EFFECT OF SILICA ON THE PROPERTIES OF

CELLULOSE ACETATE/POLYETHYLENE GLYCOL

MEMBRANES FOR REVERSE OSMOSIS

By: I MADE PENDI ADI MERTA

(2311100033)
DEFFRY DANIUS DWI PUTRA
(2311100088)

2.1 MATERIALS
MATERIAL
Cellulose acetate (CA, Mw
30,000 and acetyl content39%),

acetone

SUPPLIED BY
BDH laboratories supplies,
Poole, England.

Polyethylene glycol-600 (PEG)

Silica (SiO2)
Sigma Aldrich

2.2 Preparation of doped solutions

1.

2.

3.

4.

5.

10 g of CA was dissolved in 80 mL of acetone with

constant stirring at 80 C for 2 h.
10 g of PEG was added with regular stirring at 80 C
for 6 h.
The viscous and clear solution was obtained, which
was termed as a blended doped Solution, CA/PEG-1
[26].
The different ratios of CA/PEG (12/8, 14/6 and 16/4
g/g) were used to prepare three additional doped
solutions, labeled as CA/PEG-2, CA/PEG-3 and
CA/PEG-4 respectively.
The casting solutions were allowed to cool down to
room temperature (25 C) and were kept for 24 h in a
sealed ask to remove micro bubbles formed in the

2.3 Membrane physical

Characterization
1.

2.

3.

4.

The doped solution was spread slowly on glass plate by

maintaining uniform thickness with the help of micrometer
adjustable lm applicator (Ref: 1117/300 Sheen instruments).
The temperature of casted membranes was lowered
immediately to 0 C for 15 min to induce (TIPS). The TIPS
causes the formation of dense and asymmetric structure.
It was followed by precipitation under controlled evaporation
by increasing temperature up to 60 C [27].
The skinned membranes, thus formed [28] were carefully
removed from the glass plates by using a sharp knife. The
thickness of the resulting membranes was measured and
was found in the range of 50200 microns.

2.4 Modication of doped solutions

1.

2.

Silica (15%, w/v) was dispersed in alkaline solution (10 mL)

before adding to the CA/PEG-4 blended dope solution with
constant stirring for 2 h at 80 C.
The membranes (CPS-1CPS-5) were casted and dried
following the same procedure as mentioned in Section 2.3

3. Characterization
3.1. Membrane performance
3.1.1. Experimental set up of RO rig
3.1.2. Water content
3.1.3. Permeate ux (J)
3.1.4. Salt rejection
3.2. Membrane permeability
3.3. Contact angle measurement
3.4. Fourier Transform infrared spectroscopy (FTIR)
3.5. Thermal analysis
3.6. Mechanical stability
3.7. Scanning electron microscopy (SEM)

4. Results and discussions

4.1. Membrane performance

Table 1. CA/PEG-1 membrane showed a maximum ux of 0.87 L/h m2 while it

exhibited minimum salt rejection capacity of 52%. CA/PEG-4 membrane had
81.5% salt rejection and its ux was 0.35 L/h m2.

Results and discussions

It was observed that with the increased content of cellulose
acetate, the water content, ux and membrane permeability
was decreased while the salt rejection capacity was increased
remarkably.
PEG is hydrophilic in nature and acts as pore former [38].
CA/PEG-1 membrane, with maximum quantity of PEG, showed
increase in water ux, but at the same time salt rejection was
compromised. This might be attributed to the formation of
macro voids [39] on membrane which allowed the passage of
salt along with water. Moreover, the diffusion rate of water was
accelerated by the presence of PEG due to its hydrophilic
nature. PEG increased the tendency of pore formation and as
a consequence ux was increased.

Result

Similarly, the ux of all modied membranes also increased with the

increase in silica content. CPS-5 membrane has highest ux of 2.46 L/h
m2
The salt rejection increased from 81.5% to 92% for CPS-4 membrane as
a result of incorporation of silica particles [42]

4.1.1. Analysis of membrane fouling during permeation

Fig. 3 shows tthe ux

increased remarkably with the
increase of SiO2 content.
The increase in permeation
ux was due to the increase in
surface hydrophilicity which
was
rendered by SiO2
particles.

4.2. Contact angle

In general, a smaller contact

angle corresponds to a more
hydrophilic material
Fig. 4 represents digital
image of a liquid droplet on a
dry surface of all membranes
in which the contact angle
() is measured according to
the sessile drop method

4.3. Contact angle

Fig. 5 that there is

decrease in contact angle
by increasing silica particle
concentration.
These results
demonstrated that silica
particle can improve
hydrophilicity of membrane.
The less hydrophilic
surface shows larger
contact angle with the
surface and vice versa.

4.4. Mechanical stability

Fig. 10. It was noteworthy

that the elongation-atbreak, tensile stress and
Young's modulus initially
increased with the
addition of SiO2 particles
and reached at peak
when the SiO2 particle
concentration was 4%
(w/v) and then declined
as the SiO2 particle
concentration was further
increased. Yan et al.

4.5. SEM analysis

Fig. 12 (af) represents the

images of modied
membranes with different
silica loadings.
The top surface morphology
is shown on Fig. 12(a). It
was observed that microsize silica particle (0.51
m) were distributed in the
membrane.
The interaction of silica
particles with polymer
disrupts the mobility of
polymeric chains resulting in
the formation of
macroscopic defects [29].
But as concentration

CONCLUSION

The modied membranes resulted into an improved trend in the

salt rejection and permeation properties. CPS-4 had 92% salt
rejection which provided almost 11% increase in salt rejection
capacity compared with the control membrane (81.5%).
The mechanical stability of the modied membranes, increased
from 1 to 4% (w/v) of silica loading. Further increase in SiO2
particles in the casting solution resulted in the decrease of tensile
strength and elongation at break.
The SEM images revealed incorporation of silica particles within
the asymmetric composite membrane, that improved hydrophilicity
of the composite membrane also enhanced fouling resistance.
This study showed a critical need for optimizing the silica particle
loading, as overloading of silica may not be advantageous for RO
performance and has negative impact on the RO membrane
properties.