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Ali Aljanabi. 1 16
Ali Aljanabi. 1 16
A procedure for synthesis of pure and composite membranes based on cellulose dissolved in NaOH-urea/
thiourea solutions was developed. The phase inversion method was employed for cellulose solution
conversion to supported and non-supported membranes. The use of tetraethyl orthosilicate (TEOS) as
precursor in synthesis of composite cellulose membranes produced significant changes in their structure
and pervaporation behaviour. The obtained membranes were tested for the pervaporation of ethanol-water
system. Pervaporation performances, which were evaluated in terms of total permeate flux, separation
factor and pervaporation separation index, strongly depended on TEOS loading, ethanol concentration and
operation temperature.
Keywords: alcohols dehydration, cellulose membrane, permeate flux, pervaporation, separation factor,
swelling degree
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(me m0 ) 100
(1)
m0
Pervaporation tests
Pervaporation experiments were carried out in a batch
stirred cell operated under vacuum. The supported
membrane was put on a sintered steel disk, 5 m average
pore diameter, welded to the top of the lower compartment.
The upper compartment containing the feed ethanol-water
mixture was closed in order to stop any loss from feed.
Before starting an experiment, the membrane was
equilibrated for 30 min with a liquid mixture of the same
composition as that of the feed. The swollen membrane
was then placed in the pervaporation device and the feed
liquid was charged to the upper compartment, wherein a
magnetic stirring was used to mix the ethanol-water
solution. This stirring aimed at minimizing the mass
transfer resitance between the feed liquid and membrane.
A vacuum of 100 mbar was applied to the lower
compartment by means of a vacuum pump (Sartorius,
Japan) and the permeate was collected in an ice trap.
The liquid temperature in the feed compartment and
the system mass were measured before starting (ti , mi)
and after finishing ( t f , m f) an experiment. Total
pervaporation flux, Jp, was estimated using eq. (2), where
m is the mass of the permeate collected during the
pervaporation time, , and A the effective membrane
area.
mi m f
m
Jp =
(2)
w / eth =
(Yw / Yeth )
( X w / X eth )
(3)
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PSI = J p ( w / eth 1 )
(4)
151
XRD measurements
XRD analysis for PC and 10CC membranes aimed at
obtaining quantitative data on their crystallinity. Results
presented in figure 3 and table 1 for dry membranes
emphasize that 10CC membrane has a cristallinity larger
than that of PC, i.e., 73.5 % vs. 53 %. These values are lower
than those of dry bacterial cellulose membranes (usually
over 95% [42]), which were successfully tested for
pervaporation separation of ethanol-water system [28].
OM measurements
Rheological measurements
Rheological tests of casting solutions with and without
TEOS were conducted at two values of operation
temperature (25 and 40 C), four levels of TEOS loading (050 %) and a shear rate ranging from 0.5 to 122 s-1.
Plots in figure 5, describing the variation of shear stress,
(Pa), depending on shear rate, (s-1), emphasize the
following aspects: (i) for pure cellulose and 10 % TEOS
casting solution at 25 C, the dependency between and
is linear (eq. (5)) and the intercept (0) is about 0 Pa,
corresponding to a newtonian fluid whose dynamic
viscosity is equal to the line slope (); data presented in
figure 5 and table 2 highlight similar values of viscosity, i.e.,
0.476 Pas and 0.518 Pas, respectively; (ii) for pure
Table 1
XRD ANALYSIS RESULTS
152
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Swelling tests
Because there is a strong dependence between the
pervaporation performances and membrane swelling, the
establishment of the effect of operational parameters on
the swelling degree, SD, is an important issue. Swelling
Fig. 5. Shear stress, , vs. shear rate, , at 25 C (a) and 40 C (b) for casting solutions with and without TEOS.
Table 2
DYNAMIC VISCOSITY OF CASTING
SOLUTIONS DEPENDING ON PROCESS
PARAMETERS
Table 3
DEPENDENCE OF SWELLING DEGREE (%) ON WATER MASS
PERCENTAGE IN THE FEED, cw, TEOS MASS LOADING AND
OPERATION TEMPERATURE
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153
Table 4
THE EFFECT OF WATER MASS PERCENTAGE IN THE FEED, cw, AND
TEOS MASS LOADING ON ACTIVATION ENERGY, Ep, AND PERMEATION
RATE CONSTANT, Jp0
Fig. 7. Total pervaporation flux, Jp, vs. water mass percentage in the
feed, cw, at various values of TEOS mass loading and pervaporation
temperature
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Table 5
PERFORMANCES OF LIQUID
MIXTURE PERVAPORATION USING
HYDROPHILIC MEMBRANES
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155
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