Separation and Purification Technology 56 (2007) 143149

Distillation of methanolwater solution in hollow fibers

Guoliang Zhang a,b, , Lan Lin b , Qin Meng a , Youyi Xu a
a

College of Materials Science and Chemical Engineering, Zhejiang University, Hangzhou 310027, PR China
College of Biological and Environmental Engineering, Zhejiang University of Technology, Hangzhou 310014, PR China
Received 18 December 2006; received in revised form 17 January 2007; accepted 18 January 2007

Abstract
Non-porous hollow fibers were used as more excellent structured packing over normal packing in the distillation of methanolwater system. Due to
their special geometry, a column with hollow fibers could easily work 310 times higher above the limit where flooding usually occurs in conventional
cases. A small height of transfer units at 8 cm and the overall mass-transfer coefficient Kx based on the liquid-side at 2.3 105 mol/cm2 s were
obtained experimentally. Compared with theoretical estimation from earlier studies, it was found that the liquid side was mostly responsible for the
total resistance of mass transfer, which was similar to the conventional distillation process at low concentration, although mass transfer resistance
in the membrane and the vapor could not be negligible.
2007 Elsevier B.V. All rights reserved.
Keywords: Hollow fibers; Distillation; Methanolwater system; Mass transfer coefficient

1. Introduction
One of the main challenges in designing and operating conventional distillation is to maximize the mass transfer rate by
producing as much interfacial area as possible. Although conventional distillation have been workhorses of the chemical
industry for decades, an important disadvantage is the interdependence of the two fluid phases to be contacted, which
sometimes leads to many difficulties such as emulsions, foaming, unloading and flooding. For devices with moving internals,
successful operation relies on how to minimize the bubble or
droplet size of the dispersed phase and maximize the number of
bubbles or droplets, see Kister and BennettKovak [1,2]. Usually
the separation is hard to control and causes lower efficiency. An
alternative separation technology that overcomes these disadvantages and also offers substantially more interfacial area than
conventional cases is the membrane contactor, as described by
YangCussler, AlanHwang, KelleharFair and Obuskovic et
al. [36].
In this work, non-porous hollow fibers (with a 5 m polydimethylsiloxane coating) were used as special structured
packing in the distillation of methanolwater solutions. Such
Corresponding author at: College of Materials Science and Chemical Engineering, Zhejiang University, Hangzhou 310027, PR China.
Tel.: +86 571 88320863; fax: +86 571 88320863.
E-mail address: guoliangz@zjut.edu.cn (G. Zhang).

1383-5866/$ see front matter 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.seppur.2007.01.016

a column may have several advantages over many conventional

packing columns. One advantage is the large interfacial area
between vapor and condensate possible with the small diameter
fibers. This area is fixed, independent of vapor or condensate
flows. Another advantage is that the vapor fluid mechanics is
independent of the condensate fluid mechanics, so the constraints of loading and flooding are much less severe. As a result,
the hollow fiber column can be operated at much higher flows
than those normally impossible, and hence make an existing distillation column more productive. The earlier research of Zhang
and Cussler [7,8] has already showed that this geometry could
operate well above the normal flooding limit and potentially gave
a small height of transfer units (HTU), which demonstrates the
potential for reducing energy use in the most common separation of isopropanolwater solution. For comparing, another
alcoholmethanol has been tried in distillation with these nonporous fibers and the relationship between overall mass-transfer
coefficients and individual mass-transfer coefficients based on
different driving forces have been investigated here.
2. Theory
In order to study the performance of a typical hollow fiber
column in methanolwater separation and compare the results
to the former research, a benchmark of a membrane module like
those used in the past must be established first. Its mass balance
and its factual mass transfer were discussed as follows.

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G. Zhang et al. / Separation and Purification Technology 56 (2007) 143149

First, a mass balances basic for the operation of a differential

distillation column should be established [911]. The modules
in the experiments are always run at total reflux, so its geometry
implies:
AG G = AL L

(1)

where AG and AL are the area of the vapor and the liquid, G and L
are the molar vapor and liquid fluxes in the column, respectively.
As constant molar overflow is also assumed, these flows are
independent of their position. Under these conditions, balances
on methanol in both vapor and liquid give the familiar operating
line:
y=x

(2)

where y and x are methanol concentration in the vapor and the

liquid, respectively. Finally, a balance on methanol in the liquid
alone can be written as:
0 = L

dx
Kx a(x x )
dz

(3)

where Kx is the overall mass-transfer coefficient based on the

liquid-side, x x* the mole fraction driving force, a the fiber
area per lumen volume of the module, and z is the position in
the column. These mass balances are easily integrated to find
the relationship between the number of transfer units and liquid
flow:


1
1
L

= x1
=
l
(4)

NTU
Kx a
x2 (dx/(x x ))
where l is the length of the column. The number of transfer units
(NTU) is a measure of the difficulty of the separation. From
this equation, the value of experimental overall mass-transfer
coefficient can be found, and the height of transfer units (HTU),
which is a measure of the efficiency of the column, can also be
worked out by:
L
l
=
.
HTU =
NTU
Kx a

(5)

From Eq. (4), the value of NTU changes with the fluid
mechanics and the overall mass transfer coefficient based on the
liquid-side. This mass transfer coefficient is complicated and
can be shown theoretically as:
1
cL
1
1
1
=
=
+
+
KL
Kx
kL
HkG
HkM

(6)

where kG , kL and kM are individual mass transfer coefficients

based on mole fraction driving forces in the vapor, across the
membrane and in the liquid, respectively. KL is an overall mass
transfer coefficient based on a concentration difference as a driving force, cL the concentration of liquid and H is the partition
coefficient.
In order to find which phase among the vapor, liquid and
membrane control the mass transfer process, results of past
experiments were used to estimate the individual mass-transfer
coefficients and compared with factual values by calculation

[7]. For the high liquid flow above the flooding limit, the Graetz
number is given as:
Gz =

d 2 vL
DL l

(7)

where d is the diameter of hollow fiber, vL the liquid velocity, and

DL is the diffusion coefficient in the liquid. As before, the Graetz
number is always found to be large in the experiments (Gz > 4).
Under these circumstances, mass transfer in the hollow fibers can
be described by the well-known Leveque solution [12], which
is a limiting case of the more general Graetz solution applicable
when the Gz is large:
 2 1/3
kL d
d vL
Sh =
= 1.62
(8)
DL
lDL
where Sh is the Sherwood number. In the meantime, if the
Reynolds number Re in the testing module is in the range of
0.5500, a mass transfer correlation on the shell side can be
described as below [3]:


kG d
Re de 0.93 0.33
Sh =
Sc
= 1.25
D
l
 2 0.93 

0.33
d u
= 1.25 e
(9)
l
D
where de is the hydraulic diameter for the shell side of the module, which is 0.4 cm here. and are viscosity and density
of the vapor, respectively. Inserting the property values of the
vapor and the liquid [13,14], the values of kG , kL and kM can
be calculated and the overall mass transfer coefficient based on
a concentration difference KL can be obtained for comparing.
Experimental results will be discussed in the following sections.
3. Experimental
3.1. Membrane and modules
The solvent methanol was HPLC-UV grade (Sinopharm
Chemical Reagent Co. Ltd., Shanghai, China) and used as
received. About doubly distilled water was used for the preparation of the feed solutions whose molar fraction was usually
set at 0.04. The hollow fiber module, which is the main
part of this apparatus, was treated with coated, microporous
polyether sulfone fibers (Porous Media, St. Paul, MN, USA and
RDCWTT, Hangzhou, China). The fibers have an inside diameter of 0.07 cm, an outside diameter of 0.11 cm, and a 5 m
polydimethylsiloxane coating. This non-porous coating offers
little resistance to diffusion, but stopped convection very well.
The hollow fibers, installed in a glass shell with an inside diameter of 1.40 cm, were potted with epoxy. Each module had an
effective mass-transfer length of 25 cm. Other module properties were compared in Table 1 with two commercial structured
packingsCeramic and Mental raschig ring (random) [15]. The
areas per volume for hollow fibers were much larger and could be
easily increased by adding more fibers in the module, although
the void fractions of the modules were as much as those of the

G. Zhang et al. / Separation and Purification Technology 56 (2007) 143149

145

Table 1
Properties of different structured packings
Module packing

Size (mm)a

Void fraction,

Area per volume, a (m2 /m3 )

Packing factor, FP (a/3 )

Hollow fibers membrane

Hollow fibers membrane [7]
Ceramic raschig ring (random) [15]
Mental raschig ring (random) [15]

25 (number of fibers)
50 (number of fibers)
50 50 4.5
8 8 1.5

0.85
0.71
0.81
0.64

659
1587
93
570

1073
4434
175
2174

Annular packing size: diametrical height thick.

structured packing. The high efficiency of the module could

attribute to the big contact areas and its special geometry.
3.2. Equipment and process conditions
To begin an experiment, 800 ml feed solution of 0.04 mol
fraction methanol was added to the reboiler of the distillation
apparatus shown in Fig. 1. This reboiler was heated electrically
to produce vapor, which flowed up the shell side of the hollow
fiber module to a water-cooled condenser. The heating rate can
be adjusted by a FATO SVC-500VA automatic voltage regulator
and measured by a JL 4006B electric multimeter (Junling Co.,
Hangzhou, China). The condensate then ran downwards through
the hollow fiber lumens and the continuous flow was measured
volumetrically. To simplify the process analysis, the module was
always run at total reflux. The temperature difference between
vapor and liquid entering the module were carefully controlled
to prevent the sub-cooling in the vapor condenser.

3.3. Analysis and calculation

Solution concentrations were measured as 1 cm3 samples
taken from the reboiler and from the distillate in the meantime. The concentrations were determined by injecting 2 l
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 triplicate. The column was run for about 12 h to approach the
steady state, when the first sample was taken. Subsequent samples were then taken at about 1530 min intervals to ensure
steady state. These steps were repeated at different heating
rates.
The calculation of the number of transfer units from these data
is complicated because the slope of the equilibrium line is not
constant, so that m is not constant. Over the concentration range
of 0.1 < x < 0.9, the vaporliquid equilibrium data described by
Gmehling and Onken [16] fit the polynomials:
0.1 < x 0.3,

y = 0.1754 + 2.8545x 4.0810x2

(10)

0.3 < x < 0.9,

y = 0.4823 + 0.6679x 0.1571x2

(11)

Using these relations and Eq. (4), the NTUs can be obtained
experimentally as below and use for comparison with the estimates given by theory:
0.1 < x 0.3,
NTU = 0.3985(0.4828 + ln(0.5346 x) ln(0.0802 + x))
(12)
0.3 < x < 0.9,
NTU = 1.5553(ln(3.1033 + x) ln(0.9893 x) 1.5968)
(13)
4. Results and discussion

Fig. 1. Scheme of distillation in hollow fiber. The module was run at total reflux.
Liquid flowed through the lumens of the fibers, while vapor flowed counter
currently outside the fibers.

The excellent performance of membrane contactors in the

separation of isopropanolwater has been shown in the earlier experiment. In this section, the results of distillation of
methanolwater system in the hollow fiber structured packing
will be achieved. Special interest was taken in the calculation
of the mass-transfer coefficients and comparison between the
experimental and the estimated values from those theoretical
relationship of former experiments.

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G. Zhang et al. / Separation and Purification Technology 56 (2007) 143149

Fig. 2. Distillate concentration vs. heat rate. When heat rate increased, concentration of distillate at the top of the column decreased. , distillate at the top of
module; , feed at the bottom of module.

4.1. Changes of distillate concentration with heat rate

The variation of distillate concentration with heating rate in
steady state was shown in Fig. 2. The feed concentration in the
reboiler was kept almost the same and set at a mole fraction 0.04.
After reaching the steady state, samples were taken at each heat
rate and analyzed by GC. As the heat rate increased, the distillate
concentration on the top of the column decreased, which showed
a higher purity of methanol and better separation efficiency at
the lower heat rate. This was always true in the experiments
because lower heat rate meant a smaller vapor flow and thus the
lower vapor velocity. So was the liquid velocity as the column
was always run at total reflux. Therefore, the contact time of the
two fluids through the pore of membrane became longer, which
caused a better and more complete mass-transfer process. The
maximum concentration of the distillate was up to as high as
0.88 in this one-stage distillation using hollow fibers. Higher
concentration could be obtained if the still existing parallel flow,
which resulted in the insufficiency of mass-transfer was cut off.
Effective ways, including the baffle install and the flow mode
change, are intended to carry out in other experiments.
4.2. Excellent performance of hollow fiber operating above
flooding
Distillation with conventional packing usually has problems
of flooding especially when the vapor velocity is very high.
In this case, the column with hollow fibers showed excellent
performance and was easily operated at velocities greater than
that causing flooding in conventional distillations, as shown in
Fig. 3. These results were very similar to the former separation
of isopropanolwater [7]. As before, the normal flow parameter
is plotted on the abscissa, and the common capacity factor on
the ordinate. The solid curve was from the method proposed by
Sherwood in 1938 and improved by Eckert in 1970 to determine
the flood point empirically [1,9]. Experimental points above this
curve were 310 times higher beyond the limit where flooding

Fig. 3. Hollow fibers operates above flooding. A column with hollow fibers
could operate at fluxes 310 times higher above the normal flooding limit.

normally occurs and could not be reached with conventional

packing. Since vapor and liquid flowed independently along the
column and were in contact only across the membrane walls,
distillation was easy to operate above the normal flooding limit.
Further, there was no resistance for a bubble rising through liquid because there were no bubbles, and the falling liquid was not
slowed by the rising vapor, therefore a uniform distribution was
easily kept and only a very small pressure drop between 0.05
and 0.15 psi was observed in the experiment. Although there
was still a big space for optimization of the module configuration to go farther beyond flooding, the capacity shown here
and former experiment were promising and would give more
productive separation in industry.
4.3. HTU and separation efficiency
As mentioned in Section 2, the height of transfer units HTU
is a measure of the towers efficiency and can be calculated
from experimental data directly. In Fig. 4, when vapor velocity
became larger, the height of transfer units turned to be bigger,
which meant lower mass-transfer efficiency. This was because
the vapor was too fast to afford vapor and liquid being in contact
across the membrane walls. Here, the largest HTU of 36 cm at
the highest flow of 223 cm/s was only a mediocre value which
could be given by conventional packing, but the flow at which
they do so were impossible to reach in these more normal packing. This also implied that hollow fibers might provide a route to
a more productive distillation. The minimum HTU, which was
only 8 cm at the lowest vapor velocity of 116 cm/s, represented
higher separation efficiency. This enhanced efficiency was not
the result of a higher mass transfer coefficient, but results from
the plethora of interfacial area, which remained constant with
changes in operating conditions. It could be deduced that distillation in the fibers would provide not only more productive but
also more efficient separation than conventional packing.

G. Zhang et al. / Separation and Purification Technology 56 (2007) 143149

Fig. 4. The height of transfer units (HTU) vs. vapor velocity. While vapor
velocity changed, the height of mass transfer varied in the range of 836 cm,
representing a higher efficiency than conventional packings.

147

Fig. 5. The reciprocal of the number of transfer units (1/NTU) vs. liquid flow.
A linear relationship between 1/NTU and the liquid flow is predicted, showing
the experimental data fitted theoretical estimation well.

4.4. Evaluation of mass-transfer coefficients

The measurements of NTUs in hollow fiber modules would
be obtained from Eq. (4). With these measurements, Fig. 5 shows
a linear relationship between 1/NTU and the liquid flow L, which
was very consistent with theoretical estimation. As NTU was a
function of both the liquid flow L and the overall mass-transfer
coefficient based on the liquid-side Kx , an experimental Kx value
of 2.3 105 mol/cm2 s could be obtained from the slope of the
solid line, then an experimental KL,exp value of 0.0016 cm/s was
given by Kx /cL .
In order to compare this experimental value with theoretical estimation, the overall mass transfer coefficient KL based on
a concentration difference as a driving force should be calculated first. Normally, the theoretical result in Eq. (6) could be
compared to an electric circuit containing three resistances in
series, which represented resistance in the vapor 1/HkG , across
the membrane 1/HkM and in the liquid 1/kL , respectively. After
calculation, the main obstacle in the separation, which was
responsible for the total resistance could be found, and this was
very important for column design and operation optimization.
As the Graetz number was relatively large in the experiments
(Gz = 526 > 4), mass transfer inside the hollow fibers could be

described by the well-known Leveque solution, which was very

strong theory, and kL could be obtained from Eq. (8). In the
meantime, the Reynolds number Re at the vapor side in the testing module was in the range of 335650 (part of them beyond
the normal range Re = 0.5500 of parallel flow outside), mass
transfer on the shell side can roughly be described by Eq. (9)
and kG could be found. From other experiments, a mass transfer coefficient kM value for transport across the membrane was
normally about 1 cm/s [7]. This value under the assumption that
mass transfer was from the vapor into the membrane and back
into the vapor again was used first. Then the overall mass transfer
coefficient KL , a theoretical value, could easily be obtained from
Eq. (6). Table 2 illustrates the estimates of mass transfer coefficient with hollow fiber modules in different solutions and used
former results for comparison. It seemed that the mass transfer coefficients for hollow fibers in methanol and isopropanol
solutions were in the same order of the results of Zhang and
Chung et al. [3,8,17] even if there was obvious property difference between them, for example, an azeotropic point existed in
isopropanolwater system but none in methanol solutions.
The variation of resistances of mass-transfer with F-factor
was shown in Fig. 6. Here the parameter F was used to charac-

Table 2
Estimates of mass-transfer coefficient with hollow fiber modules in different systems
Mass-transfer coefficient in

Separation system
Methanol (vL = 1.65 cm/s)a

Isopropanol [7] (vL = 1.5 cm/s)a

Liquid (DL = 2 105 cm2 /s)

Gas (DG = 0.127 cm2 /s)
Partition coefficient (m = 1)
Membrane (kM from experiment)

kL = 11 104 cm/s
kG = 4.1 cm/s
H = 2.9 103
kM = 1 cm/s

kL = 8 104 cm/s
kG = 6.0 cm/s
H = 1.0 103
kM = 1 cm/s

Overall mass-transfer coefficient

KL = 7.5 104 cm/s

Kx = 2.3 105 mol/cm2 s

KL = 4.0 104 cm/s

Kx = 2.0 105 mol/cm2 s

Height of a mass transfer unit

36 cm

60 cm

Flow velocity.

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G. Zhang et al. / Separation and Purification Technology 56 (2007) 143149

Fig. 6. Variation of resistances of mass-transfer with F-factor. The data implies

the relationship of different mass-transfer coefficients, which was based on a
concentration difference as a driving force. , 1/KL ; , cL /Kx ; , 1/HkG ; ,
1/HkM ; , 1/kL .

terize performance of distillation packing as conventional cases

[1,18], it is a flow parameter and usually defined as:
1/2

F = uG G

(14)

where uG is the vapor velocity and G is the vapor density. It

was observed that the liquid side was responsible for almost
half of the total resistance, and the resistance in the gas side
was the least, which was similar to the conventional distillation
process at the lowest concentration where the liquid resistance
was the dominating contribution [19]. In these cases, the highest resistance occurred at the bottom of the column and sharply
decreased towards the top of the column. Since the modules used
in this experiment was very short and the feed concentration was
very low, it was clear from Eq. (6) that the higher values of partition coefficient H of 3 103 , compared with former value
of 103 [7], might result in a controlling resistance. An only
blemish in the calculation was the gap between theoretical 1/KL
and experimental cL /Kx (=1/KL,exp ). This seemed that the experimental condition was very different from the conditions set by
the above theories. For example, as the mass transfer coefficient
across the membrane dependent on the void fraction of the wall
and the thickness of the membrane, the real value of kM was
strongly controlled by the distribution of materials and the liquid filled in the pore. Further, the curvity of the fibers caused
in the distillation process might have great effect on vapor mass
transfer. Therefore, more experiments were needed to testify the
results.
By simplifying the mathematics, the calculated kL could be
approximately used as the overall mass transfer coefficient KL
with an additional assumption that 1/kL was very large compared
to 1/HkM and 1/HkG (see Eq. (6)), which meant the total resistance was dominated by the liquid side, even if mass transfer
resistance in the membrane and the vapor could not be negligible in the meantime. The result was shown in Fig. 7. All of
the experimental Sherwood numbers which based on the liquid
side Kx were higher than the calculated values based on Leveque

Fig. 7. Mass-transfer coefficients for hollow fiber modules. Both the Sherwood
and Graetz numbers were based on the fiber diameter. , Experimental Sherwood number which the liquid side dominates;  and solid line, calculated
Sherwood number based on Leveque correlation.

correlation. The gap turned to be smaller when the Graetz number was low. Although the Leveque correlation was theoretical
strong for laminar flow through circular tube, the results of this
experiment tended to give a higher parameter than 1.62, which
was similar to the former empirical value of Sieder and Tate
[3,20]. Since the fibers used in this experiment was organic, the
random fiber packing might be uneven along the module length
and the fiber tube could be a tortuous path after heating and solvating. Under these circumstances, how to increase the packing
interfacial area as large as possible and how to keep the shape
of fibers and module flow path in the operation was very important. The geometry change of hollow fiber membrane especially
under the high temperature and solvation effect should be paid
more attention in the following research.
5. Conclusion
The distillation in the hollow fibers showed excellent performances over conventional structured packing for the separation
of methanol/water solutions. Since the wall of the hollow fibers
was non-porous but highly permeable, they could define the
flows very well but did not compromise the mass transfer.
The vapor and liquid flows were largely independent of the
normal constraints of fluid mechanics, therefore the modules
could be operated successfully at conditions, which normally
caused severe operational problems such as emulsions, foaming,
unloading and flooding. Further, the minimum HTU of only 8 cm
at the lowest vapor velocity of 116 cm/s (KL,exp = 0.001 cm/s)
represented a higher separation efficiency, while the largest HTU
of 36 cm at the highest flow of 223 cm/s (KL,exp = 0.0016 cm/s)
was only a mediocre value which could be given by conventional packing. All these results demonstrated more productive
and higher efficient separations in hollow fibers.

G. Zhang et al. / Separation and Purification Technology 56 (2007) 143149

The overall mass-transfer coefficient Kx based on the

liquid-side, which was 2.3 105 mol/cm2 s, was obtained
experimentally and compared with theoretical estimation. It was
found that the liquid side was dominantly responsible for the
total resistance, which was similar to the conventional distillation process at the lowest concentration, although mass transfer
resistance in the membrane and the vapor could not be negligible. For tube side flow, the experimental results tended to give a
higher parameter of Leveque mass transfer correlation. Even if
the mass transfer coefficients demonstrated were typical values,
the transfer rates should be higher than normal with a large interfacial area in hollow fiber packing, and therefore would make
very different separation in industry.
Acknowledgements
The authors thank Dr. E.L. Cussler for useful discussions
while visiting CEMS, UMN. This work was primarily funded
by the Research Fund of the National Natural Foundation of
China (grant 20476096). Other financial support came from the
Zhejiang Provincial Bureau of Science and Technology, China
(grants 2005C3304 and 2006C23067).
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