Computers and Chemical Engineering 71 (2014) 210219

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Computers and Chemical Engineering
j our nal home page: www. el sevi er . com/ l ocat e/ compchemeng
Ionic liquid effects on mass transfer efciency in extractive distillation
of waterethanol mixtures
E. Quijada-Maldonado
a,
, G. Wytze Meindersma
b
, Andr B. de Haan
c
a
University of Santiago de Chile, Department of Chemical Engineering, Av. Lib. Bdo. OHiggins 3363, Estacin Central, Santiago, Chile
b
Eindhoven University of Technology, Department of Chemistry and Chemical Engineering, Eindhoven, The Netherlands
c
Delft University of Technology, Faculty of Applied Sciences, Department of Chemical Engineering, Delft, The Netherlands
a r t i c l e i n f o
Article history:
Received 13 September 2013
Received in revised form30 July 2014
Accepted 2 August 2014
Available online 11 August 2014
Keywords:
Rate-based model
Extractive distillation
Ionic liquids
Mass transfer efciency
Waterethanol separation
ASPEN

simulations
a b s t r a c t
The relatively high viscosities of ionic liquids could reduce the mass transfer efciency of the extractive
distillation process. The rate-based model was adopted to analyze this phenomenon since it predicted the
performance of an extractive distillation pilot plant using ionic liquids as solvent. For the waterethanol
separation, three ionic liquids: 1-ethyl-3-methylimidazolium chloride, 1-ethyl-3-methylimidazolium
acetate and 1-ethyl-3-methylimidazolium dicyanamide and the organic solvent ethylene glycol were
used for the analysis. Simulations were conducted for sieve trays and Mellapak

250Y. The results indi-

cate that relatively high viscosities affect the mass transfer efciency. However, the improvements in
relative volatilities obtained from the ionic liquids help to overcome this effect. However, with high sol-
vent viscosities (>65 mPa s at T =353.15 K) it was not possible to overcome the reductions. Additionally, at
higher distillate rates high relative volatilities yielded negative effects on mass transfer efciency because
of a decrease in vapor velocity.
2014 Elsevier Ltd. All rights reserved.
1. Introduction
Extractive distillation (ED) is an energy efcient technology that
allows the separation of complex mixtures by the addition of a sol-
vent at the top of the column that modies the activity coefcients
at the liquid phase to increase the relative volatilities. Fig. 1 depicts
a scheme of a conventional ED process including solvent recovery
step.
Most of the solvents used in the ED process are volatile organic
uids. Ionic liquids have lately become a real alternative as sol-
vent in extractive distillation because efforts have already been
made to successfully bring fundamental vaporliquid equilibrium
experiments to pilot plant scale experiments (Meindersma et al.,
2012). This has become possible due to their properties such as
high selectivity in ED process and negligible vapor pressure result-
ing in high recyclability and no solvent loss (Verma and Banerjee,
2010; Lei et al., 2003; Pereiroet al., 2012; Roughtonet al., 2012). The
higher selectivity requires less reux ratio and therefore less boil
up making the ionic liquids more energy efcient solvents than the

Corresponding author. Tel.: +56 227181801.

E-mail address: esteban.quijada@usach.cl (E. Quijada-Maldonado).
common solvents (Meindersma et al., 2012; Quijada-Maldonado
et al., 2013a). Furthermore, the high selectivity allows decreasing
the number of separation stages due to the increased relative
volatilities. This advantage brings reductions of capital costs and
reductions in ionic liquid usage to achieve a desired purity. Despite
the above mentioned advantages, ionic liquids show high liquid
viscosity and this could bring mass transfer limitations to the sep-
aration process.
It is recognized that increased viscosity of a solvent in ED
lowers the mass transfer efciency of the process. This is a very
important parameter in the design of a ED column because a
lower efciency leads to columns with more trays or higher
packing to achieve a required separation. This problem becomes
more important when applying ionic liquids as solvents in ED
because their viscosities can be up to 20 times higher com-
pared to the commonly used organic solvents. Other properties
such us density, surface tension and thermal conductivities are
similar to the common organic solvents (Quijada-Maldonado
et al., 2012, 2013a,b). So then, there will not be mass transfer
efciency differences between ionic liquids and common sol-
vents produced by these properties. Several studies have pointed
out the high viscosity of ionic liquids as a reason to discard
promising ionic liquids inspite of their excellent vaporliquidequi-
libriumperformance (Ge et al., 2008). There are three phenomena
http://dx.doi.org/10.1016/j.compchemeng.2014.08.002
0098-1354/ 2014 Elsevier Ltd. All rights reserved.
E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219 211
Fig. 1. Scheme of a conventional extractive distillationunit andthe solvent recovery
step.
that could help to reduce this fear for reduced mass transfer ef-
ciency:
1. The solvent is dissolved in the mixture to be separated, which
strongly decreases the solvent viscosity (Quijada-Maldonado
et al., 2012; Gomez et al., 2006a,b).
2. The high temperatures inside the ED column considerably
reduce the viscosity of ionic liquids (Quijada-Maldonado et al.,
2012).
3. The improvements in relative volatility over conventional sol-
vents help to reduce the number of separation stages which
could compensate for the negative effect of viscosity (Quijada-
Maldonado et al., 2013a).
However, the knowledge about the effect of solvent viscosity
on mass transfer efciency in distillation is fairly limited. Only one
study experimentally showed this effect (Weiss and Arlt, 1987).
In classical distillation operations, only a few studies have related
the effect of viscosity to mass transfer efciency (OConnell, 1946;
Bocker and Ronge, 2005). Furthermore, the effect of the solvent
viscosity onmass transfer efciency is not studiedyet for extractive
distillation with ionic liquids.
Therefore, the objective of this paper is to study the effect of the
solvent viscosity on the mass transfer efciency in the ED process
for the waterethanol mixture using several ionic liquids and the
commonly used organic solvent ethylene glycol (EG) by means of
a rigorous rate-based mass transfer model. In our previous work
(Quijada-Maldonado et al., 2013a) it was demonstrated that the
developed rated-based model to describe this separation using 1-
ethyl-3-methylimidazolium dicyanamide, [emim][DCA], was able
to predict the performance of an extractive distillation pilot plant
while only knowing the physical, transport and vaporliquid equi-
librium(VLE) properties of the system. Therefore, this model allows
the analysis of a possible decrease in mass transfer efciency with
solvent viscosity. On the other hand, the use of various ionic liq-
uids allows the study of a wide range of solvent viscosities and
relative volatilities. Therefore, the combined effect of viscosity and
relative volatility on mass transfer efciency is studied. Addition-
ally, the mass transfer efciency of sieve trays and Mellapak

250Y structured packing are compared and two solvent-to-feed

ratios evaluated to increase the liquid phase viscosities inside
the ED column as this is the most important operating variable
when higher purities are desired. Finally, the recovery of the ionic
Table 1
Relative volatilities, , at different S/F ratios (mass basis) for different solvents cal-
culated at the waterethanol azeotropic point and pure solvent viscosities, , at
T =298.15 and 353.15K.
Solvent [mPa s]
S/F =1 S/F =2 Ref. T =298.15K T =353.15K Ref.
[emim][Cl] 2.62 3.98
b
2597.69
a
65.18
c
[emim][OAc] 2.24 2.92
b
132.91 13.60
d
[emim][DCA] 1.89 2.58
b
14.90 4.66
d
EG 1.83 2.41 ASPEN

16.61 3.14
e
a
Extrapolated viscosity fromthree experimental data points.
b
Ge et al. (2008).
c
Fendt et al. (2010).
d
Quijada-Maldonado et al. (2012).
e
Quijada-Maldonado et al. (2013b).
liquids (see Fig. 1) has been studied elsewhere (Meindersma et al.,
2012; Jongmans et al., 2012). Hence, it is not studied in this work.
2. Case study
The separation of waterethanol mixtures by means of ED has
been an important research topic for years due to applicability
of ethanol as biofuel (Garcia-Herreros et al., 2011; Lee and Pahl,
1985; Ravagnani et al., 2010; Ligero and Ravagnani, 2003; Li and
Bai, 2012; Huang et al., 2008; Kumar et al., 2010; Gil et al., 2012;
Maciel andBrito, 2011). Table1shows thechangeinrelativevolatil-
ity of the waterethanol mixture at two different solvent-to-feed
ratios (S/F) calculatedat the azeotropic point using the NRTL model.
From this table it is observed that at both S/F ratios the order
is [emim][Cl] >[emim][OAc] >[emim][DCA] >[EG]. Eventually, the
best candidate to be chosenas a solvent wouldbe [emim][Cl] due to
the highest achieved relative volatilities followed by [emim][OAc].
This means that, anEDcolumnoperatingwith[emim][Cl] as solvent
would require less stages to achieve a required ethanol purity at
the top. Table 1 also lists the viscosities of the solvents at T =298.15
and 353.15K. Especially for [emim][Cl] relatively high values are
observed that could limit the mass transport. Here on the contrary,
a column operating with this solvent would need more separation
stages to obtain a certain ethanol top purity. However, at higher
temperatures a drastic viscosity decrease is observed. Besides that,
the solvent concentration is reduced in the mixture. For these con-
ditions the actual decrease in mass transfer efciency needs to be
analyzed.
The study of mass transfer efciency comprises the analysis of
the overall number of transfer units for trays and the overall height
of transfer units for packing:
E
OV
= exp(N
OV
) (1)
HETP = H
OV
ln()
1
(2)
1
N
OV
=
1
N
V
+

N

L
(3)
H
OV
= H
V
+H
L
(4)
where HETP is the height equivalent to a theoretical plate that rep-
resents the mass transfer efciencyof a packedcolumn; H
OV
, H
L
and
H
V
aretheoverall, liquidsideandvapor sideheight of transfer units;
N
OV
, N
L
and N
V
are the overall, liquid side and vapor side number of
transfer units and is the stripping factor. Eqs. (1)(4) describe the
change in efciency with physical properties, vaporliquid equilib-
rium and the column internals for both trays and packing. These
equations are used to compare the mass transfer efciency perfor-
mance of the different solvents studied in this work. The number
of transfer units and the height of transfer units present in Eqs.
212 E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219
(1)(4) are calculatedusing (ChanandFair, 1984, 1985) mass trans-
fer correlation for trays and (Rocha et al., 1993, 1996) for packing.
The distribution ratio is calculated using the NRTL model (Ge et al.,
2008).
3. Simulation setup
3.1. Physical properties
ASPEN

Plus radfrac with the rate-sep package enables the

use of the rate-based model to accurately evaluate the effect
of the solvent on the mass transfer efciency in the ED pro-
cess. This model needs physical and transport properties of the
mixture waterethanolsolvent to be provided. In our previ-
ous work (Quijada-Maldonado et al., 2013a) it was established
that ternary viscosities at several temperatures, ternary surface
tension data at room temperature and innite dilution diffu-
sion coefcients were the minimum requirement to accurately
predict the changes in mass transfer efciency with the sol-
vent viscosity. In this work, binary viscosities of the system
water[emim][Cl] and ethanol[emim][Cl] were experimentally
measured at several temperatures. With the help of binary vis-
cosity data for the binary mixture waterethanol (Belda et al.,
2004) it is possible to calculate the ternary viscosity of the
mixture waterethanol[emim][Cl]. The experimental method-
ology to determine liquid dynamic viscosities is described in
detail in our previous work (Quijada-Maldonado et al., 2012).
Table 2 summarizes the measured densities and dynamic viscosi-
ties at several temperatures. Secondly, ternary surface tension
data at room temperature are necessary to correctly predict the
mass transfer especially in structured packing. Therefore, ternary
surface tension data were experimentally determined for the sys-
tems waterethanol[emim][OAc] andwaterethanol[emim][Cl].
Table 3 summarizes the measured surface tension data. The exper-
imental procedure is described in (Quijada-Maldonado et al.,
2013a). The ternary dynamic viscosities and surface tension for the
other solvents were reportedpreviously (Quijada-Maldonadoet al.,
2012, 2013a,b). Finally, innite dilution diffusion coefcients are
provided in this work for innite dilution diffusion coefcients of
[emim][Cl] inwater andinethanol and[emim][OAc] inwater andin
ethanol. This propertywas measuredbymeans of determiningelec-
trical conductivities experimentally as explained in (Wong et al.,
2008). In our previous work (Quijada-Maldonado et al., 2013a) in-
nite dilutiondiffusioncoefcients were presentedfor [emim][DCA]
in water and in ethanol. Table 4 gives the measured data at several
temperatures.
Next, it was necessary to correlate the experimental data with
models available in literature. These models use parameters which
were regressed with the experimental data using the non-linear
square method. Eq. (5) is the objective function.
obj =
nexp

i=1
|
i,exp

i,calc
|

i,exp
(5)
where
i
represents any property. Binary viscosities were cor-
related using EyringPatelTeja model (Lee et al., 1999) with a
Margules type mixing rule (Eqs. (6) and (7)).
a
i,k
= [1 x
i
l
i,k
x
k
l
k,i
](a
i
a
k
)
0.5
(6)
l
i,k
= l
(1)
i,k
+
l
(1)
i,k
T
(7)
The binary parameter l
i,k
is regressed with the experimental binary
viscosities, x
i
is the mole fraction, T is the temperature and a
i
is a
parameter from the PatelTeja equation of state. Eq. (7) accounts
for the strong changes in viscosity with temperature. The regressed
Table 2
Experimental densities, , and dynamic viscosities, , of the binary mixtures (x
1
water +(1x
1
)[emim][Cl]) and (x
2
ethanol +(1x
2
)[emim][Cl]) at several temper-
atures being x
1
the mole fraction of water and x
2
the mole fraction of ethanol.
x
1
[gcm
3
] [mPa s] x
2
[gcm
3
] [mPa s]
T=323.15K
0.2963 1.12494 63.98 0.1306 1.10890 76.15
0.3946 1.12687 38.76 0.1997 1.10005 53.58
0.4933 1.12251 22.09 0.2652 1.08923 37.70
0.5818 1.11914 15.28 0.3356 1.07200 25.70
0.6211 1.11410 12.45 0.4001 1.05301 18.61
0.6715 1.10978 8.31 0.4769 1.03429 12.48
0.7407 1.09993 5.66 0.5335 1.01479 9.39
0.8002 1.08858 4.00 0.6000 0.99543 6.53
0.8665 1.06715 2.42 0.6683 0.96865 4.58
0.9344 1.02683 1.49 0.7336 0.94036 3.20
0.8012 0.91146 2.26
0.8670 0.86755 1.60
0.9333 0.82059 1.10
T =333.15K
0.2963 1.11939 41.04 0.1306 1.11994 58.76
0.3946 1.12355 28.51 0.1997 1.10437 41.89
0.4933 1.11693 15.95 0.2652 1.08559 29.86
0.5818 1.11351 11.47 0.3356 1.06568 20.42
0.6211 1.10836 9.41 0.4001 1.04692 15.01
0.6715 1.10396 6.51 0.4769 1.02815 10.30
0.7407 1.09439 4.42 0.5335 1.00861 7.88
0.8002 1.08249 3.18 0.6000 0.98906 5.56
0.8665 1.06107 2.10 0.6683 0.96216 3.98
0.9344 1.02031 1.01 0.7336 0.93329 2.81
0.8012 0.89754 2.00
0.8670 0.85976 1.42
0.9333 0.81210 0.97
T =343.15K
0.2963 1.11392 27.82 0.1306 1.09119 41.93
0.3946 1.11590 19.70 0.1997 1.08296 30.46
0.4933 1.11140 11.96 0.2652 1.07192 22.13
0.5818 1.10790 8.83 0.3356 1.05940 15.14
0.6211 1.10265 7.32 0.4001 1.04083 11.42
0.6715 1.09813 5.08 0.4769 1.02226 8.13
0.7407 1.08839 3.52 0.5335 1.00252 6.37
0.8002 1.07635 2.60 0.6000 0.98278 4.60
0.8665 1.05463 1.81 0.6683 0.95567 3.37
0.9344 1.01490 0.86 0.7336 0.92633 2.42
0.8012 0.88352 1.75
0.8670 0.85214 1.24
0.9333 0.80388 0.85
T =358.15K
0.2963 1.10585 16.96
0.3946 1.10788 12.30
0.4933 1.10322 8.22
0.5818 1.09958 6.26
0.6211 1.09410 5.27
0.6715 1.08941 3.75
0.7407 1.07935 2.64
0.8002 1.06706 2.01
0.8665 1.04406 1.36
0.9344 0.99934 0.68
Standard uncertainties u are u(T) =0.003, u(x) =5E05, u() =1E05 and the relative
standard uncertainty ur in ur() =0.0038.
parameters and the average deviation fromthe experimental data
are shown in Table 5. The ternary surface tension data were corre-
lated using FuLeeWang mixing rule (Jufu et al., 1986) depicted
in Eq. (8).
=
n

i=1
x
i

n
j=1
l
ij
x
j

i=1
n

j=1
x
i
x
j
|
i

j
|

n
m=1
l
im
x
m

n
r=1
l
jr
x
r
(8)
where
i
is the component surface tension at any temperature, x
i
is the mole fraction and l
i,j
is the binary parameter that is regressed
with the experimental data. Table 6 provides the regressed
E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219 213
Table 3
Experimental surface tension, , for the system systems (x
1
water +x
2
ethanol +1(x
1
+x
2
)[emim][Cl]) and system (x
1
water +x
2
ethanol +1(x
1
+x
2
)[emim][OAc]) at around T =298.15K.
T [K] st x
1
x
2
[mN m
1
] st
298.0 0.17 0.8553 0.0343 42.40 0.36
298.7 0.26 0.8977 0.0037 50.73 0.06
296.8 0.20 0.6163 0.2845 28.47 0.06
297.1 0.15 0.8033 0.0968 36.77 0.15
297.4 0.10 0.8969 0.0033 51.67 0.21
297.5 0.15 0.7706 0.0535 38.17 0.12
297.1 0.20 0.7167 0.0984 37.53 0.06
297.6 0.06 0.8017 0.0081 54.97 0.15
297.4 0.17 0.6577 0.1510 34.07 0.06
297.7 0.17 0.7311 0.0475 45.83 0.30
296.6 0.35 0.0967 0.6870 27.43 0.06
297.3 0.20 0.1621 0.5689 29.13 0.06
298.2 0.06 0.8607 0.0671 32.23 0.35
298.9 0.36 0.6972 0.2312 29.10 0.00
298.7 0.25 0.8811 0.0350 40.60 0.30
298.8 0.43 0.9111 0.0035 44.85 0.97
298.5 0.17 0.7375 0.1646 31.50 0.00
298.8 0.15 0.8061 0.0454 40.37 0.21
298.3 0.06 0.7525 0.0942 36.37 0.06
298.5 0.43 0.8478 0.0046 35.77 0.31
298.6 0.15 0.6802 0.1552 33.50 0.00
298.2 0.15 0.7797 0.0302 41.30 0.20
297.0 0.15 0.1088 0.7030 27.50 0.00
Table 4
Innite dilution diffusion coefcients of [emim][Cl] and [emim][OAc] in water and
ethanol, obtained measuring electrical conductivities.
T [K] Water Ethanol
[emim][Cl] [emim][OAc] [emim][Cl] [emim][OAc]
298.15 1.462 1.042 0.582 0.553
303.15 1.666 1.183 0.648 0.617
308.15 1.877 1.329 0.715 0.682
313.15 2.094 1.479 0.785 0.751
318.15 2.319 1.633 0.857 0.821
323.15 2.551 1.791 0.932 0.894
Table 5
Interaction parameters l
ij
of the Margules type mixing rule to calculate ternary
viscosities for the systemwater(1) +ethanol(2) +[emim][Cl](3) using temperature-
dependent interactions parameters.
Binary parameter l
(1)
ij
l
(2)
ij
l
(1)
ji
l
(2)
ji
l
12
0 0 0.2565 116.09
l
13
2.4909 803.94 1.3671 398.59
l
23
4.389 1569 1.7407 687.86
%ADD
a
6.18
a
%ADD=100|
calc
exp|/exp.
Table 6
Binary parameters l
ij
of the FuLiWang mixing rule to calculate ternary surface
tension at any temperature.
Binary parameter [emim][OAc] [emim][Cl]
Value Value
l
12
29.0231 52.3295
l
21
0.0626 2.4858
l
13
8.4685 8.6310
l
31
1.0605 0.0838
l
23
0.2066 22.1832
l
32
2.4044 0.2095
%ADD 3.27 3.51
%ADD=100|
calc
exp|/exp.
Table 7
Regressed parameter of Eq. (9) and the sumof squared errors (SSE).
Solvent Water
Solute a b c SSE
[emim][OAc] 0.1577 0.02195 8.357e005 1.786e007
[emim][Cl] 1.967 0.04343 0.00014 3.429e007
Solvent Ethanol
Solute a b c SSE
[emim][OAc] 0.9613 0.01521 4.643e005 5.214e007
[emim][Cl] 0.8865 0.01486 4.643e005 4.071e007
parameters. The innite dilution diffusion coefcients are easily
correlated with a second order polynomial as shown in Eq. (9).

0
i,j
= a +bT +cT
2
(9)
where
0
i,j
is the innite dilution diffusion coefcient, T is the tem-
perature and a, b, c are the regressing parameters. Table 7 lists the
regressed parameters and the average deviation from the experi-
mental data.
3.2. Process parameters
To select the process parameters some simple criteria have been
takenintoaccount. Inorder tocomparesolvents theprocess param-
eters are the same for all the solvents and internals. The most
important process parameter to study a possible decrease in mass
transfer efciency by the effect of liquid phase viscosity is the S/F
ratio. Two S/F ratios are used to increase the liquid phase viscos-
ity in the column and also to increase the effect of the solvent
on the separation (Ge et al., 2008). Additionally, the effect of the
vaporliquid ratio on mass transfer efciency is analyzed since this
property strongly depends on the vaporliquid equilibriumperfor-
mance provided by the solvent. Ionic liquids show improvements
in relative volatility with regard to the common organic solvents as
it was observed in Table 1. These improvements lead to a different
vaporliquid ratio inside the EDcolumn. This could have an impact
onmass transfer efciency as well. Therefore, twodistillate-to-feed
ratios (D/F) are selected.
The other process parameters are the feed ow rate, feed con-
centration, feed temperature and the reux ratio. The rst of these
parameters is the feed ow rate which should allow to use a rela-
tively small column diameter to assume that the liquid on the tray
is completely mixed in the horizontal direction and thus the tray
efciency is the same as the point efciency (Lockett, 1986; Taylor
and Krishna, 1993). The feed concentration was set at 50% (w/w).
Next, the feed and solvent temperatures are unimportant param-
eters in mass transfer efciency. However, the used temperature
should be close to the temperatures inside the ED column. Finally
the reux ratio was set at a xed number. It is worth noting that,
the scope of this work is to study the effect of relative volatilities
and solvent viscosity on mass transfer efciency. Therefore, these
process parameters were used without an optimization. Table 8
resumes the process parameters.
Sieve trays and Mellapak

250Y are the selected internals for

this study. Sieve trays are the most commonly used internal in
industryandthe mass transfer correlationis verywell known(Chan
and Fair, 1984, 1985). On the other hand, Mellapak

250Y is the
standard structured packing and also the mass transfer correlation
and parameters used in it are very well known in literature (Rocha
et al., 1993, 1996). The chosen owmodels for themare plug ow
and countercurrent respectively. Table 9 summarizes the features
of these internals that were taken with the purpose to decrease to
214 E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219
Table 8
Operating conditions.
Variable Value
Feed owrate [kgh
1
] 100
Ethanol concentration at feed [wt%] 50
Feed temperature [

C] 70
Solvent temperature [

C] 70
Distillate-to-feed ratio (mass) 0.4 and 0.5
Solvent-to-feed ratio (mass) 1 and 2
Reux ratio 2
Condenser pressure Atmospheric
Table 9
Used column internal characteristics in the simulations for 100kgh
1
of mixture
and 50wt% ethanol as a base owand feeding concentration respectively.
Parameter Value
Sieve tray
Tray spacing [m] 0.5
Number of stages (real stages including reboiler and condenser) 22
Feed tray 12
Solvent tray 2
Weir heights [m] 0.05
Hole diameter [m] 0.005
Deck thickness 10gauge
Number of passes 1
Pitch Triangular
Hole area/active area 0.12
Flooding 70%
Mellapak

205Y structured packing

Packing height [m] 6
Feed point [m] 3
Packing material Stainless steal
Flooding 70%
the maximumextent the effect of other variables on mass transfer
efciency. In trays, the tray spacing is high enough to avoid liq-
uid entrainment and the tray layout (weir height, hole diameter)
avoids the possibility of having weeping. These two phenomena:
liquid entrainment and weeping are well documented to decrease
the mass transfer efciency elsewhere (Lockett, 1986). The rest of
the parameters like deck thickness, number of liquid passes and
the hole area-to-active area ratio were default values in ASPEN

Plus.
The feed stage was put in the middle. To set the packing height
in the packed column which is related somehow to the number
of stages in the tray column we applied the following relationship
(Kister et al., 2007):
H
P
= (HETP)N
real
E
O
(10)
Eq. (10) relates the number of real stages in a tray column with
the height of a packed column through the HETP and the section
efciency, E
O
. To our knowledge, values of section efciency or
Murphree tray efciency for ED of waterethanol mixtures with
EG or another organic solvent cannot be found in open literature.
However, section efciency values can be found in the literature
for the distillation of waterethanol mixtures in a plate column
(Rhodes and Slachman, 1937) where the value of section efciency
is approximately 70%. Next, the HETP value can also be obtained
from a Sulzer

brochure (Sulzer Chemtech, 2006). Thus, the HETP

for Mellapak

250Yis approximately0.4mfor atmospheric distilla-

tion. Therefore, the minimumpacking height required to represent
14 equilibrium stages as used in this work is 5.6m, which will be
rounded to 6m. Finally, the owrates in the sieve tray column and
packed column were set at 70% of the ooding owrates for all the
solvents. A summary is given in Table 9.
4. Results
4.1. Sieve tray column
First of all, the viscosity proles for all the solvents over the
column height are shown in Fig. 2 at two S/F ratios. The region
above tray 12 is the rectifying section (left side), and below it
is the stripping section (right side). In the rectifying section the
solvent concentrationis higher thaninthe stripping section. There-
fore, higher liquid phase viscosities are encountered. However,
a higher concentration of the solvent allows a better separa-
tion effect as well. Fig. 2a clearly shows the effect of the pure
solvent viscosity (see Table 1) on the resulting liquid phase vis-
cosities inside the column. The viscosity order in this zone being:
[emim][Cl] >[emim][OAc] >[emim][DCA] >EG. Inthe stripping sec-
tion the liquid viscosity drops for all four solvents as the solvent
concentration is reduced by dilution with the feed stream. All the
liquid phase viscosities inthis zone are comparable witheachother
having a value around 1mPa s. When increasing the S/F ratio to 2
(Fig. 2b), the proles showan obvious rise in liquid phase viscosity
again following the order of the pure solvent viscosities. In Fig. 2a
and b it is observed that at these S/F ratios the liquid phase vis-
cosities are not as high as could be expected because of the high
temperatures inside the ED column and the dilution of the solvent
in the waterethanol mixture.
The effect of the liquid phase viscosities on the mass transfer
coefcients is shown in Fig. 3 for both S/F ratios. In Fig. 3a it is
observed that the value of these coefcients followthe same order
as the liquid phase viscosity inside the columnindicating that there
is an effect of the solvent viscosity on mass transfer. In the stripping
section EG shows signicantly higher mass transfer efciency val-
ues than the ionic liquids who show similar values to each other.
This is due tothe higher temperatures nearbythe reboiler produced
by the evaporation of EG. These higher temperatures are because of
the lower water content whenusingEGthanthe columncontaining
anionic liquidincreasingtheboilingtemperature. Whenusingionic
liquids as solvent more water is extracted due to the hydrophilic
behavior of the presented ionic liquids. To show more clearly the
effect of viscosity on mass transfer, the S/F ratio is increased. Fig. 3b
conrms an overall decrease of all the mass transfer coefcient
proles by the increased liquid phase viscosities. However, the dif-
ferences betweenthe two S/F ratios are limited because anincrease
in the solvent concentration leads to an increase in the boiling
point of the mixture and thus the temperature proles. The higher
the temperature the lower the liquid phase viscosity and the less
resistance to mass transfer.
Fig. 4 shows the tray efciency proles over the ED column
calculated using Eq. (1). The rectifying section shows lower mass
transfer efciencies than the stripping section due to the effect of
solvent viscosity. At S/F =1(Fig. 4a) the differences betweenthe sol-
vents are relatively small, and the mass transfer efciency order is
[emim][OAc] >[emim][DCA] >EG>[emim][Cl]. This order does not
exactly follow the viscosity order shown in Fig. 2. Therefore, the
viscosity is not the only important effect in calculating the mass
transfer efciency as observed in Eq. (1). Table 1 gives the relative
volatility values at two S/F ratios. Ionic liquids are able to outper-
form the relative volatilities of the common organic solvents as it
has previously found in literature (Lei et al., 2003). In this table
it is observed that very good relative volatilities are produced by
[emim][OAc]. This property enhances the mass transfer efciency
even though having relatively high viscosity. However, [emim][Cl]
shows the highest relative volatility (see Table 1) and also very high
liquid phase viscosities (see Fig. 2a). Here, due to the high viscosi-
ties this property becomes the predominant factor in mass transfer
efciency. Therefore, moderately high viscosities are not an impor-
tant factor in mass transfer efciency when combined with high
E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219 215
4 8 12 16 20
0.5
1.0
1.5
2.0
2.5

[
m
P
a
s
]
[emim][Cl]
[emim][OAc]
[emim][DCA]
EG
a)
4 8 12 16 20
Tray number
b)
Stripping Stripping Rectifying Rectifying
Fig. 2. Viscosity proles along the column for (a) S/F =1 and (b) S/F =2 (mass basis) formed when the different solvents are added to the column and D/F =0.4 (mass basis).
4 8 12 16 20
0
2
4
6
8
10
Stripping Rectifying Rectifying
1
0
0
0
0
x
k

[
m
s
-
1
]
[emim][Cl]
[emim][OAc]
[emim][DCA]
EG
a)
4 8 12 16 20
Stripping
Tray number
b)
Fig. 3. Averaged-liquid-side mass transfer coefcient, k, proles over the column for (a) S/F =1 and (b) S/F =2 (mass basis) calculated for the different solvents added to the
column and D/F =0.4 (mass basis). The column is numbered fromthe top to the bottom.
values of relative volatility. However, the relative volatility does
not enhance mass transfer efciency sufciently in the presence of
a very viscous ionic liquid.
To support these observations the S/F ratio is increased
(Fig. 4b). In the rectifying section, the tray efciency order is
[emim][OAc] >[emim][DCA] [emim][Cl] >EG. Although, there is
an increase in liquid phase viscosity for this S/F ratio (see Fig. 2b),
[emim][OAc] does not show a signicant decrease in the tray ef-
ciency proles between S/F ratios because the increase of it also
produces an increase in relative volatility and this last property
is predominant in calculating the mass transfer efciency. This is
not seen for the rest of the solvents where the increase in liquid
phase viscosity does have an important impact on mass trans-
fer efciency. For example, EG exhibits a drastic decrease in tray
4 8 12 16 20
0.6
0.7
0.8
0.9
Rectifying Rectifying
E
O
V
[emim][Cl]
[emim][OAc]
[emim][DCA]
EG
a)
4 8 12 16 20
Tray number
b)
Stripping Stripping
Fig. 4. Tray efciency proles along the column for (a) S/F =1 and (b) S/F =2 (mass basis) calculated when the different solvents are added to the column and D/F =0.4 (mass
basis). The column is numbered fromthe top to the bottom.
216 E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219
4 8 12 16 20
0.6
0.7
0.8
0.9
E
O
V
[emim][Cl]
[emim][OAc]
[emim][DCA]
EG
b)
Stripping Stripping Rectifying
a)
4 8 12 16 20
Rectifying
Tray number
Fig. 5. Tray efciency proles along the column for (a) S/F =1 and (b) S/F =2 (mass basis) calculated when the different solvents are added to the column and D/F =0.5 (mass
basis).
efciency when increasing the S/F ratio. As observed in Table 1 EG
has a minor impact on the relative volatility when compared to
the rest of the solvents. Therefore, the changes in tray efciency
correspond directly with changes in the liquid phase viscosity. A
very interesting case is [emim][Cl]. The decrease in mass transfer
efciency is not as drastic as would be expected fromthe viscosity
increase alone. This is due to the large increase in relative volatility
at this S/F ratio (see Table 1) compensating the effect of viscosity
to some extent.
In the stripping section and for S/F =1, there is an increase in
mass transfer efciency for all the solvents since the solvent con-
centrationis reduced by dilutionwiththe feed streamand viscosity
is a less important issue. Indeed, there are no signicant differences
in mass transfer efciency between solvents. For S/F =2,
[emim][OAc] shows the highest tray efciency values and the
rest of the solvents showa slight decrease with regard to S/F =1.
The effect of the solvent on mass transfer efciency in the strip-
ping section could become more important at different operating
conditions. One example is the use of a higher D/F ratio to with-
drawmore vapor fromthe condenser. This is depicted in Fig. 5 that
shows the tray efciency proles for both S/F ratios at an increased
D/F ratio of 0.5 instead of 0.4.
From Fig. 5 it is clear that the rectyng section exhibits the
same trend as the previuos operating conditions (D/F =0.4). How-
ever, large differences in mass transfer efciency between D/F
ratios are observed in the stripping section especially at S/F =2
0.5
0.6
0.7
0.8
4 8 12 16 20
0.5
0.6
0.7
0.8
4 8 12 16 20
b)
Rectifying Rectifying Stripping Stripping
u
S
/
u
s
a
t

f
lo
o
d
in
g
[emim][Cl]
[emim][OAc]
[emim][Cl]
EG
a)
D/F = 0.4
Rectifying
b)
u
S
/
u
s
a
t

f
lo
o
d
in
g
Tray number
[emim][Cl]
[emim][OAc]
[emim][DCA]
EG
a)
D/F = 0.5
Stripping Stripping Rectifying
Fig. 6. Ratio vapor velocityvapor velocity at ooding proles for (a) S/F =1 and (b) S/F =2 (mass basis).
E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219 217
6 4 2
0.5
1.0
1.5
2.0
2.5
6 4 2 0

[
m
P
a

s
]
Packing height [m]
[emim][Cl]
[emim][OAc]
[emim][DCA]
a)
Stripping Stripping Rectifying Rectifying
b)
Fig. 7. Liquid phase viscosity proles along the column for (a) S/F =1 and (b) S/F =2 (mass basis) calculated when the different solvents are added to the column and D/F =0.4
(mass basis).
(Figs. 4b and 5b). At S/F =1 (Figs. 4a and 5a) the differences are
less noticeable. Let us focus on why these differences are produced.
When increasing the D/F ratio more vapor is withdrawn from the
condenser, mainly ethanol, increasing the less volatile components
at the bottomof the column: water and solvent. The watersolvent
concentration in this zone depends on the relative volatility of the
system. Then, the explanation is that the higher the relative volatil-
ity, the lower the ethanol concentration at the bottom. Since water
requires more energy to be evaporated, the mass transfer efciency
drops due to the decrease in the vapor velocity. Indeed, the drop
in the mass transfer efciency proles follows the inverse order
of those relative volatility values in Table 1. These decreases in
mass transfer efciency are more noticeable at S/F =2 since the
concentration of the solvent is higher than at S/F =1. At S/F =2 the
separation effect of the solvent on the mixture becomes stronger
and this decreases more the concentration of ethanol at the bottom
of the column and this produces even less vaporizable ethanol and
thus vapor velocity. This is observed in all the proles generated
when using ILs but more pronounced for the case of [emim][Cl]
with a drastic mass transfer efciency decrease at S/F =2. To show
the decrease in vapor velocity and therefore the decrease in mass
transfer eciency, Fig. 6 shows the ratio of vapor velocity/vapor
velocity at ooding (u
VS
/u
VS,ooding
) for both S/F ratios and both D/F
ratios. Markeddecreases invapor velocity are observedfor bothD/F
ratios and when using the ionic liquids. These decreases are more
marked at S/F =2 for both D/F ratios. However, at D/F =0.5 drastic
drops invapor velocity are observedfor bothS/F ratios. These drops
are even found in the rectifying section at S/F =2. The lower pro-
duction of vapor decreases the mass transfer efciency. Therefore,
the viscosity is not the only property that lowers the mass transfer
efciency in the rectifying section.
In conclusion the distribution ratios can play either a positive
or negative role in the separation of waterethanol mixtures. For
D/F =0.4 the distribution ratios can overcome mass transfer limita-
tions caused by moderately high liquid phase viscosities. However,
for D/F =0.5, adverse mass transfer efciencies are obtained when
using ionic liquids in the stripping section.
4.2. Mellapak

250Y structured packing

The mass transfer efciency of the waterethanol separation is
studied for the same operating conditions as the sieve tray column
but now using Mellapak

250Y structured packing. The analysis

will followthe same structure, meaning that, fromthe liquid phase
viscosity prole we analyze the posible decrease in mass transfer
efciency for D/F =0.4. Fig. 7 depicts the liquid phase viscosity pro-
les over the column. The same trends and viscosity values as with
the column containing sieve trays are observed because this prop-
erty does not depend upon the internals. Next, Fig. 8 shows the
average mass transfer coefcient proles over the column. These
coefcients drop in the rectifying section as compared to the strip-
ping section by the effect of liquid phase viscosity. The effect is
clearly observed with [emim][Cl] that shows the lowest values and
EG that shows the highest ones. This trend is the same as sieve
6 4 2
0.0
0.4
0.8
1.2
1.6
2.0
6 4 2 0
Stripping Rectifying
1
0
0
0
0
x
k
L

[
m
/
s
]
Packing height [m]
[emim][Cl]
[emim][OAc]
[emim][DCA]
a)
Stripping Rectifying
b)
Fig. 8. Averaged mass transfer coefcient proles along the column for (a) S/F =1 and (b) S/F =2 (mass basis) calculated when the different solvents are added to the column
and D/F =0.4 (mass basis).
218 E. Quijada-Maldonado et al. / Computers and Chemical Engineering 71 (2014) 210219
6 4 2
0.1
0.2
0.3
0.4
6 4 2 0
Stripping
H
E
T
P

[
m
]
Packing height [m]
[emim][Cl]
[emim][OAc]
[emim][DCA]
EG
a)
Stripping Rectifying Rectifying
b)
Fig. 9. HETP proles along the column for (a) S/F =1 and (b) S/F =2 (mass basis) calculated when the different solvents are added to the column and D/F =0.4 (mass basis).
trays. Additionally, two important facts are observed. First, similar
to sieve trays, the increase in S/F ratio does not produce a signi-
cant decrease in the mass transfer coefcient proles because of a
rise in the temperature proles (boiling points) that moderates the
increase in liquid phase viscosities. Asmall decrease is observed for
[emim][Cl]. Additionally, when increasing the S/F ratio, the super-
cial liquid velocities on the packing increase. This improves mass
transfer. Secondly, the mass transfer coefcients in packing are
lower than in sieve trays. This is because in sieve trays the vapor
ows upwardandvigorously bubbles throughthe liquidonthe tray
forming a turbulent vaporliquid dispersion. Additionally, a liquid
holdup is maintained on the tray. These characteristics create a
large vaporliquid contact area and high mass transfer coefcients.
Inapackedcoluminstead, acontinuous vaporliquidcontact is pro-
moted by the interfacial area. However, a lower liquid holdup and
therefore lower contact time between phases are achieved. As a
result lower mass transfer coefcients than in trays are obtained
(Dutta, 2007).
Fig. 9shows theHETPproles over thecolumn. Themass transfer
efciency order is [emim][OAc] >[emim][DCA] >[emim][Cl] >EGin
the rectifying section for both S/F ratios. The observation of these
proles does not produce different conclusions from sieve trays.
However, two important points are noticed. Firstly, in contrast to
sieve trays, improvements in mass transfer efciency when using
ILs are obtained when increasing the S/F ratio. This is explained
by the fact that in packed columns the liquid and vapor ow
are in countercurrent and the packing surface allows an intimate
vaporliquid contact. As a result, the packed distillation column
operates closer to equilibrium than sieve trays, and thereby the
effect of the relative volatility predominates over the increase in
liquid phase viscosity. Secondly, and continuing with this observa-
tion, EGpresents the lowest mass transfer efciency (highest HETP)
for bothS/F ratios due tothe lowincrement inrelative volatility and
the increase of liquid phase viscosity.
5. Conclusions
The mass transfer efciency in extractive distillation for the
separation of waterethanol mixtures using ionic liquids and the
reference organic solvent ethylene glycol (EG) was analyzedfor two
solvent-to-feedratios andtwointernals: Sieve trays andMellapak

250Y.
With both internals, the liquid phase viscosity inside the colum
has a limitedimpact onmass transfer coefcients. Whenincreasing
the solvent-to-feed ratio, there is a slight decrease in all the mass
transfer coefcient proles in sieve trays. In Mellapak

250Y, this
decrease is less pronounced.
In sieve trays, relatively high viscosities affect the mass trans-
fer efciency. However, the improvements in relative volatilities
shown by ionic liquids allow to overcome this effect. Very viscous
ionic liquids (>65mPa s at T =353.15K) lower the mass transfer
efciency no matter howhigh relative volatility.
Increased distillate-to-feed ratios produce drastic mass transfer
efciency drops in the stripping section when using ionic liquids as
solvent.
In Mellapak

250Y, also the relatively high viscosities decrease

the mass transfer efciency. Nevertheless, due to improvedrelative
volatilities the effect is the same as in sieve trays. Also here, the
increase in solvent-to-feed ratio enhances mass transfer efciency
when using ionic liquids.
Acknowledgement
Financial support from the SenterNovem, The Netherlands, is
kindly acknowledged.
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