract, 5 g/L peptone, 3.3 g/L
potassium phosphate, 0.2 g/L ammonium sulfate, 0.4 g/L magne-
sium sulfate, and 100 g/L of biomass (waste newspaper or glucose).
The pH of fermentation broth was maintained at 5 during growth.
After 48 h fermentation at 35 8C and an agitation speed of
300 rpm, the fermentation broth was ltered through Millipore
mixed cellulose esters membrane lter paper (0.45 mm pore size
and 47 mm diameter). The ltered fermentation broth was used as
the feed for the pervaporative separation. As reference experiment,
the fermentation of glucose was considered as bioethanol without
any inhibitor to investigate the inuence of fermentation broth on
the pervaporation performance.
2.2. Preparation and characterization of PDMS membrane properties
A hydrophobic polydimethylsiloxane (PDMS) membrane was
prepared from RTV 615A (dimethylsiloxane) and RTV 651B (a
curing agent) distributed by Momentive Performance Materials,
Inc. Ten gram of RTV 615A and 1 g of RTV 615B were mixed with
20 mL of isooctane (Aldrich) in a glass beaker while stirring. After
mixed, the homogeneous solution was poured onto a Teon plate
to form a thin liquid layer. The plate was held at 70 8C in an oven
for 24 h to dry and crosslink a hydrophobic PDMS membrane. The
membrane was peeled off the plate after curing and cut to the size
of the membrane cell for the pervaporative separation and
the characterization of the membrane properties.
To measure the degree of swelling, a membrane sample was
equilibrated for 24 h in mixtures of water and ethanol. The sample
was dried at 75 8C until a constant dry weight was obtained. The
degree of swelling (DS) was calculated as follows:
DS
W
s
W
d
W
d
100 (1)
where W
s
denotes weight of the swollen membrane and W
d
the
weight of the sample membrane before immersion.
Using a sessile drop technique, the contact angle of PDMS, a
measure of its hydrophobicity, was measured with a contact angle
meter, FACE CA-S150 (Kyowa Interface Science, Japan); a higher
contact angle indicates more hydrophobic [19]. The thickness of
PDMS was measured using a thickness gauge (Mitutoyo, Japan).
2.3. Pervaporative separation of bioethanol
The membrane module was a circular at-plate pervaporation
cell made of stainless steel with an effective area of 16.61 cm
2
.
Details of the experimental setup are found from the previous
studies [12,20]. A temperature-controlled water bath was used to
heat the feed to the desired temperature (from 20 to 60 8C). The
feed was kept at an atmospheric pressure, whereas the pressure of
the permeate maintained below 5 mmHg using a vacuum pump in
all experiments. One liter of examined solutions (synthetic
solution of ethanol/water and bioethanol produced by fermenta-
tion) in a conical ask was circulated at 1.8 L/min.
The permeate was initially collected in the cold trap immersed
in liquid nitrogen and was then sampled periodically. The
pervaporation performances, ethanol ux (J
p
) and separation
factor (a), were considered as follows:
J
p

W
A
m
t
(2)
a
y=1 y
x=1 x
(3)
where W is the weight of the condensate (g), A
m
the membrane
area (m
2
), t the duration of the sample collection (h), and x and y
the weight fraction of components in feed and permeate,
respectively.
The consecutive experiment was carried out to investigate the
inuence of fermentation broth on the permeation performance as
follows: pervaporation of synthetic solution with 5.0% ethanol,
three repeated pervaporation of bioethanol from the fermentation
broth of waste newspaper, and synthetic solution with 5.0%
ethanol.
In this study, the concentration of chemical compositions such
as ethanol, xylose and acetic acid was determined using high-
performance liquid chromatography (HPLC) equipped with a
refractive index (RI) detector (Waters 2414, USA) using a Rezex
RPM column (4.6 mm 300 mm; Phenomenex, USA). HPLC-grade
water was supplied at a ow rate of 0.6 mL/min as a mobile phase
and the temperature was controlled at 40 8C. The mobile phase was
ltered using Millipore mixed cellulose esters membrane lter
paper (0.45 mm pore size and 47 mm diameter).
3. Results and discussion
3.1. Characterization of membrane properties
The degree of swelling, which depends on the nature of the
polymeric material and the homogeneity of the membrane,
determines not only the dimensional stability of the membrane,
but also affects its selectivity and permeability. The degree of
swelling value of the PDMS membrane in ethanol/water binary
mixtures as a function of ethanol concentration is shown in Fig. 1.
The degree of swelling of the PDMS membrane was small in water,
then the values linearly increased as the ethanol concentration
increased. The degree of swelling was within 4852% at high ethanol
concentrations, similar results reported from a previous study [13].
The contact angle of the PDMS membrane was measured to
78.0 1.08 by the sessile drop technique, which indicates that the
PDMS membrane surface is hydrophobic. The thickness of PDMS was
measured by the thickness gauge to be 91 3 mm.
3.2. Pervaporation membrane performance in synthetic solutions
3.2.1. Preliminary pervaporation experiments
As a preliminary study, the pervaporative separation was
carried out at the initial ethanol concentration of 5.0% and the
L.T.P. Trinh et al. / Journal of Industrial and Engineering Chemistry 19 (2013) 19101915 1911
temperature of 40 8C. The ethanol concentration in the product
showed stable values of around 30% at 5 h or longer. In the case of
ethanol ux in Fig. 2(a), the values increased at the initial stage and
reached a stable value. The separation factor showed stable values
of 810 at around 5 h or longer, as shown in Fig. 2(b).
3.2.2. Inuence of temperature on pervaporation performances
In pervaporation, temperature affects solubility and diffusivity
in the membrane structure and thus process performance [21]. The
inuence of temperature on the pervaporation performances was
investigated in the pervaporative separation at a feed concentra-
tion of 5.0%. Fig. 3(a) shows the amount of the transported ethanol
through the PDMS membrane with increasing temperature. As
shown in the gure, the ethanol in product was measured about
35% at higher temperatures than 30 8C.
Fig. 3(b) shows the inuence of the operating temperature on
the ethanol ux and separation factor. The ethanol ux increased
as the temperature increased. The value was measured to 38 g/
m
2
h at 60 8C, which is about 10 times higher than that at 20 8C. It is
suggested that a higher ethanol ux value at high temperature is
related to the increased swelling capacity and water desorption
due to weak adsorption capacity on the membrane surface [22].
The separation factor was kept between 9 and 10 even with
different operating temperature.
Ethanol in water (%)
0 2 4 6 8 10 12
D
e
g
r
e
e

o
f

s
w
e
l
l
i
n
g

(
%
)

0
10
20
30
40
50
60
Fig. 1. Degree of swelling of PDMS membrane in the binary mixture of ethanol and
water.
Time (h)
0 2 4 6 8 10 12
E
t
h
a
o
l

F
l
u
x

(
g
/
m
2
h
)
0
2
4
6
8
10
12
14
(a) Ethanol flux
Time (h)
0 2 4 6 8 10 12
S
e
p
a
r
a
t
i
o
n

f
a
c
t
o
r
0
2
4
6
8
10
12
(b) Separation factor of ethanol
Fig. 2. Ethanol ux and separation factor with duration time (initial concentration:
5.0%, temperature: 40 8C).
Temperature (
o
C)
10 20 30 40 50 60 70
E
t
h
a
n
o
l

i
n

p
r
o
d
u
c
t

(
%
)
0
10
20
30
40
50
(a) Ethanol in product
Temperature (
o
C)
10 20 30 40 50 60 70
E
t
h
a
n
o
l

f
l
u
x

(
g
/
m
2
h
)
0
5
10
15
20
25
30
35
40
S
e
p
a
r
a
t
i
o
n

f
a
c
t
o
r
0
2
4
6
8
10
12
14
Ethanol flux
Separation factor
(b) Ethanol flux and separation factor
Fig. 3. Inuence of the operating temperature on the pervaporation performance
(ethanol concentration: 5.0%).
L.T.P. Trinh et al. / Journal of Industrial and Engineering Chemistry 19 (2013) 19101915 1912
The temperature dependence of the permeation ux can be
expressed by an Arrhenius-type relationship:
J
p
A
p
exp
E
a
RT

(4)
where J
p
is the permeation ux, A
p
the pre-exponential factor, R the
ideal gas constant, T the temperature, and E
p
the apparent
activation energy of permeation. The apparent activation energy
accounts for the effect of temperature on the driving force, which
characterizes the temperature dependence of the permeability
through membrane.
Based on the relationship between permeation ux of ethanol
and temperature, the apparent activation energy of ethanol
permeation was calculated to be 46.0 kJ/mol, similar to that of
the previous study [13]. In the relationship between water ux and
the operating temperature, the apparent activation energy of
water permeation was calculated to be 41.2 kJ/mol. The higher
activation energy value indicates that ethanol ux increases more
rapidly than water ux [23]. It is suggested that the ethanol ux
increases more signicantly than water as the operating tempera-
ture increases.
3.2.3. Inuence of the initial ethanol concentration on pervaporation
performances
In this study, the feed concentration was increased from 0.5% to
10.0% in order to observe the inuence of feed concentration on
pervaporation performance. Fig. 4(a) shows the ethanol concen-
tration in the product with increasing feed concentration. The
ethanol concentration in the product showed similar values at
ethanol concentrations lower than 1.0% in the feed. At ethanol
concentrations higher than 1.0% in the feed, however, the
recovered ethanol concentration increased linearly, showing that
the ethanol concentration in the product was 43% at a feed
concentration of 6.0%. The ethanol concentration in product did not
increase signicantly at concentrations higher than 8.0%, as shown
in the gure.
Solution-diffusion is the generally accepted mechanism of
mass transport through non-porous membranes. In a pervapora-
tive separation, mass transport through membrane is a rate-
controlling process, which is generally governed by the Ficks rst
law. The mass ux is proportional to the feed concentration and
the driving force is the difference between feed and permeate
concentration [9].
In the inuence of the initial ethanol concentration on the
process performance, ethanol in product in terms of ethanol ux
and separation factor has a strong dependence on the feed
concentration. The ethanol ux showed similar values of around
2.42.8 g/m
2
h at concentrations lower than 1.0%. Then, the ux
increased linearly at concentrations higher than 1.0%, resulting in
Initial ethanol concentration in feed (%)
0 2 4 6 8 10 12
E
t
h
a
n
o
l

i
n

p
r
o
d
u
c
t

(
%
)
0
10
20
30
40
50
60
(a) Ethanol in product
Initial ethanol concentration in feed (%)
0 2 4 6 8 10 12
E
t
h
a
n
o
l

f
l
u
x

(
g
/
m
2
h
)
0
10
20
30
40
50
60
S
e
p
a
r
a
t
i
o
n

f
a
c
t
o
r
0
5
10
15
20
Ethanol flux
Separation factor
(b) Ethanol flux and separation factor
Fig. 4. Inuence of the initial ethanol concentration on the pervaporation
performance (temperature: 40 8C).
Duration time (h)
0 2 4 6 8 10 12 14
E
t
h
a
n
o
l

f
l
u
x

(
g
/
m
2
h
)
0
5
10
15
20
25
30
(a) Ethanol flux
Duration time (h)
0 2 4 6 8 10 12 14
S
e
p
a
r
a
t
i
o
n

f
a
c
t
o
r
0
2
4
6
8
10
12
14
16
(b) Ethanol separation factor
Fig. 5. Permeation ux and separation factor of bioethanol from the fermentation
broth of waste newspaper.
L.T.P. Trinh et al. / Journal of Industrial and Engineering Chemistry 19 (2013) 19101915 1913
increased ethanol ux, up to 52 g/m
2
h, at a feed concentration of
10.0%, as shown in Fig. 4(b).
Considering the inuence of the initial ethanol concentration
on the separation factor, the estimated values were notably high
at low concentration (0.5%) with 18.9 in Fig. 4(b). At concentra-
tions higher than 1.0%, the resulting values did not increase
signicantly with increasing feed concentration. In general,
separation factor will decrease due to the enlargement of free
volume in membrane structure, which was reported in the
previous studies [13,22].
3.3. Bioethanol production and pervaporative separation
3.3.1. Bioethanol production by the fermentation
In general, ethanol yield reaches a maximum value as the
substrate is consumed during anaerobic fermentation. In the
fermentation of glucose as the substrate, the substrate was
completely consumed after 48 h during fermentation by S.
cerevisiae to produce 4.9% bioethanol with the yield of 94%. The
waste newspaper was fermented using the same condition with
the fermentation of glucose. The ethanol concentration was
measured to 4.1% after the 48 h fermentation.
3.3.2. Pervaporation of bioethanol produced by the fermentation
The pervaporative ethanol separation was executed at the
temperature of 40 8C in the fermentation broth. The ethanol
concentration in the product showed stable values of around
40% at 4 h or longer. At an initial stage, the ethanol ux in
Fig. 5(a) increased and reached a stable value of higher than
20 g/m
2
h at around 8 h. The value of the separation factor
showed stable values of 1012 at around 4 h or longer, as shown
in Fig. 5(b).
Table 1 shows the pervaporative separation results of
bioethanol from the fermentation of glucose. With three
repeated experiments of ethanol recovery fromthe fermentation
broth, the ethanol ux and the separation factor in the
pervaporation of bioethanol were estimated to 15.7 g/m
2
h and
9.0, respectively. The ethanol concentration in the product was
measured to be 28.5%. The resulting values somewhat lower
compared with the result for the pervaporation of the synthetic
binary solution at 5.0% in Fig. 4(a). The decrease in the
permeation performances is related to the adsorption of organics
on the membrane surface [17].
3.3.3. Pervaporation of bioethanol from fermentation of waste
newspaper
In this study, the consecutive pervaporative separation experi-
ments were carried out using the fermentation broth of waste
newspaper. Table 2 shows the pervaporative separation of
bioethanol produced by the fermentation of waste newspaper.
Like the permeation results of the bioethanol produced the
fermentation of glucose, the permeation ux and separation factor
of bioethanol produced by the fermentation of waste newspaper
decreased due to membrane fouling [24,25]. Between three
repeated pervaporation experiments, the membrane was rinsed
by the circulation of water. Then, the pervaporation of ethanol in
Table 1
Pervaporative separation of bioethanol from fermentation of glucose.
Experiments Ethanol in feed (%) Ethanol ux (g/m
2
h) Separation factor of ethanol Ethanol in product (%) Total ux (g/m
2
h)
Run 1 4.7 16.8 9.0 28.1 51.2
Run 2 4.9 15.4 8.7 29.0 48.9
Run 3 4.6 14.8 9.2 28.5 49.7
Average 15.7 9.0 28.5 49.9
(1.0) (0.3) (0.5) (1.2)
Table 2
Pervaporative separation of bioethanol from fermentation of waste newspaper.
Experiments Ethanol in feed (%) Ethanol ux (g/m
2
h) Separation factor of ethanol Ethanol in product (%) Total ux (g/m
2
h)
Waste newspaper
Run 1 4.2 13.2 7.4 24.3 49.1
Run 2 4.1 11.5 7.3 23.7 46.3
Run 3 3.8 13.0 8.9 26.1 55.0
Average 12.6 7.9 24.7 50.1
(0.9) (0.9) (1.3) (4.4)
Synthetic solution
a
Before 4.9 13.5 7.2 27.2 49.8
After 4.7 15.4 8.0 28.4 54.3
a
The synthetic solution is the binary mixture of water and ethanol.
Table 3
Comparison of the process performance in the pervaporation of PDMS membrane.
Thickness (mm) Temp. (8C) Ethanol (wt%) Flux (g/m
2
h) Separation factor Ref.
40 5.0 (synthetic solution) 16 11 This work
91 40 4.7 (bioethanol)
a
16 9
40 4.0 (bioethanol)
b
13 8
128 30 3.0 (synthetic solution) 10 2 [13]
87 50 5.0 (synthetic solution) 236 25 [26]
200 25 10.0 (synthetic solution) 193 9 [27]
a
Bioethanol was produced by the fermentation of glucose.
b
Bioethanol was produced by the fermentation of wastepaper.
L.T.P. Trinh et al. / Journal of Industrial and Engineering Chemistry 19 (2013) 19101915 1914
the binary mixture of ethanol and water was executed and the
permeation results to investigate the inuence of the membrane
fouling on the permeation performance. As shown in Table 2,
the membrane fouling could be easily removed by a simple water
rinsing method and the pervaporation performance could be
restored, as well, as reversible membrane fouling [18].
Table 3 compared the pervaporation results of bioethanol
produced by the fermentation of waste newspaper and glucose
and synthetic solutions of binary mixture of ethanol and water.
As shown in the table, the permeation ux and the separation
factor slightly decreased due to chemical species in the
fermentation broth. In the analysis result of fermentation broth,
the concentration of xylose and acetic acid was measured to
1.28 (0.03) g/L and 0.42 (0.02) g/L, respectively. The pervapora-
tion results of PDMS membrane in this study showed relatively
good performance when the pervaporation performance of the
present study was compared with the reported results. In the
study, the pervaporative separation of bioethanol from the
fermentation of waste newspaper was carried out without any
signicant decreasing process performance.
4. Concluding remarks
In this study, a hydrophobic polymeric polydimethylsiloxane
(PDMS) membrane was used for the pervaporative separation of
bioethanol from the fermentation of glucose and waste newspa-
per. In the preliminary study, the ethanol ux in the synthetic
model solution of ethanol and water increased as the temperature
increased due to increased swelling capacity and weak water
adsorption on the membrane surface. Ethanol ux showed a
strong dependence on feed concentration due to solution-
diffusion mechanism. The pervaporative separation of bioethanol
from the fermentation of waste newspaper showed decreased
values due to the organic deposition. However, the pervaporation
performance could be restored by a simple water rinsing method
as reversible fouling. The study showed that the hydrophobic
pervaporation membrane could be used for the pervaporative
separation of bioethanol from the fermentation of waste
newspaper without any signicant decreasing process perfor-
mance.
Acknowledgement
This research was supported by the Bio-industry Technology
Development Program (Project No. 112034-1), Ministry for Food,
Agriculture, Forestry and Fisheries, Republic of Korea.
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