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Fabrication of Nano porous
membrane for Ultra filtration
Supervised by: Dr. M. Mujahid
ADNAN ALAM
MS MATERIAL AND SURFACE
ENGINEERING
REG#2011-NUST-MS PhD-MS-E-02
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Contents
Phase Inversion Process
Membrane Fabrication
SEM Results AFM Results
FT-IR Results
XRD Results
De-Ionized water Flux Results
Future Work
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Phase Inversion Process
Liquid Liquid Phase Inversion
Mass transfer takes place, i.e. the
solvent from the polymer solutiondiffuses into the precipitation bath,
whereas the non-solvent diffuses into
the polymer solution. Thus, solution
composition is changed which takes to
a de-mixing process.
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Pore Formation Mechanism
The polymer solution in solvent results inhomogenous polymer-solvent solution.
When this solution in exposed in
precipitation bath containing non-solvent,exchange between solvent and non-
solvent takes place.
Solvent leaves polymer solution creatingvoids while non-solvent diffuses in
polymer, precipitating it into membrane
structure. 6
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Membrane Modules
UF membrane modules are
Tubular Hollow-fiber
Spiral wound configurations
Flat sheet
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Materials for Membrane
Polymer (Cellulose Acetate)
Pore gen (Chitosan)
Solvent (Formic Acid)
Non-solvent (Water)
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Limitations of Cellulose Acetate
Membrane
Thermal stability
Poor film making properties Mechanical properties
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Improvement in CA by Chitosan
Hydrophilic properties increase
Mechanical strength and mechanical
toughness increase
Anti bacterial activity
Excellent film forming ability
Chitosan non-toxic Chitosan as crosslinking agent
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BLEND RATIO
Cellulose Acetate: Chitosan: Formic Acid
10 : 3 : 150
Cellulose Acetate =1gm
Chitosan = 0.3 gm
Formic Acid = 15 ml
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Cellulose acetate based
membrane
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Cellulose acetate (CA) and Chitosan
Formic Acid
Constant stirring
De-aeration
casting on glass
Solvent Evaporation
Non-solvent addition
Membrane drying
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Casting & Blending
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Solution To Avoid Membrane
Shrinkage
Method # 1 Method # 2
1. Membrane immersion
in aqueous isopropylalcohol solution for 24
hrs.
2. Immersion in a mixture
of isopropyl alcohol andhexane solution for 24
hrs.
3. Immersion in pure
Hexane and than dryingin desiccators.
Drying in desiccators
keeping membranestretched.
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SEM RESULTS(Air dried
membrane)
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SEM RESULTS(Air dried
membrane)
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Cont…
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Cont…
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(Solvent dried membrane)
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Cont…
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Cont…
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Cont…
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Cont…
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Cont…
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Cont…
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SEM Conclusions
Membrane is porous
Uniform distribution of pores
Pore size ranges in UF limits (10-
100nm)
Reproducibility of results
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AFM (Air dried membrane)
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AFM (Solvent dried
membrane)
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Conclusions of AFM
Pore diameter confirmation
Surface Roughness Presence
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Comparison of AFM & SEM
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Structure Of Cellulose Acetate
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Structure Of Chitosan
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FT-IR
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0 500 1000 1500 2000 2500 3000 3500 4000 4500
-10
0
10
20
30
40
50
60
70
80
T r a n s m i t t a n c e %
Wave number(cm-1)
cellulose acetate
0 500 1000 1500 2000 2500 3000 3500 4000 4500
30
35
40
45
50
T r a n s m i t t a n c e %
wave number(cm-1)
Chitosan
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500 1000 1500 2000 2500 3000 3500 4000
0
20
40
60
80
100
T r a n s m i t t a n c e %
wave number (cm-1
membrane
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Comparison
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500 1000 1500 2000 2500 3000 3500 4000
-10
0
10
20
30
40
50
60
70
80
90
100
T r a n s m i t t a n c e %
Wave number (cm-1)
cellulose acetate
membrane
Chitosan
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Conclusion Of FT-IR
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The absorption peaks in FTIR spectrum of cellulose
acetate is attributed to the vibrations of the acetate group
at
1790 cm-1 (C=O),
1370 cm-1 (C-CH3),
and 1045 cm-1 (C-O-C).
The FTIR spectrum of Chitosan is characterized by
absorption bands at 3352 (-OH stretching),
2878 cm-1 (-CH3 stretching),1560 (N-H bending),
1404 cm-1 (-OH bending),
1077 cm-1 (C-O bending),
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Cont…
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All prominent peaks in both cellulose acetate and
Chitosan are present in membrane spectrum,
also broad hydroxyl peak in cellulose acetate
become narrow and shift in Position.
Therefore, these changes in the IR spectra
suggested that there is homogenous blending
between Chitosan and cellulose acetate inmembrane.
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XRD
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10 15 20 25 30 35 40
0
50
100
150
200
250
300
I n t e n s i t y
Thetea
Cellulose acteate
10 15 20 25 30 35 40
0
100
200
300
400
500
600
I n t e n
s i t y
Thetea
Chitosan
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10 15 20 25 30 35 40
0
20
40
60
80
100
120
140
160
I n t e n s i t y
Thetea
Membrane
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10 15 20 25 30 35 40
0
100
200
300
400
500
i n t e n s i t y
Thetea
Membrane
Cellulose acteat
Chitosan
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Conclusions of XRD
XRD pattern of Chitosan exhibited characteristiccrystalline reflections at approximately 21 θ .
Cellulose acetate XRD spectrum indicates an obvious
broad peak at 22 θ and this peak verified that Celluloseacetate had denser semi crystalline structure.
In XRD spectrum of membrane, both above mentioned
characteristics peaks of Chitosan and cellulose acetateshifts their position along with intensity. This change
clearly confirms successful blending of both Chitosan
and cellulose acetate in membrane
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P it C fi ti b Fl
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Porosity Confirmation by Flux
Rate
Water flux was measured by
Jw = Q/A . ∆t
Where
Q: Amount of permeate
A: Area of membrane
∆t: Time of sampling
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0.01 10.3 0.0103 0.00422 2.440758 0.01666666 146.445556
0.02 24.5 0.0245 0.00422 5.805687 0.01666666 348.341372
0.03 41.1 0.0411 0.00422 9.739336 0.01666666 584.360423
0.04 48 0.048 0.00422 11.37441 0.01666666 682.464728
0.05 74.9 0.0749 0.00422 17.74882 0.01666666 1064.92934
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0
200
400
600
800
1000
1200
0.01 0.02 0.03 0.04 0.05
f l u x ( L / m 2 h r )
Pressure(bar)
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0.01 10.1 0.0101 0.00422 2.393365 0.01666666 143.601953
0.02 23.9 0.0239 0.00422 5.663507 0.01666666 339.810562
0.03 40.7 0.0407 0.00422 9.64455 0.01666666 578.673217
0.04 54.7 0.0547 0.00422 12.96209 0.01666666 777.72543
0.05 76.3 0.0763 0.00422 18.08057 0.01666666 1084.83456
0
200
400
600
800
1000
1200
0.01 0.02 0.03 0.04 0.05
f l u x ( L / m 2 h r )
Pressure(bar)
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0.01 17.8 0.0178 0.00422 4.218009 0.01666666 253.08067
0.02 24.9 0.0249 0.00422 5.900474 0.01666666 354.028578
0.03 31.3 0.0313 0.00422 7.417062 0.01666666 445.023875
0.04 37.4 0.0374 0.00422 8.862559 0.01666666 531.753767
0.05 44 0.044 0.00422 10.42654 0.01666666 625.592667
0
200
400
600
800
0.01 0.02 0.03 0.04 0.05
f l u x ( L / m 2 h r )
Pressure(bar)
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0
200
400
600
800
1000
1200
0 0.01 0.02 0.03 0.04 0.05 0.06
flux(L/m2 hr) 11feb
flux(L/m2 hr) 13 feb
flux(L/m2 hr) 14feb
F
l
u
x
R
a
t
e
Pressure (bar)
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Future Work
Optimization of the process by varyingthe Chitosan content.
Waste water treatment/ proteinrejection and results analysis
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