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Investigation of Dip-Coating Parameters Effect on The Performance of

Alumina-Polydimethylsiloxane Nanofiltration Membranes for Desalination

Article · October 2017

DOI: 10.22090/jwent.2017.04.002

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J. Water Environ. Nanotechnol., 2(4): 235-242 Autumn 2017

RESEARCH
ORIGINAL ARTICLE
RESEARCH PAPER

Investigation of Dip-Coating Parameters Effect on The

Performance of Alumina-Polydimethylsiloxane Nanofiltration
Membranes for Desalination
Mohammad Hadi Yousefi, Mohamad Mahdi Zerafat*, Majid Shokri Doodeji, Samad Sabbaghi

Faculty of Advanced Technologies, Nano Chemical Engineering Department, Shiraz University, Shiraz, Iran
1

Received: 2017-04-07 Accepted: 2017-05-10 Published: 2017-10-15

ABSTRACT
The objective of this work is to investigate the effect of dip-coating parameters on the performance
of Alumina-PDMS hybrid nanofiltration membranes for water desalination. Ceramic supports used
in this work were prepared with a 340 nm average pore size and 34% total porosity. The aim is to
determine optimum conditions of dipping time, PDMS concentration, and withdrawal speed in
order to achieve high rejection and flux values. Dip-coating parameters were considered as dipping
time (60 - 120 s), withdrawal speed (5 - 15 mm/s) and PDMS concentration (10 - 20 wt. %). Hybrid
membranes were characterized using FE-SEM and FTIR analysis techniques. Pure water flux and
salt rejection were also measured to evaluate the rejection performance. Alumina-PDMS hybrid
nanofiltration membranes fabricated with dipping time = 120 s, withdrawal speed = 15 mm/s and
10 wt. % PDMS exhibited the best performance giving 30.5% rejection for NaCl and 53.8% for
Na2SO4.

Keywords: Alumina; Dip-Coating; Hybrid Membranes; Nanofiltration; PDMS

How to cite this article

Yousefi MH, Zerafat MM, Shokri Doodeji M, Sabbaghi S. Investigation of Dip-Coating Parameters Effect on The
Performance of Alumina-Polydimethylsiloxane Nanofiltration Membranes For Desalination. J. Water Environ.
Nanotechnol., 2017; 2(4): 235-242. DOI: 10.22090/jwent.2017.04.002

INTRODUCTION
Membrane separation processes have found performance under solvent resistant conditions,
several applications in various industrial processes. i.e. improving chemical and mechanical stability,
Nanofiltration with a low energy consumption reducing swelling effects of polymeric membranes
can be a good alternative for separation purposes and enhancement of solvent affinity [2]. Hybrid
as a pressure driven membrane-based process membranes can be prepared using ceramic
intermediate between reverse osmosis (RO) and substrates and polymeric top layers through sol-gel
ultrafiltration (UF), rejecting very small moieties dip-coating [3, 4], spray coating [5], self-assembly
due to relatively high charge and pores smaller than [6], grafting [7] and spin coating [8]. Among
2 nm [1]. these, dip-coating as a simple and inexpensive
Inorganic-organic hybrid nanofiltration technique is considered as one of the most desirable
membranes can have advantages such as selectivity, alternatives. Dip-coating provides opportunities to
high flux as well as chemical and thermal resistance explore the impact of coating parameters such as
with mechanical stabilities under pressures up to 20 polymer concentration and dipping time during
bar. Much focus is devoted to the development of the fabrication procedure to obtain a membrane
new classes of membranes for improving filtration with the desired pore diameter and flux-rejection
* Corresponding Author Email: [email protected] combination [9].

This work is licensed under the Creative Commons Attribution 4.0 International License.
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 M.H. Yousefi et al. / Effect of Dip-coating Parameters on Hybrid NF Membranes

Various polymers are used as the top layer of linking agent to create a dense network structure
hybrid ceramic-polymer membranes. PDMS with grafted inside the ceramic pores. Grafting reactions
a unique set of characteristics including high free were successfully carried out and approved by
volume, backbone flexibility, thermal and chemical permeability-rejection tests. Coupling agents were
stability, hydrophobicity and solubility in non-polar found to create network structures with a higher
solvents [10], is among polymers used as the thin density grafted in the γ-alumina pores [24]. Nandi
selective layer in different membrane processes et al. prepared CA–ceramic composite membranes
like pervaporation [11] and thin film composite using the dip-coating technique. Ceramic supports
(TFC) nanofiltration [2, 12]. PDMS membranes were prepared from kaolin with an average pore size
are mostly prepared on polymeric supports such as of 560 nm and total porosity of 33%. Dip-coating
polyethersulfone (PES) [13], polyethylene (PE) [14], parameters were the concentration of CA solution
polysulfone (PS) [15], cellulose acetate (CA) [16], (2-8 wt.%) in acetone and dipping time (30-150 s) [9].
poly(vinylidene fluoride) [17], polyetherimide (PEI) In this study, hybrid nanofiltration membrane
[18], polyacrylonitrile (PAN) [19] and polyamide preparation using dip-coating is performed for
(PA) [20], although ceramic supports are also utilized. investigation of dip-coating parameters. Low-cost
For example, Hong et al. carried out pervaporation ceramic supports were prepared using α-alumina
of IPA and water using PDMS/ceramic composite powder as the raw material [25]. According to previous
membranes prepared via dip-coating. The variation studies, alumina-PDMS hybrid membranes are used
of selectivity and flux at various feed compositions for pervaporation [21, 26] and SRNF [2]. However,
and operating temperatures was explained through this study is devoted to desalination for investigating
plasticization by IPA and capillary condensation the dip-coating parameters (dipping time, withdrawal
of water [21]. Song & Hong fabricated cellulose speed) and PDMS concentration in n-heptane in order
acetate–ceramic membranes by dip-coating and to optimize the membrane performance regarding
rotation drying technique using a ceramic support flux and rejection of inorganic salts.
with a 100 nm surface average pore size and CA
concentration of 20% tested for dehydration of EXPERIMENTAL
ethanol and isopropanol [8]. Xiangli et al. prepared Materials and Methods
a PDMS/ceramic composite membrane for α-Alumina (Al2O3), Polyvinyl alcohol (PVA),
pervaporation. The results showed that polymer n-heptane, Tetraethyl orthosilicate (TEOS) and
concentration was the most significant variable dibutyltin dilaurate were purchased from Merck
influencing permeation and selectivity. Maximum Co. and used as received. Hydroxy terminated
flux of 19.5 kg m-2 h-1 was obtained under following polydimethylsiloxane (PDMS) was obtained
preparation conditions: polymer concentration = from Sigma-Aldrich (Mw= 18000 g mol-1) and a
7.4wt%, crosslink agent concentration = 10wt.% kinematic viscosity of 750 cSt. Sepahan Irman Tech
and dip-coating time = 60 s [22]. Kim et al. coated dip-coater (Iran) was also used for film application.
PDMS on a polysulfone (PSF) support for propylene
recovery from off-gas stream. They prepared a novel Characterization
organic-inorganic composite membrane by adding Surface and cross-section morphologies of the
silica nanoparticles to the PDMS solution and the composite membranes were characterized by SEM
results showed enhanced separation factor and and FE-SEM. Samples were dried under vacuum
propylene permeance enhancement from 5.2 to 7.3 at 25 °C for 40 min and coated with gold before
and 31 to 36 GPU, respectively (1 GPU equals 10−6 SEM imaging. The chemical composition of the top
cm3/cm2 s cmHg) [23]. layer of the modified support or the Al2O3/PDMS
Polysiloxane-based polymers like PDMS have composite NF membrane was characterized using
often been used as polymeric SRNF [2, 10]. Pinheiro ATR-FTIR technique.
et al. designed a new fabrication method for grafting
PDMS on a supported γ-alumina membrane (pore Support Preparation
size = 5 nm) using polysiloxane mono(2,3 epoxy) The substrate is prepared through dry casting
polyether terminated polydimethylsiloxane:(PDMS) technique (Fig. 1). A proper amount of alumina
[2]. Tanardi et al. described grafting of mesoporous powder is mixed with a 7 wt% PVA solution. The
alumina membranes with hydride terminated suspension is pressed in a template, then sintered at
polydimethylsiloxane with vinyltriethoxysilane 1250 ºC for 2 h [3].

236 J. Water Environ. Nanotechnol., 2(4): 235-242 Autumn 2017

 M.H. Yousefi et al. / Effect of Dip-coating Parameters on Hybrid NF Membranes

Preparation of composite membrane Flux and rejection experiments

PDMS/ceramic composite membranes were Rejection performance tests were conducted
prepared by the conventional dip-coating method. with a cross-flow membrane module at 20 °C. The
PDMS was dissolved in n-heptane and then the schematic diagram of the apparatus is shown in Fig. 2.
crosslinking agent (TEOS) and 0.2 wt% catalyst At steady state, the weight of permeate collected
dibutyltin dilaurate were added to the polymer in the flask was measured to obtain the total flux, (J):
solution. The polymer mixture was stirred at V
room temperature for 30 min and degassed J= (1)
A × t
under vacuum. The outer surface of the ceramic
Where V is the total mass permeated during the
support was polished with 600 mesh sandpaper
experiment time interval t and A is the effective
and washed several times with deionized water
membrane area.
under ultra-sonication and dried in open air
Feed and permeate salt concentrations were
at room temperature. Nomenclature of various
measured using electric conductivity meter
composite membranes fabricated with varying
(Ecomet conductivity meter C65) in order to
PDMS concentration in n-heptane (10 – 20 wt. %),
calculate the salt rejection according to:
dipping time (60 – 120 s) and withdrawal speed (5
–15 mm/s) are presented in Table 1. Cs − Cd
α = × 100% (2)
Cs
Where, Cs and Cd denote the salt concentrations
of feed and permeate.

RESULTS AND DISCUSSION

Membrane morphology
Fig. 3 shows the FE-SEM image of the alumina
substrate, showing a dense and uniform structure
preventing crack formation at high operating
pressures.
FE-SEM micrograph of the hybrid alumina-

Table 1: Nomenclature of different fabricated PDMS/ceramic

Table 1
composite membranes.
Dipping PDMS conc. Withdrawal
Sample
Time (s) (wt%) speed (mm/s)
M1 60 10 15
M2 120 10 15
M3 120 20 15
Fig. 1: Schematic of Dry pressing process. M4 120 20 5

Fig.1

Fig. 2: Schematic diagram of membrane modal apparatus for membrane performance tests: (1) feed tank, (2)
pump, (3) Pressure valve, (4) valves, (5) Pressure gauge, (6) membrane module, (7) permeate flask.

Fig.2
J. Water Environ. Nanotechnol., 2(4): 235-242 Autumn 2017 237
 M.H. Yousefi et al. / Effect of Dip-coating Parameters on Hybrid NF Membranes

PDMS membrane (M2) substrate structure is given stretching of methyl (CH3-) groups of PDMS. The
in Fig. 4 which confirms PDMS coating on the strong peak at 1245 cm-1 is caused by symmetric
substrate surface. C–H bending and peaks at 871 cm-1 and 791 cm-1
are caused by Si–C vibration and CH3 rocking
ATR-FTIR ANALYSIS from the SiCH3 group. The two peaks at 1095 and
The modified support and hybrid NF membranes 1017 cm-1 are ascribed to the Si–O–Si bond. These
(M2) were characterized using ATR-FTIR (Fig. 5). peaks at 791, 1017, 1095, 1245 cm-1 and 2968 cm-1
The peaks at 2968 cm-1 and 2924 cm-1 are ascribed confirm the presence of polydimethylsiloxane
to C–H asymmetric stretching and symmetric groups on the α-Al2O3/PDMS membrane [4, 27].

(a) (b)
Fig. 3: FE-SEM images of alumina support membrane: (a) top surface image, (b) cross-section image.

Fig. 3

(a) (b)
a b
Fig. 4: FE-SEM image of Alumina/PDMS hybrid nanofiltration membrane (M2). (a) Top view, (b) Cross-section view.

Fig. 3
238 FIG.4
J. Water Environ. Nanotechnol., 2(4): 235-242 Autumn 2017
 M.H. Yousefi et al. / Effect of Dip-coating Parameters on Hybrid NF Membranes

Effect of dip-coating parameters the membrane support at 0.6 MPa operating pressure
Dip time and withdrawal speed are investigated which is in agreement with Gestel’s data for inorganic
as well as polymer concentration. The variations of composite membranes [28]. Fig. 6 shows the effect of
parameters are given in Table 2 with their relative pressure on pure water flux of hybrid nanofiltration
rejection characteristics. High dip time and low membranes with different dip-coating parameters.
polymer concentration are needed to obtain high Pure water flux for both support and Hybrid NF
salt rejection. At 120 s dip time and 10 wt. % membrane exhibits a linear relationship with pressure
polymer concentration and 15 mm/s withdrawal and pure water flux is enhanced by increasing the
speed the highest rejection is obtained as 30.5% for operating pressure [29].
NaCl and 53.8% for Na2SO4.
Feed concentration
Pure water fluxes Salt concentration can influence the rejection
Fig. 6 shows that pure water fluxes of the membrane performance of hybrid membranes [1]. Fig. 7 shows
support and hybrid NF membrane vary with the the effect of feed concentration on the rejection for
operating pressure. Pure water flux is 81 L m−2 h−1 for single salt NaCl and Na2SO4 solutions. All filtration

Fig. 5: ATR-FTIR absorbance spectra of (a) alumina substrate, (b) Alumina/PDMS hybrid nanofiltration membrane (M2).

80 Fig. 5 60
70 Na2SO4 NaCl
pure water fluxes (L m-2h-1)

50
60
40
50
Rejection %

40 30
M1-60-10-15
M2-120-10-15
30 M3-120-20-15 20
support membrane
20
10
10

0 0
0.08 0.16 0.24 0.32 0.4 0.48 0.56 0.64 0 0.02 0.04
Operating pressure (MPa) Concentration (mol.L-1)
Fig. 6: Effect of operating pressure on pure water flux. Fig. 7: Effect of feed concentration on the rejection performance.

Fig.7
Fig. 6
J. Water Environ. Nanotechnol., 2(4): 235-242 Autumn 2017 239
 M.H. Yousefi et al. / Effect of Dip-coating Parameters on Hybrid NF Membranes

measurements were conducted at 0.5 MPa based Membrane performance for salt rejection
on M2-120-10-15 dip-coating parameters. In Figs. 8, 9 and10 show the effect of operating
0.0001–0.04 mol L-1 concentration range, alumina- parameters on the salt rejection of the composite
PDMS membrane exhibited higher retention NF membranes for NaCl and Na2SO4 solutions. All
rates toward di-valent cations compared to the filtration measurements were conducted at feed
mono-valent cation. Decreased rejection with salt concentration = 0.001 mol L-1.
concentration can be explained by the decreased Fig. 8 shows the rejection of Na2SO4 and NaCl
thickness of the electric double layer with increased increased from 45.8 to 53.8 and 23.7 to 30.5 while
salt concentration (i.e. higher ionic strength) and dipping time was increased from 60 (M1-60-10-
hence lower rejection rates [30, 31]. 15) to 120 s (M2-120-10-15). This salt rejection

Table 2
Table 2: Dip-coating parameters and rejection of membranes at 0.6 MPa operating pressure.
Dipping Polymer Withdrawal Rejection Rejection
Number
time (s) concentration (wt%) speed (mm/s) Na2SO4 (%) NaCl (%)
M1 60 10 15 49.1 27.2
M2 120 10 15 53.8 30.5
M3 120 20 15 46.1 22.1
M4 120 20 5 50.1 27

60 60

50 50

40 40

NaCl R%
Na2SO4 R%

30 30

20 20

10 10

0 0
0 0.1 0.2 0.3 0.4 0.5 0.6
Operating pressure (MPa)
Fig. 8: Effect of operating pressure (MPa) and dip-coating parameter on the Rejection%.
Fig. 8

60 60

50 50

40 40
Na2SO4 R%

NaCl R%

30 30

20 20

10 10

0 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Operating pressure( MPa)
Fig. 9: Effect of operating pressure (MPa) and dip-coating parameter on the Rejection%.
Fig.9

240 J. Water Environ. Nanotechnol., 2(4): 235-242 Autumn 2017

 M.H. Yousefi et al. / Effect of Dip-coating Parameters on Hybrid NF Membranes

60 60

50 50

40 40
Na2SO4 R%

NaCl R%
30 30

20 20

10 10

0 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
Operating pressure( MPa)
Fig. 10: Effect of operating pressure (MPa) and dip-coating parameter on the Rejection%.
Fig. 10

enhancement can be due to the increased polymer NF membrane, rejection of 30.5% for NaCl and
coating on the ceramic membrane resulting in rejection of 53.8% for Na2SO4 are obtained.
smaller porosity and pore sizes in the hybrid
membrane. So, due to sieving mechanism, salt ACKNOWLEDGEMENTS
rejection is increased [9]. Thanks to Iran National Science Foundation
Fig. 9 shows the rejection of Na2SO4 and NaCl (INSF) for financial support of the project.
increasing from 46.1 to 53.8 and 22.1 to 30.5 when
the polymer concentration was reduced from 20 CONFLICT OF INTEREST
wt.% (M3-120-20-15) to 10 wt% (M2-120-10-15). The authors declare that there are no conflicts
So, increasing the polymer solution concentration of interest regarding the publication of this
results in the reduction of salt rejection. manuscript.
According to Fig. 10, rejection of Na2SO4 and
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