Journal of Membrane Science 375 (2011) 6368

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Journal of Membrane Science

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

Nanoporous polyethersulfone (PES) membrane with enhanced ux applied in

forward osmosis process
Youngbeom Yu a , Sunkeun Seo a , In-Chul Kim b , Seockheon Lee a,
a
b

Korea Institute of Science and Technology, Water Environment Center, 39-1 Hawolgok-dong, Seongbuk-gu, Seoul 136-791, South Korea
Korea Research Institute of Chemical Technology, Environment & Resources Research Center, 100 Jang-dong, Yuseong-gu, Daejeon 305-343, South Korea

a r t i c l e

i n f o

Article history:
Received 29 August 2010
Received in revised form 15 February 2011
Accepted 15 February 2011
Available online 22 February 2011
Keywords:
Polyethersulfone
Nanoporous
Forward osmosis membrane
Water ux
Reverse solute ux

a b s t r a c t
A forward osmosis (FO) membrane process uses the natural phenomenon of osmosis, which occurs when
two solutions of differing concentration are placed on opposite sides of a semipermeable membrane.
Therefore, osmotic pressure is highly inuenced by the properties of the semipermeable membrane in
an FO membrane process. In this study, the properties of commercial polyamide (PA) and cellulose triacetate (CTA) membranes were analyzed, and the water ux and reverse solute ux were evaluated
in FO mode. The major properties of an FO membrane that enhance its performance are its thickness,
hydrophilicity, and structure. This work developed a high-performance polyethersulfone (PES) membrane for FO membrane process applications. The PES membrane consists of an active layer formed atop
a support layer that includes a backing lled with polymer. The water ux was maximized by forming a
loose nger-like structure and generating nano-sized pores to increase porosity. The reverse solute ux
was minimized by maintaining the thickness of the support layer including the backing. The performance
of the PES membrane was compared with that of commercial HTI-CTA membrane. The properties of the
PES membrane attributed to the high water ux and low reverse solute ux.
2011 Published by Elsevier B.V.

1. Introduction
Pressure-driven membrane processes such as reverse osmosis (RO) are widely used in seawater desalination and wastewater
reuse [17]. However, forward osmosis (FO) is a potential alternative to pressure-driven membrane processes and has been gaining
popularity in recent years [818]. The FO process is a water treatment technology using osmotic pressure. It is expected to save
more energy than the RO process, which uses hydraulic instead of
osmotic pressure. However, adequate membranes for use in the FO
process have not yet been developed. In addition, there are challenging problems, including the method for recovering the draw
solution. Therefore, it is difcult to apply the FO process to water
treatment at the present time. If its problems are solved, however,
the FO process has the potential to become an alternative to the RO
membrane process.
Osmotic pressure occurs when two solutions with different
concentrations are placed on opposite sides of a semipermeable
membrane. For the FO process, the difference between the concentrations of the two solutions has a large effect on osmotic
pressure. In addition, the osmotic pressure can be inuenced by

Corresponding author. Tel.: +82 2 958 5829; fax: +82 2 958 5839.
E-mail address: seocklee@kist.re.kr (S. Lee).
0376-7388/$ see front matter 2011 Published by Elsevier B.V.
doi:10.1016/j.memsci.2011.02.019

the properties of the semipermeable membrane. Therefore, many

researchers have studied the physical and chemical properties of
membranes that maximize osmotic pressure [1927]. The major
membrane properties that affect osmotic pressure are the thickness, hydrophilicity, and structure of the membrane. In addition,
the reverse solute ux also has an effect on osmotic pressure. Permeating the draw solution into the feed solution prevents the FO
process from operating because the reverse solute ux is one of the
factors that diluted draw solution decreases osmotic pressure. In
this study, the water ux and reverse solute ux were evaluated
with respect to the properties of a commercial CTA-FO membrane
and a PA-RO membrane. A nanoporous PES membrane was then
developed and evaluated against the commercial membranes.
2. Materials and methods
2.1. Chemicals and membranes
Polyethersulfone (PES, BASF, Germany) was used as polymer. 1-methyl-2-pyrrolidinone (NMP, anhydrous, 99.5%), N,Ndimethylformamide (DMF, anhydrous, 99.8%) were used as solvent.
1,3-Dioxolane, polyvinylpyrrolidone (PVP), and polyethyleneglycol (PEG) were used as additive. Sodium chloride (NaCl, powder,
99.5%) was used as the solute of the draw solution. Polyester nonwoven fabric (PET, Sanko, Japan) was used as a backing for the
PES supports. Two kinds of commercial asymmetric cellulose tri-

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Y. Yu et al. / Journal of Membrane Science 375 (2011) 6368

acetate forward osmosis membranes (CTA, Hydration Technology

Innovations LLC, USA) were used as a membrane of CTA material.
One of them uses mesh as a backing, and the other uses fabric as
a backing. Two kinds of commercial thin-lm composite seawater reverse osmosis membranes (TM-820, Toray, Japan) were used
as a membrane of PA material. One of them is original and the
other is modied by removing PET. The micrographs of the membranes were obtained utilizing a eld emission scanning electron
microscope (FE-SEM) (NOVA NanoSEM200, FEI Company, USA). The
contact angle measurements were performed with a goniometer
(DM 500, Kyowa Interface Science, Japan). The equilibrium contact
angle measurements are based on the measurements described by
Marmur [28].
2.2. Casting of PES-FO membrane
PES was dissolved in a solvent of NMP and DMF and additives of
1,3-dioxolane, PVP, PEG. The polymer solution was stirred at room
temperature (20 C) for 24 h. The PET nonwoven fabric was attached
to a clean glass plate using laboratory adhesive tape. A casting knife
(YBA-5, Yoshimitsu, Japan), set at a gate height of 150 m, was
used to spread the PES solution onto the PET nonwoven fabric. The
whole composite was immediately immersed in a nonsolvent bath
and was allowed to sit in a nonsolvent bath for 24 h. The PES-FO
membranes were stored in deionized (DI) water at 4 C replaced
regularly prior to the experiments.
2.3. Synthetic wastewater
Glucose (C6 H12 O6 , 98%), ammonium sulfate ((NH4 )2 SO4 , 99%),
potassium nitrate (KNO3 , 99%), and dipotassium hydrogenphosphate (K2 HPO4 , 98%) were used as solute of synthetic wastewater.
Total organic carbon (TOC), total nitrogen (TN), and total phosphorous (TP) were measured in the synthetic wastewater. The water
quality of synthetic wastewater is shown in Table 1.

Table 1
Water qualities of the synthetic wastewater.
Parameter

TOC

TN

TP

Conc. (mg/L)

54.61

16.26

3.06

The TOC was measured with a total organic carbon (TOC) analyzer (TOC-VCPH, Shimadzu, Japan). The TN and TP were measured
in accordance with standard methods (Standard Method 4500-N C.
and 4500-P J.) [29].
2.4. Lab-scale FO membrane performance systems
The FO membrane test unit consists of a at-sheet type membrane cell, two gear pumps (Cole Parmer, USA), the feed and draw
solution reservoirs, a magnetic stirrer (Thermo scientic, USA), a
water bath circulator (JS Research Inc., Republic of Korea), a digital scale (CAS, Republic of Korea), and a digital conductivity meter
(HACH, USA). In the FO membrane test unit, the feed and draw
solution are each held in a 2 L reservoir and fed to the membrane cell by the gear pumps. The draw solution was 3 M NaCl.
The draw solution reservoir was placed on a digital scale, and the
weight changes were monitored by a computer to record the permeate ux. The membrane cell, which contains equally structured
channels on both sides of the membrane, was placed in a rectangular channel with cell dimensions of 77 mm 26 mm 3 mm. No
spacer was used in the channel for the membrane performance
experiments. The cross-ow velocity was 8.5 cm/s. The feed and
draw solution temperatures were controlled by the water bath
at approximately 20 C. The water bath temperature was maintained by circulating chilled water through a stainless-steel coil
immersed in a water bath. A digital conductivity meter was placed
in the feed and draw solution reservoirs, and the conductivity
changes were monitored by a computer to record the reverse solute
ux.

Fig. 1. SEM micrographs of the cross-section of the commercial PA-RO and CTA-FO membranes: (a) fabric-PA, (b) no fabric-PA, (c) fabric-CTA, (d) mesh-CTA.

Y. Yu et al. / Journal of Membrane Science 375 (2011) 6368

65

3. Results and discussion

3.1. Properties of commercial PA and CTA membranes
Fig. 1 shows the cross-sectional SEM micrographs of two commercial PA and two commercial CTA membranes. Fig. 1(a) and (c)
shows the micrographs of PA and CTA membranes in which fabric
was used as the backing. In these gures, the thickness of the membrane was about 150 m. Fig. 1(b) shows the micrographs of the PA
membrane after the fabric backing was removed. Fig. 1(d) shows
the micrographs of the CTA membrane in which mesh was used as
the backing. In these gures, the thickness of the membrane was
about 50 m.
The commercial PA and CTA membranes were characterized in
terms of surface contact angle, thickness, and structure. The results
are summarized in Table 2.
3.2. Water ux and reverse solute ux with respect to membrane
properties
Fig. 2 shows the water ux and reverse solute ux of two commercial PA membranes and two commercial CTA membranes. A 3 M
NaCl solution was used as a draw solution, and DI water was used as
feed water. The water ux and reverse solute ux were monitored
every 3 min for 20 h.
Fig. 2(a) shows the water ux and reverse solute ux of PA
membranes with or without a fabric backing. The fabric-PA membrane and no fabric-PA membrane have the same hydrophilicity.
The no fabric-PA membrane is thinner than the fabric-PA membrane because the fabric used as a backing is removed. The water
ux and reverse solute ux increased 2- and 10-fold, respectively,
by reducing the thickness of the 100 m backing. When the feed
solution is placed against the active layer and the draw solution
against the backing layer, the internal concentration polarization
(ICP) phenomenon, in which the draw solution is diluted by the
permeate water within the support layer of the membrane, occurs
on the permeate side [3033]. For the fabric-PA membrane, this
diluted draw solution is present at the boundary of the active and
support layers. Therefore, both the reverse solute ux and water
ux also decrease by the diluted draw solution. Although reducing
the thickness of the backing can increase the water ux, this also
increases the reverse solute ux. The reverse solute can negatively
inuence the FO process. First, the reverse solute ux can cause the
water ux in the FO process to decrease because the draw solution
is diluted by the reverse solute ux. Second, if the FO membrane
is submerged in a bioreactor, a draw solute can be concentrated
on the bioreactor by the reverse solute ux. The reverse solute ux
must be minimized in order to improve the operation of the FO
process. Consequently, reducing the thickness of the backing is not
an ideal method for developing FO membranes.
Fig. 2(b) shows the water ux and reverse solute ux of the
fabric-PA and fabric-CTA membranes. These membranes have the
same backing, as well as a similar membrane thickness of about
150 m. The contact angle values of the two membranes were
72.20 and 52.88, respectively. This means that the two membranes
have different hydrophilicities; specically, the fabric-CTA membrane is more hydrophilic than the fabric-PA membrane. Given

Fig. 2. Water ux and reverse solute ux of the commercial PA-RO and CTA-FO
membranes: (a) a comparison of experimental results on fabric-PA and no fabric-PA,
(b) on fabric-PA and fabric-CTA, (c) on no fabric-PA and mesh-CTA.

Table 2
Characteristics of commercial PA-RO and CTA-FO membranes.
Parameter

Contact angle ( )
Thickness (m)
Structure of backing

PA-RO

CTA-FO

Fabric-PA

No fabric-PA

Fabric-CTA

Mesh-CTA

72.20
150
Fabric

72.20
50
No fabric

52.88
150
Fabric

73.70
50
Mesh

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Y. Yu et al. / Journal of Membrane Science 375 (2011) 6368

Fig. 3. Schematic diagram of the PES-FO membrane.

that the contact angle value of the membrane surface decreased

by 25%, the water ux increased by about 4-fold; there was no
remarkable difference in the reverse solute ux. The reverse solute
ux was determined by the membrane structural parameter and
active-layer salt permeability coefcient, both of which are related
to the porosity, tortuosity, and thickness of the membrane [34].
The fabric-PA and fabric-CTA membranes are observed to have a
similar tortuosity, and thickness of the membrane in the crosssectional SEM micrographs of Fig. 1. This suggests that the two
membranes have a similar reverse solute ux. When a membrane
surface becomes more hydrophilic, the water ux can increase
without a further increase in the reverse solute ux. Therefore,
increasing the hydrophilicity of a membrane surface is better than
reducing the thickness of the membrane backing, because it can
selectively increase the water ux without increasing the reverse
solute ux.
Fig. 2(c) shows the water ux and reverse solute ux of the no
fabric-PA and mesh-CTA membranes. These membranes have similar hydrophilicities and thicknesses (50 m). As shown in Fig. 1, the
two membranes have differently structured layers. The layer of the
no fabric-PA membrane has a very dense sponge-shaped structure
[Fig. 1(c)]. On the other hand, the layer of the mesh-CTA membrane
has a very loose nger-shaped structure [Fig. 1(d)]. Whereas the
sponge-shaped structure signicantly increased the resistance to
mass transfer, the nger-shaped structure decreased it [35]. As the
layer of the mesh-CTA membrane had a nger-like shape, the water
ux increased 2-fold; there was no marked difference in the reverse
solute ux. In this case, the water ux can increase without a further
increase in the reverse solute ux. Therefore, the ideal method for
increasing the water ux and minimizing the reverse solute ux is
to maintain an adequate thickness of the membrane backing, make
the membrane surface more hydrophilic, and create layers with a
nger-shaped structure.
3.3. Concept and characterization of the nanoporous PES-FO
membrane
Fig. 3 shows a schematic diagram of the structural concept of the
PES-FO membrane. This membrane is fabricated with a backing and
a polymer solution. Fabric is used as the backing. PES, solvent, and
additives are used for the polymer solution. The PES-FO membrane
consists of active and support layers. The active layer has a ngerlike shape and includes the top layer. The top layer has a dense
sponge-like structure with nano-sized pores. The support layer is
formed by lling the backing with the polymer solution.
Fig. 4 shows the SEM micrographs of both morphologies of
the active surface and a cross-section of the PES-FO membrane.
The micrograph in Fig. 4(a) shows that the active surface of the

Fig. 4. SEM micrographs displaying the structure of the PES-FO membrane at the (a)
top surface of the active layer, (b) cross-section including PET nonwoven fabric and
(c) a magnied view of the dense, sponge-like morphology near the active layer.

PES-FO membrane has valley morphology. The top surface of the

PES-FO membrane has nano-sized pores. The PES-FO membrane
has a larger pore size than the commercial FO and RO membranes.
Pore size has an effect on the removal rate, the results of which
will be explained in detail in the next section. Fig. 4(b) and (c)
shows micrographs of the morphology of a cross-section on the

Y. Yu et al. / Journal of Membrane Science 375 (2011) 6368

67

Table 3
Characteristics of developed PES-FO membrane.
Membrane

Contact angle ( )

Thickness (m)

Structure of backing

PES

82.60

150

Fabric

PES-FO membrane. The average thickness of the membrane is about

150 m. The top layer (12 m) of the active layer has a dense
sponge-like morphology. Although this top layer rejects foulants,
it hinders the water ux. The active layer below the top layer has
a nger-like morphology. The nger-shaped structure decreases
the resistance to water ux. N,N-dimethylformamide (DMF) and
1-methyl-2-pyrrolidinone (NMP) were used as solvents for the PESFO membrane. The pore morphology is determined by the polymer
precipitation rate; slow precipitation produces sponge-like pores,
and rapid precipitation produces nger-like pores [36,37]. Given
that DMF precipitates slowly, it forms the sponge-like top layer of
the PES-FO membrane. In contrast, NMP precipitates rapidly, and
thus forms the nger-like active layer.
On the other hand, 1,3-dioxalane, polyvinylpyrrolidone (PVP),
and polyethyleneglycol (PEG) were used as additives for the PESFO membrane. After casting the polymer solution on the backing,
it was placed in a nonsolvent (water) bath. The solvents and additives were removed from the nonsolvent bath to form membrane
pores. 1,3-Dioxalane is highly volatile. Given that it volatilizes faster
than the solvent in the nonsolvent bath, it has a much smaller
pore size. In addition, PEG and PVP increase the viscosity of the
polymer solution. A polymer solution with high viscosity forms a
denser membrane structure in the nonsolvent bath. Therefore, 1,3dioxalane, PEG, and PVP induce the formation of nano-sized pores
on the top layer of the PES-FO membrane.
The PES-FO membrane was characterized in terms of surface
contact angle, thickness, and structure. The results are summarized
in Table 3.
3.4. Performance of the nanoporous PES-FO membrane
Fig. 5 shows the water ux and reverse solute ux of the meshCTA and PES-FO membranes. A solution of 3 M NaCl was used as a
draw solution, and DI water was used as feed water. The water ux
and reverse solute ux were monitored every 3 min for 20 h. The
PES-FO membrane achieved a water ux nearly twice as high as that
of the commercial mesh-CTA membrane. Commercial mesh-CTA
membranes have smaller pore sizes than the PES-FO membrane.
Given the latter had nano-sized pores, the water ux increased
2-fold. The decrease in the reverse solute ux was 2-fold greater
than that of the commercial mesh-CTA membrane. The commer-

Fig. 6. Removal efciencies of the mesh-CTA and PES-FO membranes in synthetic

wastewater.

cial mesh-CTA membrane was quite thin, with a thickness of about

50 m. In comparison, the PES-FO membrane was about 150 m
thick. With an adequate thickness for the PES-FO membrane, the
reverse solute ux decreased about 2-fold.
From the results of Figs. 25, the factors that increase the water
ux and minimize the reverse solute ux are as follows. The key
factor that minimizes the reverse solute ux is the maintenance
of the support layer, including the backing of the membrane, at an
adequate thickness. Three factors increase the water ux: making
the membrane surface more hydrophilic, forming a nger-shaped
membrane layer, and increasing the pore size of the membrane.
These factors were incorporated in a nonporous PES membrane
to achieve high performance. The support layer of the membrane
was kept to an adequate thickness, the layer of the membrane had
a nger-like shape, and nano-sized pores were introduced in the
membrane. In order to achieve a water ux that is superior to
that of the PES-FO membrane, a polymer that is more hydrophilic
than PES should be used. Generally, polyacrylonitrile (PAN) is more
hydrophilic than PES. Future studies will need to evaluate the FO
membrane using PAN.
Fig. 6 shows the removal efciencies of the mesh-CTA and
PES-FO membranes in synthetic wastewater. For the commercial
mesh-CTA membrane, the total organic carbon (TOC) and total
phosphorous (TP) showed high removal efciencies of over 99%,
and the total nitrogen (TN) showed removal efciencies of over
96%. For the PES-FO membrane, TOC, TN, and TP achieved removal
efciencies of about 94%. The commercial mesh-CTA membrane
showed higher removal efciencies than the PES-FO membrane.
Nonetheless, the PES-FO membrane demonstrated potential to be
used as a membrane for the FO process.

4. Conclusion

Fig. 5. Water ux and reverse solute ux of the mesh-CTA and PES-FO membrane.

In this study, the properties of commercial PA and CTA membranes were analyzed, and the water ux and reverse solute ux
were evaluated in FO mode. Although reducing the thickness of
the backing can increase the water ux, this also increases the
reverse solute ux. The reverse solute ux needs to be minimized
in order to improve the operation of the FO membrane process,
as it can negatively affect the FO process. Consequently, reducing
the thickness of the backing is not an ideal method for developing
FO membranes. Increasing the hydrophilicity of a membrane surface can selectively increase the water ux without increasing the
reverse solute ux. Therefore, increasing hydrophilicity of a membrane surface is preferable to reducing the thickness of membrane.
The selective increase in the water ux also occurs when the layer
has a nger-shaped structure.

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Y. Yu et al. / Journal of Membrane Science 375 (2011) 6368

A high-performance nanoporous PES membrane was developed

for FO membrane process applications. The PES-FO membrane
achieved a water ux nearly twice as high as that of a commercial mesh-CTA membrane. The decrease in the reverse solute ux
was twice that of the commercial mesh-CTA membrane. Although
the removal efciencies were lower than those of the commercial
mesh-CTA membrane, they were greater than 94% for TOC, TN, and
TP. The performance of the nanoporous PES membrane is adequate
for the FO membrane process. An FO membrane with even better
performance might be fabricated by substituting PES with a more
hydrophilic polymer.
Acknowledgements
The authors would like to thank the Korea Institute of Science
and Technology (KIST) research project (title: Core technologies for
the wastewater reuse using membrane technology) for supporting
this study.
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