CH2112 WASTE WATER TREATMENT - PHYSICAL UNIT OPERATION & CHEMICAL UNIT

PROCESSES
SRM University
Super-Hydrophobic Coating on Fiberglass Cloth
for Selective Removal of Oil from water
Deli Zang, Feng Liu, Ming Zhang, Xiaogang Niu, Zhengxin Gao, Chengyu Wang
Chemical Engineering Journal, 24 September 2014
MATERIALS USED
Fiberglass cloth (obtained locally)
Amino-silica particles
Bisphenol - A epoxy resin (E-54) [as caking agent]
Octadecyltrichlorosilane (OTS) [for hydrophobization]

PROCESSES INVOLVED
Fabrication of amino-silica particles
Synthesis of superhydrophobic fiberglass cloth
Characterizations SEM, and water contact angles (CAs)
Application in water-oil separation
FABRICATION OF AMINO-SILICA PARTICLES (Sol-gel process)

10 mL of ammonia solution (28.0%, catalyst)

mixture of 180 mL anhydrous ethanol, 20 mL Tetraethoxysilane (TEOS) and 20 mL deionized
water (under magnetic stirring for 2 h)

Reaction left at room temperature for 12 h. Silica particles were separated from the turbid liquid
by centrifugation, purified by ethanol to remove unreacted substance, and then dried in an oven
at 50
o
C

In the next process, 5 mL 3-Aminopropyltriethoxysilane (APS)

beaker containing 5 mL deionized water and 25 mL anhydrous ethanol under magnetic
stirring to form APS hydrolysate.
Afterwards, APS hydrolysate
(added dropwise)
100 mL anhydrous ethanol solution with 4.0 g silica via 12 h of magnetic stirring at 60
o
C.
Finally, the amino-silica particles were successfully obtained through centrifugation in ethanol
and drying at 60
o
C for 10 h.
SYNTHESIS OF SUPERHYDROPHOBIC FIBERGLASS CLOTH

The fiberglass cloth sample was first dipped into epoxy resin acetone solution (3%, m/v) for 30
min, entirely dried with nitrogen
Then introduced in 0.5% amino-silica aqueous solution
Subsequently, the sample was washed with deionized water and dried in a vacuum oven at 80
o
C
for 12 h to obtain epoxy/silica coating on fiberglass cloth surface.
The epoxy/silica coated fiberglass cloth was immersed into OTS ethanol solution, which was
prepared by mixing 100 mL anhydrous ethanol, 2 mL OTS, 0.25 mL H
2
O and 0.05 mL glacial
acetic acid together under the condition of stirring. The unity was maintained at 60
o
C for 2 h.

In the end, fiberglass cloth was removed, rinsed with anhydrous ethanol to get rid of redundant
OTS, and then dried completely to get superhydrophobic fiberglass cloth.
MICROSCOPIC STRUCTURE OF THE SUPERHYDROPHOBIC FIBERGLASS CLOTH
The surface appearances of pristine and as-prepared fiberglass cloth were typical monitored by a
scanning electron microscope :










SEM images of pristine fiberglass cloth (a-b)as-prepared superhydrophobic fiberglass cloth (c-d)
WETTABILITY OF SUPERHYDROPHOBIC FIBERGLASS CLOTH SURFACE
Evaluated by exploring contact angle through a drop on specimen.

Photographs of water droplets on pristine fiberglass cloth (a)OTS-coated fiberglass cloth (b)epoxy/silica-
coated fiberglass cloth (c)superhydrophobic fiberglass cloth (d)
According to theoretical principle of surface wettability, the prepared composition coating
on the surface of fiberglass cloth, which consisted of silica particles and low surface free
energy decorated by OTS, could efficiently prevent water from penetrating the interspaces
and cavities of sample under the action of capillary pressure.

Therefore, the as-treated fiberglass cloth was superhydrophobic.
APPLICATION IN THE FIELD OF WATER-OIL SEPARATION
As soon as water-oil mixture was poured onto the superhydrophobic fiberglass cloth surface, oil
content would penetrate through and fall into the middle vessel. Meanwhile, water droplet was
left behind and tumbled out of fiberglass cloth surface into outboard beaker along the exterior of
middle positioned vessel.

(a) water and diesel oil mixture: the volume of water and diesel oil is equal; (b) the executive procedure
of the separation; (c) separation is complete: diesel oil in middle vessel and water in outboard beaker
REUSABILITY OF SUPERHYDROPHOBIC FIBREGLASS CLOTH
Investigating separation efficiency after numerous of water-oil separation recycles

Variation of the water contact angle and separation efficiency of superhydrophobic fiberglass cloth
with recycle numbers of water-oil separation.
After 30 recycles, separation efficiency of superhydrophobic fiberglass cloth ranged from
98% to 94% and water contact angle varied from 154 to 150, indicating that
superhydrophobic fiberglass cloth still displayed high separation efficiency.

In the above experiment, superhydrophobic fiberglass cloth displayed wonderful water-oil
separation capacity and reusability.

Thus, superhydrophobic fiberglass cloth would be able to extend its application in removing
spilled oil.
CONCLUSIONS
To sum up, we have put forward a simple approach to the fabrication of superhydrophobic
composition coating on fiberglass cloth surface through the generation of amino-silica
followed by OTS hydrophobization.
This is the first reported technique for fiberglass cloth to receive water-repellent property
which can be applied to separate oil from water.
The results clearly showed that the homogeneous deposition of amino-SiO
2
particles had
caused sufficient roughness, while OTS induced low surface energy. The contact angle tests
demonstrated that as-prepared fiberglass cloth displayed wonderful superhydrophobic
performance with water contact angle of 154.
It is important that superhydrophobic fiberglass cloth has been employed to purify oily
wastewater with separation efficiency as high as 98%.

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