Chemical Engineering and Processing 45 (2006) 747754

Experiment and prediction of breakthrough curves for packed

bed adsorption of water vapor on cornmeal
Hua Chang, Xi-Gang Yuan , Hua Tian, Ai-Wu Zeng
State Key Laboratory of Chemical Engineering, Chemical Engineering Research Center, School of Chemical Engineering and Technology,
Tianjin University, Tianjin 300072, PR China
Received 16 November 2005; accepted 5 March 2006
Available online 10 March 2006

Abstract
The adsorption isotherms of water vapor on cornmeal and the breakthrough curves at 82100 C were measured in a fixed-bed apparatus for
ethanol dehydration. Using the water isotherms measured and fitting the experimental data to fixed-bed model for breakthrough curve, the effective
diffusivity of water was obtained. The effective diffusivity was estimated and used to predict breakthrough curves at other adsorption conditions.
The controlling factor for mass-transfer resistance was discussed.
2006 Elsevier B.V. All rights reserved.

Keywords: Adsorption isotherm; Effective diffusivity; Ethanol dehydration; Breakthrough curve; Adsorption model

1. Introduction
Starchy materials can adsorb and remove water from alcohol
vapors to dry fuel grade ethanol in an energy-efficient man-
ner [14]. The adsorption and desorption of water on starchy
materials, especially, i.e. cornmeal, corn grits and pure starch,
for ethanol dehydration have been extensively studied [116].
The success of this dehydration method seems related to the
differences in the rate of adsorption, as well as differences in
the strength of interaction between each species and the adsor-
bent. Compounds which exhibit either weak interactions or slow
rates of adsorption are expected to be readily separated from
those that exhibit strong, relatively fast interactions with the
adsorbent [13,17]. Due to strong polar attraction between water
molecules and the hydroxyl groups of the adsorbent, water can
adsorb on the adsorbent faster and stronger than ethanol, which
is known as major mechanism for the selective adsorption of
water [9,13]. Corn grits have been used in large-scale fermenta-
tion alcohol plants producing fuel-grade ethanol [1821]. Works
on modified-starch material as desiccant for industrial applica-
Abbreviations: ads., adsorbent; concentr., concentration; Temp., tempera-
ture
Corresponding author. Tel.: +86 22 27404732; fax: +86 22 27404496.
E-mail address: yuanxg@tju.edu.cn (X.-G. Yuan).
tions in drying air using PSA (pressure swing adsorption) can
also be found recently [1720,22].
A number of studies have been published concerning the
adsorption behavior of water vapor on starchy material, includ-
ing the measurement of equilibrium isotherms and breakthrough
curves [2,4,8,13,16]. However, there has been little attempt to
correlate them with equilibrium and kinetic information except
work of Hills and Pirzada [23] for prediction of breakthrough
curves on steamed and flaked cornmeal. Our aim is to measure
the water isotherms in bench-scale apparatus and apply it to
process model for breakthrough curve prediction. By fitting the
experimental data to model of breakthrough curve, the effective
diffusivity of water was estimated and validated by predicting
breakthrough curves at some other operation conditions.
2. Experimental
The corn meals used as adsorbents are from Wuqing County
in north China, with a granularity of <0.45 mm. All the adsor-
bents were dried for 8 h in air-convection oven at 105 C. One
hundred and twenty grams of dried cornmeal were used in
all runs. To provide vapor feeds with different concentrations,
waterethanol mixtures with different concentrations were pre-
pared by mixing anhydrous ethanol and water.
Fig. 1 is the experimental apparatus used in this work. In
Fig. 1a, a transparent column of 0.9 m long and 0.025 m i.d.

0255-2701/$ see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2006.03.001
748 H. Chang et al. / Chemical Engineering and Processing 45 (2006) 747754
Fig. 1. Diagram of experimental apparatus for fixed-bed adsorption: (1) adsorber; (2) adsorbent; (3) support packing; (4) oil bath; (5) kettle and electro-heater; (6)
and (7) condenser; (8) voltage controller; (9) gas blowout; (10) cold trap; (11) cooling water; (12) rotameter.
with oil bath jacket was used as adsorber and packed with corn-
meal, which is supported from the bottom and covered from
the top by a layer of random packing, respectively. Thermo-
points are arranged along the axial direction of the column with
intervals of 0.1 m to measure the temperatures of the bed at the
corresponding positions. The kettle was heated by electro-heater
to provide the ethanolwater vapor feed. The superficial veloc-
ity of vapor in the adsorber was controlled through regulating
the voltage on the electro-heater with a voltage controller. The
temperatures were monitored by multi-road heat resistance con-
tact thermometer, the compositions of samples were analyzed
by HP5890 gas chromatogram workstation, and the mass of the
material was weighed by Mettler AE163 electrical scale with the
precision of 0.0001 g. The temperature of the adsorber was kept
well above the dew point of the vapor feed to avoid condensing.
The experiment was divided into two steps, the adsorption
step (Fig. 1a) and the desorption step (Fig. 1b). Using the appa-
ratus of Fig. 1a, 120 g adsorbent was packed in the adsorber and
the vapor feed went through the adsorber and the ethanol rich
product was collected at the outlet end of condenser 7. The adsor-
ber was operated for 300 min and the breakthrough curves can
be obtained by measuring the concentration of outlet solution at
intervals of set time.
When the adsorption operation had finished, the experiment
passed to step 2 where the adsorber was flushed by 106 C nitro-
gen gas for 240 min using the same apparatus but configured as
Fig. 1b. The desorbed material was collected in the cold trap that
was cooled by liquid nitrogen, weighed by Mettler AE163 and
analyzed by gas chromatogram. At the moment when the adsorp-
tion operation stopped, the void spaces in the system including
those within the bed and in the pipelines were supposed to be
full of vapor feed, which could be flushed to the cold trap during
the desorption operation, and then, should be subtracted from
the desorbate to correct the experimental data, assuming that
the ideal gas condition holds. Note that we assumed that quan-
tities of water and ethanol sorbed on the inner surface of the
shells of the column and tubes and on the support packing are
negligible compared to those collected in the cold trap. With the
assumption that the adsorbed ethanol and water at the first phase
almost completely desorbed at the second phase, the equilibrium
amount of water and ethanol adsorbed can be determined by the
quantity and the concentration of the desorbate.
The pipelines the vapor went through were heated by heat
tape to avoid condensing and the pipelines above the adsorber
were kept at little high temperature to prevent condensation back
to adsorber.
3. Models considered in this work
3.1. Linear adsorption isotherm
Assuming linear adsorption according to Henrys law for
dilute concentration of water, the adsorption isotherm for water
can be correlated as a linear adsorption isotherm, which is given
by
q = Kc (1)
where K is the adsorption equilibrium constant for a linear
adsorption isotherm and q denotes the mass of water adsorbed
in mol m3 adsorbent and c is the concentration of water in
mol m3 .
3.2. Model for breakthrough curves
The aim of the experiments was to attempt to predict mass-
transfer diffusivity and breakthrough curves from the measured
 H. Chang et al. / Chemical Engineering and Processing 45 (2006) 747754 749

adsorption isotherm. In the case of isothermal adsorption, the where = (kKZ/u) ((1 b )/b ) is the dimensionless distance
differential equations can be written as follows [24]. coordinate, = k(t(Z/u)) the dimensionless time coordinate,
and erf(x) is the error function that is defined as
3.2.1. Mass balance on water on an element of column
erf(x) = erf(x) (7)
A mass balance on the solute for the flow of fluid through  x
a differential adsorption-bed length, dZ over a differential time 2
e d
2
erf(x) = (8)
duration, dt, gives: 0
2 c (uc) c (1 b ) q and coordinate transformations for Z and t, convert the equa-
DL + + + =0 (2) tions to a much simpler form of erf(x). The approximation given
Z2 Z t b t
by Eq. (6) is known to be acceptable and the error could be
where the first term accounts for axial dispersion with eddy dif- within 0.6% for > 2.0.
fusivity DL , the second term permits an axial variation in fluid Klinkenberg model [24,25] has also included the following
velocity, and the fourth term that is based on q, the mass-average approximate solution for the profiles of solute concentration in
adsorbate loading per unit mass accounts for the variation of q equilibrium with the average sorbent loading:
throughout the adsorbent particle. Eq. (2) gives the concentra-
 
c q 1  1 1
tion of solute in the bulk fluid as a function of time and location = 1 + erf (9)
in the bed. cF qF 2 8 8
where c = q/K and c /cF = q/qF , where qF is the loading in
3.2.2. Linear driving force model for mass transfer [24] equilibrium with cF .
q
= k(q q) = kK(c c ) (3) The simple model of Klinkenberg, giving c/cF as a function
t of dimensionless time , and dimensionless bed length , was
where q* is the adsorbate loading in equilibrium with the solute not worse than more sophisticated models, and could be known
concentration c, in the bulk fluid. c* is the concentration in equi- as adequate for preliminary design purpose [26].
librium with average loading q; k is the overall mass-transfer The equilibrium constant K for a given temperature can be
coefficient in s1 , which includes both external and internal correlated by experimental data. By fitting the experimental
transport resistances; and K is the adsorption equilibrium con- breakthrough curves to Eq. (6), the overall mass-transfer coeffi-
stant for a linear adsorption isotherm in Eq. (1). cient k can be estimated. Then by Eqs. (4) and (5), the effective
diffusivity De can be evaluated. In addition, the breakthrough
3.2.3. Relationship for the factor Kk [24] curves at various conditions can be predicted by De which has
R2p been obtained.
1 Rp
= + (4)
kK 3kc 15De 4. Results and discussion
where kc is the external mass-transfer coefficient in m/s, De is
effective diffusivity in m2 /s and Rp is adsorbent particle radius All the results of the experiment were listed in Table 1. From
in m. The first term in Eq. (4) is the overall mass-transfer resis- the data in Table 1, considerable ethanol was also adsorbed on
tances, the second and third term is external one and internal the cornmeal in all runs, which must be recovered by recycling
one, respectively. to a distillation stage if it is used for the separation process.

3.2.4. The correlation for external mass-transfer coefcient 4.1. Linear model of adsorption isotherm for water
The external transport coefficient of particles in fixed-bed can
be correlated by [24]: The adsorption isotherms of water are shown in Fig. 2. By
fitting the experimental results of adsorption isotherm to the lin-
1/3
Sh = 2 + 1.1Re0.6 Sci (5) ear isotherm represented by Eq. (1), the adsorption equilibrium
constant at different temperatures was correlated and listed in
where Sh = Shrewoodnumber = Kc Dp /Di , Re = Reynolds num-
Table 2. From Fig. 2, it can be seen that the linear correlation
ber = Dp G/, and Sci = Schmidt number = /Di .
represent the isotherm fairly well with the value of the correla-
By Eq. (5), external mass-transfer coefficient kc can be esti-
tion coefficient R2 as 0.9666 for 91 C at dilute concentration of
mated from Sh.
water. The linear adsorption isotherms for water were used in the
The analytical solution of a simplified form of Eq. (2), in
prediction of breakthrough curves in after mentioned section.
which negligible axial dispersion, constant fluid velocity u, and
the linear driving force mass-transfer model were assumed, was 4.2. Prediction of effective diffusivity
summarized by Ruthven and discussed in detail by Klinkenberg
[25]. An adopted approximate solution is that of Klinkenberg By least square correlation:
[24]:
 2



   ci   ci 
c 1 1 1 min f (k) = (10)
1 + erf + + (6) cF cF experimental result
cF 2 8 8
750 H. Chang et al. / Chemical Engineering and Processing 45 (2006) 747754

Water adsorption capacity

q (mol H2 O/m3 ads.)

888.8398
1938.1697
817.5243
1318.8561
1374.6437
2118.8588
2636.8131
637.1892
1219.7844
capacity (g/g ads. 102 )
ethanol adsorption

Fig. 2. Adsorption isotherm for water and its linear model (solid line).
7.47
7.01
3.01
3.18
2.52
2.73
2.77
1.56
1.59
Water adsorption capacity

A fitted value of parameter k can be obtained as (ci /cF ) in Eq.

(6) is only a function of overall mass-transfer coefficient k at
(g/g ads. 102 )

the condition that other variables such as bed depth Z, equilib-

rium isotherm constant K, the bed void fraction b , and constant
velocity u, are known. The error for the model prediction with
1.89
4.11
1.74
2.80
2.92
4.50
5.60
1.35
2.59

optimum k can be expressed by

 n
The relative humidity


 ((ci /cF ) (ci /cF )experimental result )2
of ethanol, Pi /Pis


 i=1
Sy = (11)
n1
0.858
0.764
0.596
0.563
0.547
0.504
0.477
0.446
0.410

where Sy is standard deviation for the prediction to experimen-

tal result. The smaller the value of Sy , the better the effect of
The relative humidity

prediction.
Changing the value of k to minimize Eq. (10), the opti-
of water, Pi /Pis

mal k is obtained as 2.7813 103 s1 with Sy being 0.101

for the operation condition of bed temperature of 91 C, bed
0.133
0.294
0.091
0.163
0.208
0.304
0.381
0.065
0.153

depth 43 cm, superficial velocity of 1.64 cm/s and 6.2 wt.%

water concentration feed. The comparison of correlation break-
through curve and experimental one is shown in Fig. 3. The
Water concentration,

deviation from zero for experimental result at low can be

c (mol H2 O/m3 )

Note: temp.: temperature; ads.: adsorbent; concentr.: concentration.

explained by the measurement error from the humidity of

air. Using the same method, the overall mass-transfer coeffi-
cient k at different temperature can be estimated, and it was
2.3169
5.1122
2.1978
3.9232
4.9922
7.3120
9.1567
2.1142
5.0116

found that the values so obtained for k almost keeps con-

stant at 2.7813 103 s1 , with Sy being 0.057 and 0.086
for 82 and 100 C, respectively. The breakthrough curves for
Vapor feed concentr. of

the other two temperatures of 82 and 100 C are shown in

Figs. 4 and 5.
ethanol (%)

97.4
93.8
97.4
95.2
93.8
90.5
87.8
97.5
93.8
Run conditions and results

Table 2
Adsorption equilibrium constant in linear adsorption isotherms for water on
Bed temp.

cornmeal
Temperature ( C)
( C)

K
82
82
91
91
91
91
91
100
100

82 379.89
Run no.
Table 1

91 293.07
100 252.15
1
2
3
4
5
6
7
8
9
 H. Chang et al. / Chemical Engineering and Processing 45 (2006) 747754
Fig. 3. Comparison of breakthrough curves between experimental results ((
)
points) and Klinkenbergs model (solid line) (bed temperature of 91 C, bed
depth 43 cm, superficial velocity of 1.64 cm/s, water concentration feed of
6.2 wt.%).
Fig. 4. Comparison of breakthrough curves between experimental results ((
)
points) and Klinkenbergs model (solid line) (bed temperature of 82 C, bed
depth 43 cm, superficial velocity of 1.26 cm/s, water concentration feed of
6.2 wt.%).
Fig. 5. Comparison of breakthrough curves between experimental results ((
)
points) and Klinkenbergs model (solid line) (bed temperature of 100 C, bed
depth 43 cm, superficial velocity of 1.70 cm/s, water concentration feed of
6.2 wt.%).
751
Fig. 6. Prediction of breakthrough curves for different bed depths (solid line)
and comparison with experimental results (points) (bed temperature of 91 C,
superficial velocity is 1.60 cm/s, water concentration feed of 6.2 wt.%).
4.3. Predictions of breakthrough curves and comparison
with experimental results
Generally, Klinkenbergs [24] models, Eqs. (6) and (9), could
be used respectively to predict the breakthrough curves and pro-
files of solute concentration in equilibrium with the average
sorbent loading for different bed depth at same other operational
conditions. In this paper, we try to predict the breakthrough
curves for different bed depth, as well as different velocity
and different water vapor concentration by using the value of
k obtained in the foregoing section.
The breakthrough curve predictions for different bed depths
and the comparison with experimental data are shown in Fig. 6.
From Fig. 6, it can be seen that with the value of k as
2.7813 103 s1 , the breakthrough curves for similar velocity
but different bed depth can be well predicted with the calcu-
lated Sy from Eq. (11) being 0.052, 0.046, 0.045 and 0.051 for
22, 28, 43 and 46 cm bed depths, respectively. This indicates that
Klinkenbergs [24] model is quite adequate for our experimental
conditions, and that it is valuable for industrial applications. The
profiles of solute concentrations in equilibrium with the average
sorbent loading for different bed depths are shown in Fig. 7.
The shapes of the profiles of solute concentration in the bed
for different bed depths are similar with those of breakthrough
curves.
The breakthrough curve for large superficial velocity of
4.31 cm/s at 91 C was predicted in Fig. 8, and different water
concentration of vapor feed in Fig. 9. As seen from Fig. 8,
the model of Klinkenberg [24] gives a good fit to the experi-
mental points with Sy of 0.060 for the same concentration of
vapor feed but a different superficial velocity. Thus, in spite
of the sweeping assumption involved in Klinkenbergs [24]
model, direct measurement on a small sample can be used to
predict the breakthrough curves of a larger adsorber by means
of the numerical solution of the model. However, from Fig. 9,
Klinkenbergs [24] model cannot give perfect fit for different
vapor concentration. The corresponding values of Sy are 0.141,
0.143, and 0.242 for 9.5, 12, and 20 wt.% water concentration
feed, respectively. This indicates that with the water concentra-
752 H. Chang et al. / Chemical Engineering and Processing 45 (2006) 747754
Fig. 7. Prediction of profiles of solute concentration in equilibrium with the
average sorbent loading for different bed depths (bed temperature of 91 C,
superficial velocity is 1.60 cm/s, water concentration feed of 6.2 wt.%).
Fig. 8. Prediction of breakthrough curves for large velocity (solid line) and
comparison with experimental results ((
) points) (bed temperature of 91 C,
bed depth 43 cm, superficial velocity of 4.31 cm/s, water concentration feed of
6.2 wt.%).
Fig. 9. Prediction of breakthrough curves for different water concentrations
(solid line) and comparison with experimental results ((
) points) (bed temper-
ature of 91 C, bed depth 43 cm, superficial velocity of 1.80 cm/s).
Fig. 10. Comparison of breakthrough curves between experimental results ((
)
points) and Klinkenbergs model (solid line) with the updated k value (bed
temperature of 91 C, bed depth 43 cm, superficial velocity of 1.76 cm/s, water
concentration feed of 20 wt.%).
tion increases, the prediction is getting worse. If we assumed
that Sy larger than 0.11 is unacceptable, it can be concluded
that the value of k as 2.7813 103 s1 cannot be applied to
predict the breakthrough curves for different vapor concentra-
tions. A larger slope in the beginning of S-shape breakthrough
curves suggests a much larger mass-transfer rate than that in
the end. While at the end of the breakthrough curves, the small
slope in the end of S-shape breakthrough curves indicates that
adsorption rate becomes very small when adsorbent approach-
ing to equilibrium. In fact, the breakthrough curve prediction
from Klinkenberg model [24] is symmetrical. Even with an
updated value of k, which was obtained as 1.1125 103 s1
by re-minimize the criterion of Eq. (10) with the experimen-
tal results for 20 wt.% water concentration feed, the value of
Sy was as high as 0.177. The key here is that, the break-
through curve demonstrated under relative higher water con-
centration are becoming far from being symmetric and cannot
be predicted well with Klinkenberg model [24], as seen in
Fig. 10.
4.4. Analysis of mass-transfer resistance
According to Eq. (5), the external mass-transfer coefficient
for different operation conditions can be estimated. The esti-
mation results are listed in Table 3. From Table 3, the overall
mass-transfer resistance 1/kK increases with the increasing of
temperature, and the internal mass-transfer resistance is con-
trolling factor due to (R2p /15De ) (1/kK)  (Rp /3kc ) even
for large velocity at the end of breakthrough curves. This is con-
sistent with the fact that the overall mass-transfer coefficient
obtained at low superficial velocity can be used to predict well
the breakthrough curves for large superficial velocity, that is, the
overall mass-transfer coefficient is similar for both low velocity
and high velocity due to the fact that internal mass-transfer is
controlling factor. As a result, the estimated value for De is in
the order of 2.5 109 m2 s1 .
 H. Chang et al. / Chemical Engineering and Processing 45 (2006) 747754 753

Table 3
Values of parameters for different operation conditions

T ( C) K k ( 103 s1 ) u0 ( 102 m/s) b u ( 102 m/s) Rp ( 106 m) (kg/m3 ) ( 105 Pa s) Di ( 105 m2 /s)

82 379.89 2.7813 1.26 0.3 4.20 225 1.486 1.085 1.642

91 293.07 2.7813 1.64 0.3 5.47 225 1.443 1.111 1.736
91 293.07 2.7813 4.31 0.3 14.37 225 1.443 1.111 1.736
100 252.15 2.7813 1.70 0.3 5.67 225 1.421 1.137 1.809

T ( C) Re Sci Sh kc (m/s) 1/kK Rp /3kc ( 104 ) R2p /15De De ( 109 m2 /s)

82 2.589 0.445 3.486 0.127 0.946 5.898 0.946 3.568

91 3.194 0.444 3.684 0.142 1.227 5.278 1.226 2.752
91 8.395 0.444 5.007 0.193 1.227 3.883 1.226 2.752
100 3.186 0.443 3.680 0.148 1.426 5.071 1.425 2.368

5. Conclusions Re Reynolds number = Dp G/

Rp radius of adsorbent (m)
The adsorption isotherms for water at 82100 C was mea- Sy standard deviation for the prediction
sured in a fixed-bed apparatus. The water isotherms were lin- Sci Schmidt number = /Di
earized and applied to the prediction of breakthrough curves. Sh Sherwood number = kc Dp /Di
By fitting the experimental results of breakthrough curves to the u effective velocity of vapor (m/s)
model of Klinkenberg, the overall mass-transfer coefficient was u0 superficial velocity of vapor (m/s)
estimated as 2.7813 103 s1 and successfully used for the
prediction of breakthrough curves at different superficial veloc- Greek letters
ity and different bed depth, but cannot predict well the break- viscosity of vapor (Pa s)
through curves for different vapor concentration. The simple dimensionless distance coordinate
model of Klinkenberg, giving c/cF as a function of dimension- density of vapor (kg m3 )
less time , and dimensionless bed length , was not worse than dimensionless time coordinate corrected for displace-
the more sophisticated model, and could be known as adequate ment
for preliminary design purpose. The analysis of mass-transfer b bed void fraction
resistance indicated that water adsorption on cornmeal was con-
trolled by the internal mass-transfer resistance for both the low
and high velocity at the end of the breakthrough curves. References

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