Effect of organic additive peg 600 on ultrafiltration performance of pes membranes

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© I A E M E
EFFECT OF ORGANIC ADDITIVE (PEG 600) ON
ULTRAFILTRATION PERFORMANCE OF PES
MEMBRANES
T. BALAMURALI, B. PREETHA
Department of Chemical Engineering, Annamalai University,
Annamalai Nagar, Chidambaram -608002, Tamil Nadu, India
26
ABSTRACT
The polyethersulfone (PES) is fabricated with presence of PEG in 15 to 20 wt % of composition The
pure water flux increased on addition of 2.5 wt % of PEG in all composition of PES. The increase in
flux is attributed to the surface hydrophilicity of PES and it also clearly signifies the impact of pore
architecture on PES. The mass transfer coefficient was also investigated by using protein solutions.
The average pore size, number of pores and porosity enhanced, when 2.5wt of PEG in PES.
However, the average pore size, number of pores and porosity suppressed when higher concentration
PEG dded from 19 and 20 wt%. Sugar solution concentration studies were performed wherein 27-
30 % rejection, much higher than that of PES without PEG was observed.
Keywords: Polyethersulfone; Sugar Solution Concentration; Hydrophilicity; Porosity; Water Flux
1. INTRODUCTION
The development of polymer membranes advances in the field of materials science has
created great opportunities for major progress in the field of membrane science. Polymer membranes
composed of hydrophilic materials are developing due to their higher durability and performance in
many separation applications [1, 2]. Hydrophlic materials blended or architecturally position in the
membrane matrix, are attractive because of their enhanced properties, such as high perm-selectivity,
higher hydrophilicity, and enhanced fouling resistance [3,4]. These advances have motivated for
large number of studies to explore novel membrane in the fabrication of tailor-designed polymer
properties. Inspite of high research activity in the area of blending their application in membrane
science is only slowly developing. PES is the material of choice for numerous membrane
applications due to its outstanding mechanical strength, thermal stability, and formability [5,6]. The

2. International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976
6480(Print), ISSN 0976 – 6499(99(Online), Volume 5, Issue 11, November (2014), pp.
26
main disadvantage is its low hydrophilicity and permeability leading to increased membrane fouling.
Hence, blending of PEG 600 was investigated to fabricate better membranes by increasing the
permeability by increasing the weight
weight. Barth et al. [7] has emphasised that PES, which is more
suitable le for liquid state separations.
Chakrabarty et al [8] reported the effect of PEG 400,PEG 6000
and PEG 20,000 on the morphology and performance
DMAc as solvent separately. From this work, they concluded that solvents and molecular weights of
PEG play a significant role on flux properties
NMP as solvent and PVP as an additive in the fo
showed that PVP suppresses the formation of
demixing in presence of NMP/PVP.
various compositions on membrane performance and morphology was investigated by Rahimpour et
al [10]
In the current study, PEG has been were added by varying PES/DMF ratio in membrane
casting solution followed by phase inversion method. The addition of PEG was leading to alter
properties and change in pore structure in casting solution that eventually affects membrane
formation and permeability properties.
2. EXPERIMENTAL SECTION
2.1. Materials
PES (Veradale 3000) was supplied by Solvay Solexis (India) limited.
dimethylformamide was purchased from Qualigens fine chemicals, Glaxo India limited. All
chemicals used were of analytical grade. Ultrapure water was produced in the laboratory using
Millipore pilot plant. The effluent was obtained from Seshasayee paper mills, Erode
Figure 1
2.2. Preparation of PES/PEG membrane
The 15 to 20 wt % of composition of PES were dissolved in 85 to 80 wt % of N, N’
dimethylformamide (DMF) solvent. Further the 2.5 wt % of
The solution was mixed with PES using mechanical stirring for 3 h. The detailed composition of
casting solution is described in Table 1. The homogenous casting solutions were then made into a
thin film of 400 μm thickness on a finely levelled glass plate by using a thin film applicator
(Elcometer) made of stainless steel. After leaving for partial evaporation for 30 s, the film was then
immersed rapidly into the non-solvent phase (water) maintained at 10ºC. Phase inver
membrane formation occurs at this stage and for the complete solvent exchange, the film was kept
immersed in water bath for 24 h. Later, the formed PES membranes were preserved in 1 % formalin
solution.
27
of PSf membranes prepared w
eparately. of the membranes. The work of Boom et al.
formation poly(ethersulfone) (PES) membrane
macro voids by reducing the possibility of delayed
The blend of PES/cellulose acetate phthalate (CAP) with
ane roperties ormamide 1: Chemical Structure of polyethersulfone
. PEG added in to all PES/DMF solution.
ness –
6-36 © IAEME
] with NMP and
[9] using
sulfone) N, N’-
Erode, India.
N’-
inversion method of

3. International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976 –
6480(Print), ISSN 0976 – 6499(Online), Volume 5, Issue 11, November (2014), pp. 26-36 © IAEME
A t
=
a = (5)
The average pore radius, R , can be calculated using the following equation.
100 a (6)
28
2.3. Permeability studies
Permeation studies were carried out using constant-volume, variable-pressure UF stirred dead
end flow cell (model Cell-XFUF076, Millipore, USA). Using ultrapure water, flux study has been
performed for PES membranes. The test membranes initially soaked in 70 % ethanol were taken and
mounted on the UF unit under 60 psi trans-membrane pressure (TMP). The flux readings were noted
at steady state conditions for 10 min at 25ºC. The membrane in the UF unit had an effective surface
area of 38.5 cm2. The water flux (Jw) of each membrane was quantified based on the following
equation (1):
(1)
where V, A and t are respectively the permeate volume, membrane effective area, and permeation
time.
2.4. Membrane resistance
The pure water flux of PES membranes can be used to determine their membrane resistance.
Membrane resistance (Rm) indicates the resistance offered by the membranes to the feed flow. Rm of
PES membranes are determined from the following equation (2):
P
D
m J
w w
R
×
=
h
(2)
where P is the TMP and w is the viscosity of the feed.
2.5. Pore Statistics
The average pore radius ( R ), surface porosity or porosity percentage and number of pores of
all blend membranes were determined by UF of dextran polymers of different molecular weights.
The analysis of dextran was performed with an UV spectrophotometer at max = 485 nm [11]. The
molecular weight of a solute with solute rejection percentage (%SR) greater than 80% may be used
to evaluate R with the following equations.

4. p
C
% 1 ×100
= −
f
C
SR (4)
where, Cp = concentration of permeate; Cf = concentration of feed. Average solute radii, known as
Stoke radii, can be evaluated according to the procedure developed [12]. From the values of %SR,
the average solute radius, a , was derived from the Sarbolouki equation, which is constant for each
molecular weight of dextran.
0.096 0.59 0.128 0.5 M + M
2

5. =
SR
R
%
V
J w × D

6. International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976 –
6480(Print), ISSN 0976 – 6499(Online), Volume 5, Issue 11, November (2014), pp. 26-36 © IAEME
The surface porosity, , of the membrane was calculated by the orifice model given below assuming
that only the skin layer of the membrane is effective in separation Sarbolouki et al (1982).
e (7)
= (8)
29
100
3
×
J w p μ
D
=
P R
where μ is the viscosity of the permeate water in (Pa.s), Jw is the pure water flux of the membrane in
(m3/m2.s), R is the average pore radius in (Å) and P is the transmembrane pressure in (Pa).
From the values of and R , the number of pores, n, per unit area (m2) can be calculated from
the following expression [13].
e
2 R
n
p
2.6. Mass transfer coefficient
The concentration of the solute at the membrane surface is greater than that of the bulk
resulting from concentration polarization. This can be studied using the film layer model that
assumes a zone where the concentration decreases from the membrane to the surface at a distance
inside the retentate phase. For partial retentions, the flux equation is

8. (7)
The observed retention, Robs and true retention, R are expressed as in equation (8) and (9)
respectively.

9. (8)

10. (9)
Where, Jv is volume flow per unit area and time through the membrane, m/s; k is mass transfer
coefficient, m/s; Cm is membrane concentration in contact with the high pressure interface, mol/m3;
Cp is permeate concentration, mol/m3 and Cf is feed concentration, mol/m3.
Using the equation (8) and (9) the equation (7) can be rewritten as following form.
(10)
Where, Ro is the observed retention coefficient and R is the true retention coefficient. ln [(1-Ro)/Ro]
was plotted against Jv for experiments with various membranes. The plots showed a linear fit. From
the corresponding line equation, the slope (1/ k) and intercept ln [(1-R)/R] were obtained. From
which, the mass transfer coefficient, k, and true retention coefficient, R, were determined [14].
2.7. Concentration of sugarcane juice
The sugarcane juice is obtained from vellore co-operative sugar mills ammundi. It is then
subjected to clarification by adding lime. The clear super latent liquid is taken without any
disturbance and collected in a 1000 ml measuring jar. The concentration of the total sugars in the

11. International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976 –
6480(Print), ISSN 0976 – 6499(Online), Volume 5, Issue 11, November (2014), pp. 26-36 © IAEME
feed and permeate streams were determined by collecting samples and analyzing through pol
measurement [15]. It may also be noted that on a dry basis, the total concentration of sucrose and
dextrose exceed 85 % of the total dissolved solids. The raw juice is treated with milk of lime under
constant stirring to raise the pH from around 5.0 to 8.0. The liming was carried out at room
temperature (~ 30 °C) .experiments revealed that 2.3 gram of lime was required to raise the pH to
8.0. The treated juice was then kept undisturbed for around 2 hours to facilitate the settling of solids.
The observed retention for total dissolved solids (R°TDS) and sugars(R°s) were calculated by
following equation.
° ! #
(9)
30
° ! #$

12. #$
(10)
%'()* +,
-./0 1 !22 (11)
3456 7 1 78 1 4569:;=?
@@ @AB 1 CD?9
3. RESULTS AND DISCUSSION
3.1. Effect of PES and PEG composition on water content
It is well known that the adsorbed water in membrane is beneficial for water permeation in
the membrane. However, excess water content can lead to the deterioration of mechanical strength of
the membrane due to its dissolving nature for the membrane material. As can be seen from Table 1,
the water content of the membranes decreased with increasing concentration of PES, ratio of the
membrane increased with increasing SD, owing to the increase of the hydrophilicity. The water
content of the PES membranes with PEG additive was measured and shown in Table 2
Table 1 Membrane casting composition, PWF, Water content and pore architecture of PES
membranes without PEG 600
Type PES
(%)
Solvent
(DMF)
(wt%)
PWF
(l/m2h)
Water
Content
(%)
Rm
(kPa l-1.m2.h)
R#
(Å)
N±
(×1012)
e * × 10-5
(%)
PES1 15 85 18.0 80 2.8 55 7.98 7.21
PES2 16 84 15.8 74 3.5 43 6.33 5.98
PES3 17 83 12.3 70 5.5 40 5.00 4.33
PES4 18 82 6.5 65 7.0 38 4.42 3.00
PES5 19 81 Noflux 40 -- -- -- --
PES6 20 80 No flux 35 -- -- -- --

13. International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976 –
6480(Print), ISSN 0976 – 6499(Online), Volume 5, Issue 11, November (2014), pp. 26-36 © IAEME
It was evidently seen that the water content increased with an increase of PEG amount, the
water content of all modified PES membranes was higher than that of the PES virgin membrane. It
was realized that the addition of PEG increased the porosity of the modified PES membranes, which
might be due to the addition of PEG into casting solution would be leached out to coagulation bath
and result in formation of pores, the formed pores would be filled with water. However, all the
values of PES modified membranes were lowest value when compared with CA modified
membranes
3.2. Effect of PES and PEG composition on pore architecture of membranes
In our case the addition of PEG in the dope formulation enhances performance. According to
Kesting [16], the role of additives also serves to increase the membrane water content (degree of
swelling), porosity, pore size of the membranes. It is obvious that adding small amount of PEG and
solvent (DMF)/PEG ratio enhanced the efficiency. The higher ratio of DMF/PEG (85/2.5 wt%)
indicates a lower amount of PES in the dope solutions and this apparently improved the pore
architecture of the membranes. When the amount of PEG is added in PES/DMF dope solution the
formation of nuclei having PEG rich phase takes place very slowly compared to the diffusion of non
solvent into the polymer solution so that nuclei with the high solvent concentration are absent
resulting in macrovoids suppression. However, 1 wt% increment of PES from 1wt% from 15 to 20
wt%, low viscosity dope solution containing low amount of PEG increases the precipitation rates and
this also enhanced the formation of macrovoids. The results are presented in Table 1.
Table 2 Membrane casting composition, PWF, Water content and pore architecture of PES
membranes with PEG 600
#average pore radius,±number of pores per 1 m2 area, *surface porosity
The obtained data indicate that the mean pore size of membranes decreases with increasing
the PES concentration in the casting solution up to 20/80 of polymer and solvent ratio. The pore
architecture altered to the left with the increment of PEG concentration in the casting solution. The
31
Type
PES
(%)
PEG 600
wt (%)
Solvent
(DMF)
(ml)
PWF
at 345 kPa
(l/m2h)
Water
Content
(%)
Rm
(kPa l-1.m2.h)
R#
(Å)
N
±
(×1012)
e * × 10-5
(%)
PES-P1 15 2.5 85 22 85 3.0 60 9.6 8.23
PES-P2 16 2.5 84 19 80 3.3 56 8.3 8.00
PES-P3 17 2.5 83 15 73 4.8 53 8.0 7.8
PES-P4 18 2.5 82 10 70 6.5 50 7.3 5.8
PES-P5 19 2.5 81 4.8 66 8.0 45 6.4 5.0
PES-P6 20 2.5 80 2.5 60 11.0 38 5.2 3.7

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calculated results of pore density and surface porosity of the membranes are improved by adding
PEG into the PES.
3.3. Effect of PEG 600 on mass transfer coefficient of PES membranes
In ultrafiltration membranes preparation, PEG is highly soluble with DMF and PES solution,
and therefore, it can be washed out together with the solvent from the membrane film to the
coagulation bath or vice versa. The rates of diffusivity of PEG is much slower than the solvent
(DMF). Therefore, the PEG in solvent (DMF) take more time to reach the surface and this will give
ample time for the polymer aggregates on t op of it to form a thicker and denser layer. Hence, mass
transfer value differ from 9.6 to 10.1 X106 m/s, in case of PES membranes without PEG and with
PEG (Table 3).
Table 3.Mass transfer coefficient and true retention of the membranes
Membrane No Mass transfer Coefficient X106 m/s True retention %
PES1 9.6 90.4
PES2 8.5 88.0
PES3 8.0 86.1
PES4 7.1 85.9
PES5 6.6 81.0
PES6 5.6 68.0
PES-P1 10.1 89.3
PES-P2 9.7 90.6
PES-P3 9.0 89.8
PES-P4 8.0 86.3
6PES-P5 7.3 78.1
PES-P6 6.1 70
The mass transfer associated is obviously very important to gain knowledge of the phase-separation
mechanism during membrane formation because the mass transfer behavior plays
important roles in determining the pore formation on inside and surface of membranes.
3.4. Effect of PEG composition on pure water flux of PES membranes
The water flux of PES membranes without PEG 600 showed lower water flux than that of
PES membranes with PEG 600 (Table 4 and 5). The water flux for membrane PES-1 with 15 wt5
and 85wt% solvent combination was highest, followed by flux decreased for PES2 to PES-6 The
flux for PES-6 was on the lower value. Although the percent variation in flux looks on a higher side
for PES membranes with PEG 600, due to addition of PEG 600 in PES casting solution (17.4 times).
The difference in flux values of membrane by making with PES with PEG 600 and PES without
PEG 600 could be attributed to the larger pore size variations in the latter cases. This is evident from
the pore size architecture on surface of the membranes. This is further supported
by rejection studies
32
3.5. Concentration of sugarcane juice
The percentage of retention of sucrose increased as the PEG content added in the
formulations. This observation is in agreement with work done on ultrafiltration membranes by
several authors [17,18] that small amount of hydrophilic additives promote the retention through the
membrane. However, it is also noticed that if PEG is totally absent in the dope solution did not
match with the support porosity, probably due to the DMF/PEG processing during their manufacture.

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6480(Print), ISSN 0976 – 6499(Online), Volume 5, Issue 11, November (2014), pp. 26-36 © IAEME
Further, It is possible that the presence of low amounts of PEG probably caused rapid formation of
nuclei having PEG rich phase compared to the diffusion of non solvent into the polymer solution. It
can be seen from Table 4.14, retention of solids and sucrose from 17 and 15.8% to 29 to 24%, when
PEG added in PES/DMF dope solution. In addition, lower amount of hydrophilic additives in
ultrafiltration membrane caused the polymer particle at the surface to swell mainly in the vertical
direction thus creating spaces between the polymer structures, allowing solutes to pass through
easily.
Table 4. Retention of sucrose and solids of PES membranes with PEG 600
33
Type
Feed of sugar solution Permeate of sugar solution Retention of
solids
(%)
Retention of
Sucrose (%)
Brix
(%)
Pol
Pol
(%)
Purity
(%)
Brix
(%)
Pol
Pol
(%)
Purity
(%)
PES1 14.5 46 11.3 78.27 10.5 35 8.5 79 11 6.21
PES2 14.5 43 10.6 73.3 11 36 9.4 68.5 12 8.8
PES3 14.5 46 11.3 78.27 13 36.8 7.8 70 13.0 11.0
PES4 14.5 43 10.6 73.3 14.5 37.2 10.0 86.8 17.2 14.11
PES5 -- -- -- -- -- -- -- -- -- --
PES6 -- -- -- -- -- -- -- -- -- --
In this study, the effect of PEG on PES membranes for sugar solution concentration is
observed the increasing sugars solids percentage with addition of additives results in horizontal
polymer swelling and this is a hindrance of the solute passage thus solids percentage increased.
These results show that the formulated UF membrane produced in PES, is capable to concentrate
sugar from solution and are comparable to the with PEG and without PEG membrane found (Table
4.15). Moreover, feed solution purity and permeate solution purity shows small change during
ultrafiltration. Further, sugar industry, generally needs to be higher purity in dilute solution by the
UF membrane produced. The results achieved showed that the UF membrane produced in our study
was useful for commercialized PES membrane.
3.6. Effect of PES and PEG composition in transmembrane pressure (TMP)
The effect of PES composition and PEG on sugar solution flux at various transmembrane
pressures is shown in the Figures. 2 and 3. It is seen that within the range of 0 to 414 kPa, with
increase in transmembrane pressure, solution increases almost linearly for all the membranes. This is
due to the increase in effective driving force (transmembrane pressure) required for permeation
dilute solution through membarnes.

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Table 5. Retention of dextran, sucrose and solids of PES membranes without PEG 600
34
Type
Feed of sugar solution Permeate of sugar solution Retention of
solids
(%)
Retention of
Sucrose (%)
Brix
(%)
Pol
Pol
(%)
Purity
(%)
Brix
(%)
Pol
Pol
(%)
Purity
(%)
PES-P1 13 40.2 9.9 76.1 13 35 10 83 17 15.8
PES-P2 15 41 10.1 66.7 12.5 33.0 9.70 80 16.5 14.0
PES-P3 15 41 10.1 66.7 11.5 35.0 8.0 75 19 18
PES-P4 12.5 41 10.2 81.9 11.5 36. 9.0 81 22 19.5
PES-P5 12.5 41 10.2 81.9 10.5 34 8.5 82 25 20.8
PES-P6 12.5 40.3 9.97 79.7 10.5 33.2 8.5 81 29 24.0
The solution flux is also seen to decease with increase in PES composition form 15 to 18% in
dope solution. Further, in case of 19 % and 20% of PES, there is no solution flux collected, which is
due rigid and more domination polymer phase during membrane formation.
Figure 2. Effect of TMP on sugar solution flux of PES membranes without PEG 600
The result clearly indicates that addition of PEG influence the formation of pores in the
membranes, which affect the permeability as the latter is conceptually related to its pores for UF
membranes. The PEG completely from the membrane matrix, which are hydrophilic in nature, are
compelled to stay inside the matrix permanently, thus, making the membrane more hydrophilic.
From this observation, it is possible that trace amount of PEG may always remain entrapped in the
membrane matrix. This in turn can change the hydrophobic behavior of polyethersulfone membrane
to hydrophilic behaviour. Thus, in addition to porosity, increase in hydrophilicity with increase in

17. International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976 –
6480(Print), ISSN 0976 – 6499(Online), Volume 5, Issue 11, November (2014), pp. 26-36 © IAEME
addition of 2.5 wt% may be another important reason to enhance such performances of the sugar
solution concentration
Figure 3. Effect of TMP on sugar solution flux of PES membranes with PEG 600
35
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