Desalination 223 (2008) 417–426

Separation of alcohol–water solutions by distillation

through hollow fibers

Guoliang Zhanga,b*, Lan Linb, Qin Menga, Youyi Xua

a
College of Materials Science and Chemical Engineering, Zhejiang University, Hangzhou 310027, P.R. China
b
College of Biological and Environmental Engineering, Zhejiang University of Technology,
Hangzhou 310014, P.R. China
Tel/Fax +86(571)88320863; email: guoliangz@zjut.edu.cn
Received 24 December 2006; accepted 3 January 2007

Abstract
New results of investigation on distillation in hollow fiber structured packing are discussed. The membranes used
here for separation of methanol, ethanol and isopropanol-water solutions are non-porous hollow fibers, unlike those
of membrane distillation. The fibers are non-selective with coating and have little resistance to mass transfer. Because
liquid flows inside the lumens of the fibers and vapor flows counter currently outside fibers, the distillation process
can avoid flooding effectively even at very high flows. As a result, a mole fraction of alcohol equal to 0.04 was
prepared as feed in all of the three solutions, and an attractive low value of the height of mass transfer unit (HTU)
less than 0.1 m could be obtained at total reflux. Although the distillate concentration drops as the heating rate rises,
as noted before, the decreasing rate of concentration and HTU in the same module seems to change inversely with
the molecular weight of alcohols. Compared with normal structured packing, the ordinate data of common
capacity factor of hollow fiber column calculated on the Eckert version of GPDC correlation were 3–10 times
higher above flooding. All these offered the possibility of distillation with better, more productive separations.
Keywords: Distillation; Hollow fiber membrane; Alcohol–water solution; Separation

1. Introduction known, conventional packed distillation columns

This paper continues to explore the distillation
process with new structured packing column, a
new type of membrane contactors. As is well
*Corresponding author.
always have some obstacles in selection of
packing material and uniform distribution of fluids
before they enter the packed bed. The interde-
pendence of the two-fluid phases which are
contacted very closely often leads to operational
problems such as emulsions, foaming, unloading
and flooding [1–3]. Using hollow fiber module is

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0011-9164/06/$– See front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.0000.00.000
418 G. Zhang et al. / Desalination 223 (2008) 417–426

an alternative effective way to overcome these

disadvantages and the relative experimental results
are proved to be promising according to Zhang
and Cussler [4,5].
Unlike most packed towers, fluids are con-
tacted flow on opposite sides of membrane and
the liquid/liquid interface forms at the mouth of
each pore. Further, the hollow fibers are supposed
to be non-selective by choosing suitable membrane-
making and coating materials and therefore be
different with earlier method called “membrane
distillation” [6–8].
The hollow fiber distillation process shown in
Fig. 1 can be potential route for faster separation,
even if there is no direct commercial value now.
Such a hollow fiber column has three advantages
over conventional packed towers. First, it offers
substantially more interfacial area than conven-
tional approaches by non-dispersive contacting
via a microporous membrane. A typical interfacial
area per volume is 201 ft2/ft3, almost triples the
value of Sulzer Mellapak structured packing
which is only 76 ft2/ft3. Second, because liquid
flows inside the fibers and vapor flows counter
currently outside fibers, the two-fluid flows are
independent and can be easily kept uniform distri-
bution to avoid flooding effectively even at very
high flows. Moreover, the flows of liquid and vapor
are now not around submerged objects and only
a very small pressure drop across the membrane is
required to ensure that the liquid/vapor interface
remains immobilized at the mouth of the pore.
Third, unlike traditional packed towers, no density
difference between fluids is required and theo-
retically hollow fiber modules can be operated
in any orientation.
Our aim is to improve product purity and sepa-
ration efficiency by using different non-selective
hollow fiber membranes in different systems.
As usual, we hope to maximize mass transfer rate
by optimizing our design and process operation.
Here, the big interfacial area will be beneficial to
make more efficient separation, according to
Bennet and Kovak [9] and Kellehar and Fair [10],
Condenser
Gauged
cylinder
Hollow
fiber
contactor
Heater
XD
Liquid
Vapor
Reboiler
XW
Fig. 1. Schematic process for hollow fiber structured
packing distillation. The hollow fiber module replaces
the conventional packed tower used for differential dis-
tillation of alcohol–water systems. The structure of new
module tower in which liquid flows inside fibers and
vapor rises counter currently outside fibers leads to very
different operational characteristics.
which means the columns of hollow fiber struc-
tured packing will perform better, with the
height of transfer unit (HTU) as small as possi-
ble. In order to do this, we will take three alco-
hol systems including methanol, ethanol and
isopropanol–water solutions for separation exper-
iments. We want to see whether the performance
of the modules worked formerly can keep well
or not and find how different alcohols affect the
separation.
 G. Zhang et al. / Desalination 223 (2008) 417–426
2. Theoretical considerations
The theoretical analysis is based on the mass
balances and transfer unit theory basic to the
operation of a conventional differential distillation
column. We begin our work with the same data
on estimates of vapor-liquid equilibrium as differ-
ential and staged distillation [3,11]. For simplic-
ity, the column of hollow fibers is operated at
total reflux, which means the total vapor and liquid
fluxes are equal in the column. The relative bal-
ances on the more volatile species in both vapor
and liquid give the operating line
y=x (1)
where y and x are the mole fraction of the more
volatile species in the vapor and the liquid, respec-
tively. Then we can get a balance on the more
volatile species in the gas phase.
dy
0 = − vG − Ka ( y − y*) (2)
dz
where vG is the gas velocity, y and y* are the gas
phase mole fractions in the actual vapor and in
the vapor which is in equilibrium with the liquid,
z is the distance measured from the bottom of the
column, K is the overall mass transfer coefficient
based on the vapor side, and a is the interfacial
area per volume between vapor and liquid. Inte-
grate this equation, we can easily find the number
of transfer units (NTU) for our column
yl dy Kal
NTU = ∫ y0 y − y*
=
vG
(3)
where y0 and yl are the specified vapor composi-
tions at the bottom (z = 0) and at the top (z = l)
of the column, l is the length of the hollow fiber
module. As usual, the NTU calculated by integra-
tion of the experimental data is a good measure of
the difficulty of the distillation and shows how
high the separation efficiency is. A larger value
means an easier separation, and a smaller one
signals a more difficult separation. As transfer unit
419
theory has been used for many years to design
absorption columns in industry, the challenge
has always been to design an appropriate height
for the packed column. The height of an absorption
column l is given by
l = NTU × HTU (4)
where HTU is the height of a transfer unit. In our
experiment, since the length of modules is set,
the true value of HTU can be easily estimated by
HTU = l/NTU (5)
Since the height of a transfer unit HTU can
be defined as the height of a packed section
required to accomplish a change in concentration
equal to the average driving force in that section,
the smaller the HTU is, the better design should be.
HTU normally is a measure of industrial tower or
column’s separation efficiency. A still smaller
HTU means more efficient and more rapid separa-
tion process, and that’s what we dream about.
The technology route of a differential distil-
lation tower structurally packed by hollow fibers
is similar to that of conventional one, as Kister
[3] described, but the process is very different.
As noted above, we start our experiment with
a very low feed concentration, and the desired
concentrations of distillate and bottom. The liquid
and vapor flows are very independent because
of the non-porous hollow fiber walls. The two-
phase flow and maldistribution in conventional
process can then be effectively prevented. The
liquid and vapor can be pumped very freely with
almost no pressure drop coming from fluid fric-
tion, and still not be bothered by loading and
flooding. Although we have little experience to
guide our choice on column designing and mate-
rial choosing, we think it important to choose the
structure and dimension of the column’s internals,
and we will specify the relative difficulty of the
separation of different alcohol systems as NTU.
We can analyze our experiment using the same
420 G. Zhang et al. / Desalination 223 (2008) 417–426
equations as given above. After measuring the
concentrations y0 and yl and calculating the NTU
value, we can estimate mass transfer coefficients
from the NTU and hollow fiber geometry and
find if they are different in different separation
systems or with empirical values of membrane
contactors elsewhere.
3. Experimental
The microporous polyether sulfone hollow
fibers (Porous Media, MN, USA and RDCWTT,
Hangzhou, China) used in this work have an inside
diameter of 0.07 cm and an outside diameter of
0.11 cm. A thin layer of 5 µm polydimethylsilox-
ane was coated on the membrane for stopping
convection. Thus liquid flow could not pass
through the wall to the vapor side while vapor
could flee out freely. From the earlier results of
Zhang and Cussler [4,5], we chose 25 fibers
in a glass shell with inside diameter of 1.40 cm
as module design basis. Each module with two
nozzles had an effective mass transfer length of
25 cm. The module properties are compared in
Table 1 with commercial structured packings –
Sulzer Mellapak [12]. The void fractions of the
hollow fiber modules are lower than those of
the conventional structured packing, while the
areas per volume are larger, according to Yang
and Cussler [13] and Kistler and Cussler [14]. The
hollow fibers were potted with SG-856 epoxy
Table 1
Properties of hollow fiber modules and structured packing
Module packing Size or type
Module 1 25 (number of fibers)
Module 2 50 (number of fibers)
Sulzer Mellapak 250Y
Sulzer BX BX 500
Raschig Rings 1 inch
Raschig Rings 1/2 inch
(Jinpeng Chem., Zhejiang, China) and HC 703
silicone (Xiguang, Wuxi, China).
All distillation experiments were run at total
reflux. In a typical experiment, all solvents includ-
ing methanol, ethanol and isopropanol (Sinopharm
Chemical Reagent Co., Ltd, Shanghai, China)
were at least HPLC-UV grade and used as received,
and an alcohol solution with a molar fraction of
0.04 was prepared as feed with doubly distilled
water. About 800 cm3 of this solution was added
to the reboiler and heated in a 350 w 98-1-C digital
auto-control heating mantle (Taisite Co., Tian-
jin, China). The heating rate was adjusted by a
FATO SVC-500 VA automatic voltage regulator
and measured by a JL 4006B electric multimeter
(Junling Co., Hangzhou, China). Then the vapor
generated flew up the shell side with liquid reflux
from condenser dropped down inside fibers con-
currently (Fig. 1). All flows were measured volu-
metrically. Solution concentrations were measured
as 1 cm3 samples taken from the reboiler and from
the distillate, respectively. The concentrations were
determined by injecting 2 μL samples into a SF
GC-1102 gas chromatograph equipped with a
temperature conduct detector (TCD) and a Super
Porapak Q steel column. The carrier gas was
hydrogen of purity 99.99%. Each concentration
was measured at least in duplicate. To begin the
experiment, we usually ran the column at a heating
rate for about 1–2 h to approach steady state, when
the first sample was taken. Subsequent samples
Void fraction, e Area per volume, Packing factor,
a (ft2/ft3) FP (a/e3)
0.85 201 327
0.71 484 1352
0.95 76 89
0.90 150 206
0.78 58 179
0.70 101 580
 G. Zhang et al. / Desalination 223 (2008) 417–426
were then taken at 15–30 min intervals to ensure
steady state.
The calculation of the NTU from these data is
complicated because the slope of each equilibrium
line for different alcohol systems is not constant,
so that m is not constant. Over the concentration
range of 0.1 < x < 0.9, the vapor–liquid equilib-
rium fit the polynomials and a data relationship
can be expressed mathematically as below [15].
Equation for methanol (no azeotropic point),
0.1 < x ≤ 0.3
y* = 0.1754 + 2.8545x − 4.0810x2 (6)
0.3 < x < 0.9
y* = 0.4823 + 0.6679x − 0.1571x2 (7)
Equation for ethanol (azeotropic concentra-
tion x = 0.881)
0.17 < x ≤ 0.33
y* = 0.348 + 1.1821x − 1.4292x2 (8)
0.33 < x < 0.68
y* = 0.4977 + 0.1791x − 0.2599x2 (9)
Equation for isopropanol (azeotropic concen-
tration x = 0.675)
0.13 < x ≤ 0.33
y* = 0.4438 + 0.5449x − 0.6984x2 (10)
0.33 < x < 0.79
y* = 0.5678 − 0.2586x + 0.6278x2 (11)
Using these relations and Eq. (3), the NTUs
and HTUs can be easily found for comparison
with different separation systems operated in the
same module. The results are given below.
4. Results and discussion
This section reports distillation separations
using a structure packing of hollow fibers. We are
especially interested in confirming its behavior
421
in different alcohol systems, finding some regular-
ity and achieving the lowest value of the height
of a transfer unit as possible as we can.
As before, we can easily operate hollow fiber
at flows greater than that causing flooding, as
shown in Fig. 2. The relationship between the
flooding gas velocity and other physical proper-
ties of the system is presented in the form of an
empirical, experimental correlation for pressure
drop in packed columns. This method was pro-
posed by Sherwood in 1938 and improved by
Eckert in 1970 to determine the flood point,
which basically remains the standard procedure
today [1,3,11]. We plot the normal flow parameter
on the abscissa, and the common capacity factor
on the ordinate. The solid curve is the empirically
determined limit of flooding. For conventional
packing, the gas velocity in an operating column
must obviously be lower than the flooding velocity
and is often chosen as one-half the predicted
1
Y = (uo2FPρ Gf { ρ L} { μ L})/(gρ H O(L))
2
0.1
0.01
Methanol
Ethanol
Isopropanol
0.001
0.01 0.1 1 10
0.5
X = (LML/GMG) (ρG/ρL)
Fig. 2. Hollow fiber distillation operate above flooding.
Like conventional distillation process, the flow para-
meter on the abscissa is plotted vs. the capacity factor
on the ordinate. All the data of methanol, ethanol and
isopropanol–water systems are at fluxes high above the
normal flooding limit, shown as the solid line.
422 G. Zhang et al. / Desalination 223 (2008) 417–426
flooding velocity obtained from a generalized cor-
relation. So points above this solid curve cannot
be reached to ensure safe operation. In Fig. 2, we
also show the data points of our experiments
with hollow fibers in different alcohol solutions.
Without exception again, all the data points of
methanol, ethanol and isopropanol–water systems
are high above the limit solid curve where flooding
normally occurs. The highest data is 3–5 times
above the solid flooding line. Since we always ran
at total reflux, these data only cover a narrow
range of abscissa in which they proceed in the
order isopropanol > ethanol > methanol. But the
results clearly show how easily hollow fiber struc-
tured packing can operate above the normal flood-
ing point. In conventional cases, people must
choose a velocity far from the flooding velocity
but not so low as to require a much larger column
which will consume more cost of power, and
lower gas–liquid velocities often lead to a nearly
proportional reduction in mass transfer rate. In
our experiments, we could potentially operate
at still higher flow rates since vapor and liquid are
in contact only across the hole of membrane walls.
There is no resistance for a bubble rising through
liquid, and the falling liquid is not slowed by the
rising vapor, just as other membrane contactors do.
That is where the hollow fiber columns always
have an advantage on.
In order to compare the operational perfor-
mance of hollow fiber with normal structural pack-
ing in distillation process, the F-factor is plotted
vs. the NTU per meter (Fig. 3). The data points
here for same hollow fiber module in different
alcohol–water systems are compared with a type
of Sulzer structured packing (Sulzer Chemtech),
shown as the solid lines. The abscissa shows a
flow parameter F, which tends to cover about the
same range for different total pressures in con-
ventional distillation, since the flooding velocity
varies with rG1/2. Parameter F, generally used to
characterize performance of distillation packing
and known as the F-factor, see Refs. [3,12], is
defined as
F = uG r G1/2 (12)
where uG is the vapor velocity, rG is the vapor
density. The data in Fig. 3 show how the NTU
increase as the F-factor gets smaller. This figure
also shows some of the results under conditions
where the normal packing will flood, and the
separation efficiency estimated from NTU can
strongly compete with some excellent industrial
structured packing such as Sulzer Mellapak.
We next turn to find how the hollow fiber
module works as flows changes from high to low.
From Eq. (3), the reciprocal of the NTU (1/NTU)
should be proportional to the vapor velocity vG.
This is partly supported by the data in Fig. 4
when vapor velocity becomes high for all the
three systems. At low vapor velocity, the NTU
keeps a relative high value for some period. We
are not sure whether there are some limits with
the geometry of our column design or it is just
4.00
3.00
NTU (1/m)
2.00
Methanol
Ethanol
1.00 Isopropanol
Mellapak
0.00
0.1 1 10
Ff at or = uGρ G1/2 (m/s(kg/m3)1/2)
Fig. 3. Operational performance of hollow fiber and
normal structural packing in distillation process. The
F-factor is plotted vs. the number of transfer units. The
data for same hollow fiber module in different alcohol–
water systems are compared with a Sulzer structured
packing, shown as the solid line.
 G. Zhang et al. / Desalination 223 (2008) 417–426 423

2.0 2.0
Methanol Methanol y = 309.97x + 0.0688
Ethanol Ethanol y = 132.49x + 0.1304
Isopropanol 1.6 Isopropanol y = 127.58x + 0.2367
1/NTU

1.2
1.0

1/NTU
0.8

0.4
0.0
80 120 160 200 240
Vapor Velocity (cm/s) 0
0 0.001 0.002 0.003 0.004 0.005 0.006
Fig. 4. The number of transfer units (NTU) vs. vapor Liquid Flow (mol/s)
velocity. The slower the vapor flows, the higher NTU
value can be got, which means more efficient separa- Fig. 5. The number of transfer units (NTU) vs. liquid flow.
tion. Further, the data curve for lower molecular weight The reciprocal of the NTU is proportional to the molar
alcohol such as methanol is steeper than ethanol and liquid flow. Higher NTU value can be got when the
isopropanol, and very close to linear when vapor velocity liquid flow becomes slower. The slope of the linear
surpass 140 cm/s. relationship is in the order of methanol > ethanol >
isopropanol.

caused by heat losses due to the simple jacket

insulation. But the trend does mean that we can
obtain faster separation and higher purity of
alcohols in our hollow fiber column simply by
reducing the flows. We can use slow flows without
reducing the interfacial area just by making sure
the liquid inside fibers are full and can run con-
tinuously. Further, the NTU for lower molecular
weight alcohol such as methanol system separation
increases faster than ethanol and isopropanol,
but at same vapor velocity, the NTU for higher
molecular weight alcohol like ethanol and isopro-
panol looks larger, which means more efficient
separation.
Since the vapor velocity in our experiments is
calculated directly from heat balance, as described
by Poling et al. [16], and there is some insulation
problem which may cause heat loss, especially
when the counter current flow is slow, we use
data read from gauged cylinder and plot Fig. 5
to show change of the NTU vs. liquid flow more
precisely. From Eq. (4), we have a similar form of
the NTU rewritten as
x1 dx ⎡K a⎤
NTU = ∫ x0 x − x*
= ⎢ x ⎥l
⎣ L ⎦
(13)
where Kx is an overall mass transfer coefficient
based on a liquid side. Now the results in Fig. 5
meet our expectation from Eq. (13) very well,
the reciprocal of the NTU is proportional to the
molar liquid flow. As above, higher NTU value
can be got when the liquid flow becomes slower,
and the slope of the linear relationship is in the
order of methanol > ethanol > isopropanol. This
gives the overall mass transfer coefficient Kx for
methanol, ethanol and isopropanol of 2.45 × 10−5,
5.73 × 10−5 and 5.95 × 10−5, respectively, in accor-
dance with the same order as former results,
according to Zhang and Cussler [4,5] and Chung
et al. [17]. The intercept on this plot may be
dependent on the properties of flow, module
configuration and the heat loss of process.
To reassure our results, we show the varia-
tion of distillate concentration with heating rate
in Fig. 6. The higher distillate concentrations
424 G. Zhang et al. / Desalination 223 (2008) 417–426

1.0 0.40

Methanol
0.8
0.30 Ethanol
Distillate Concentration (mol)

Isopropanol

0.6

HTU (m)
0.20

0.4

0.10
Methanol
0.2 Ethanol
Isopropanol

0.00
0 80 100 120 140 160 180 200
80 100 120 140 160 180 200 Heat Rate (W)
Heat Rate (W)
Fig. 7. The height of a transfer unit (HTU) vs. heating
Fig. 6. Distillate concentration vs. heating rate. As the rate. Because the heating rate is proportional to resi-
heating rate increases, the distillate concentration at the dence time in the column, the height of a transfer unit
top of module decreases. drops as the heating rate rises.

observed at the lower heating rate are consequence decreasing rate of the height of mass transfer unit
of better mass transfer in vapor/liquid interface, in the same hollow fiber module seems to change
and the relative sensitivity of distillate concen- inversely with the molecular weight of alcohols.
tration change with heating rate is methanol > Although the above results have already shown
ethanol > isopropanol. As we know, there is an a promising future for fast and efficient separation
azeotropic point for both ethanol and isopropanol in hollow fibers, we hope to do better. In conven-
solution, such as isopropanol–water azeotrope tional distillation, packing always wins by high
forming at an isopropanol mole fraction of 0.675, surface area per unit volume and high void frac-
and at present we cannot break through it with tion, so the hollow fiber can go farther with better
our owned modules in the experiments, that means characteristics on it. As before, the physical
separation of methanol solution without azeotrope properties of the system, the liquid/gas flow and
formation will be simpler and easier. the packing controls the performance of conven-
Finally, the height of a transfer unit is plotted tional packed column. That means the geometry
vs. heating rate in Fig. 7. Because the heating of packing, usually characterized as ‘Packing
rate is proportional to residence time in the column, factor’, is critical for process designing, see refs.
the height of a transfer unit drops obviously as [3,9,11]. Packing factor FP is defined as
the heating rate rises while the contacting time a
becomes shorter. In our experiments, a low-mole FP = (14)
fraction of alcohol as low as 0.04 was prepared as e3
feed in all of the three solutions, and an attractive where e is the void fraction of the packing. To
low value of the HTU less than 0.1 m could be get a bigger value of this packing factor, the
easily obtained at total reflux. The data in Fig. 6 packing in a set column should be chosen smaller
also show the same behavior as the above, the because FP is roughly proportional to the packing
 G. Zhang et al. / Desalination 223 (2008) 417–426
size (see Table 1). But even the smallest conven-
tional packing cannot get a higher packing factor
than hollow fibers whose interfacial area per
volume is large. In our experiments, a same size
module gives a packing factor of 327 ft−1 with
25 fibers and 1352 ft−1 with 50 fibers, the ampli-
fier factor is very big. That means we still have
huge space to optimize our separation in hollow
fibers. We look forward to more productive
distillation over a wider operational range and
provide more significant energy savings in the
near future.
5. Conclusions
New results have been introduced which
show the separation of methanol, ethanol and
isopropanol–water solutions with distillation using
hollow fiber structured packing. The membranes
used here for are non-porous hollow fibers, unlike
those of membrane distillation. The fibers are
non-selective with coating and have little resis-
tance to mass transfer. Because liquid flows
inside the lumens of the fibers and vapors flows
counter currently outside fibers, the distillation
process can avoid flooding effectively even at
3–10 times higher flows than conventional cases.
With a mole fraction of alcohol as low as 0.04
prepared as feed in all of the three solutions, an
attractive low value of the HTU less than 0.1 m
can be easily obtained at total reflux. Moreover,
while the distillate concentration drops as the heat-
ing rate rises, just as noted before, the decreasing
rate of distillate concentration and HTU in the
same module seems to change inversely with the
molecular weight of alcohols. Compared with con-
ventional structured packing, the hollow fibers
have a better geometry of packing and can realize
a more productive distillation and will save more
energy in separation.
Further experiments will focus on the optimiza-
tion of module structure and process design and
using more systems to validate our investigation.
425
Acknowledgments
The authors benefited from conversation with
Dr. E.L. Cussler during visiting CEMS, UMN.
This work was primarily funded by the Research
Fund of the National Natural Science Foundation
of China (grant 20476096). Other financial
support came from the Zhejiang Provincial Bureau
of Science and Technology, China (grants
2005C33040 and 2006C23067).
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