Chemical Engineering and Processing 55 (2012) 29–39

Contents lists available at SciVerse ScienceDirect

Chemical Engineering and Processing:

Process Intensification
journal homepage: www.elsevier.com/locate/cep

A contribution to the experimental determination of mass transfer in

counter-current flow through ceramic sponges
Julia Grosse ∗ , Matthias Kind
Institute of Thermal Process Engineering, Karlsruhe Institute of Technology (KIT), Kaiserstrasse 12, D-76131 Karlsruhe, Germany

a r t i c l e i n f o a b s t r a c t

Article history: Ceramic sponges were explored with established test systems from literature concerning their mass
Received 23 May 2011 transfer coefficients and effective interfacial area in counter-current flow. Absorption of carbon dioxide
Received in revised form 5 February 2012 diluted with air in caustic soda solutions as well as desorption of carbon dioxide from water into air
Accepted 7 February 2012
are used. An analysis of the measurement methods concerning reliability of the results for sponges was
Available online 17 February 2012
performed. The focus was set on effects like wetting of the sponge structure, which have to be taken into
account for any further investigation of mass transfer characteristics in sponges.
Keywords:
© 2012 Elsevier B.V. All rights reserved.
Open-celled foam
Mass transfer coefficients
Effective interfacial area
Absorption
Method validation

1. Introduction
Solid sponges are a bi-continuous monolithic network struc-
ture with void fractions up to 0.95 and a wide range of pore sizes.
These properties make them interesting as packings in chemical
engineering. Literature on sponges as porous gas burners, solar
receivers or catalyst support can be found, and reviews on possible
applications were provided by different authors [1–3]. Neverthe-
less, only a limited number of reports on sponges as column
packings are published. The characterization of sponges as a new
packing material consists of two steps, first hydrodynamics and
operating range, and second mass transfer characteristics. Sev-
eral authors report about the hydrodynamic characterization of
sponges. Studies are published by Stemmet et al. [4,5] on metal
sponges of one porosity and several pore sizes as well as by Calvo
et al. [6] for one type of metal sponge and by Leveque et al. [7] for
a single type of ceramic sponge. Bonnet et al. [8] investigates only
the wet pressure drop in co-current flow of metallic sponges. An
extensive study on the hydrodynamics of various sponges is given
by the authors [9].
Concerning mass transfer experimental data is compiled by
Leveque et al. [7] for a single type of ceramic sponges with a distil-
lation test system. Stemmet et al. [10,11] published experimental
data for mass transfer in metal sponges in co-current flow and
∗ Corresponding author. Present address: BASF SE, D-67056 Ludwigshafen,
Germany.
E-mail address: julia frauke.grosse@web.de (J. Grosse).
calculated data for counter-current flow [5]. For the use of sponges
as a catalyst carrier, Tschentscher et al. [12] investigated the mass
transfer between gas and liquid phase in a rotating sponge reactor.
The conditions in this reactor are not comparable to a conventional
separation column, as the continuous phase in the reactor is the
liquid phase with a gas phase dispersed in bubbles, whereas the
continuous phase in separation columns is mostly the gas phase,
while the liquid might flow continuously in rivulets or be dispersed
in droplets. Furthermore the mass transfer between liquid and solid
phase has been the topic of works of Tschentscher et al. [13] in
their rotating sponge reactor and of Wenmakers et al. [14] for metal
sponges with a catalytically active layer as well as for reticulated
vitreous carbon sponges [15] with carbon nanofibers [16].
Standardization of mass transfer measurements in absorption
columns is discussed in literature [17,18]. Mainly carbon dioxide is
recommended as mass transfer component either for the absorp-
tion in caustic soda solutions or for the desorption from water.
Measurements with these test systems in sponges are not pub-
lished. The aim of this work is thus to investigate mass transfer
in sponges for absorption and desorption with these test systems.
The focus is set on applicability of the test systems and reliability of
the data measured for effective interfacial areas and mass transfer
coefficients.
For the comparison with literature data for state-of-the-art col-
umn internals a literature survey lead to an abundance of possible
correlations. The ones most often used were developed by Bravo
and Fair [19], Billet and Schultes [20], Onda et al. [21], Rocha et al.
[22,23], Wagner et al. [24] and the so called “Delft-Model” by Olu-
jic [25]. They were developed for structured and random packings.

0255-2701/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2012.02.002
30 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39
Fig. 1. Sponge types used in this study: SiSiC (left), silicate (middle) and OBSiC (right).
These correlations already offer a broad range of values when calcu-
lated with the same characteristics, often covering even one or two
orders of magnitude for a predicted parameter. It is thus not possi-
ble to identify the expected order of magnitude for a new column
internal such as ceramic sponges, when no experimentally adapted
correlation parameters are available.
2. Experimental approach
Gas- and liquid-side mass transfer coefficients and the effective
interfacial area are determined by measurements with chemical
absorption and physical desorption, which were analyzed accord-
ing to the HTU–NTU-concept. The experimental setup was adapted
from Hoffmann et al. [17]. As suggested in this work as well as from
Rejl et al. [18] the absorption of carbon dioxide from air into caustic
soda solution was used for the determination of the gas side mass
transfer coefficient and the effective interfacial area using the so
called “Danckwerts plot” as proposed by Wales [26]. A second data
evaluation for the effective interfacial area was performed under
the assumption of negligible gas-side mass transfer resistance. This
assumption was checked according to Weimer and Schaber [27].
For the determination of the liquid side mass transfer coefficient
the desorption of CO2 from water in air was selected as used by
Bornhuetter and Mersmann [28] and suggested by Rejl et al. [18].
2.1. Investigated sponges
The sponge types used in this study are selected according to
their flooding behaviour investigated in an earlier study [9], where
a range of different materials was tested. The two sponge types
with an operating range comparable to state-of-the-art column
internals were chosen. A third sponge type with the next best per-
formance was also selected. All sponge elements were cylinders of
100 mm diameter. They were produced by different manufacturers
in a replication process after the method of Schwartzwalder and
Somers [29]. The first sponge type was a commercially available
silicon carbide sponge infiltrated with pure silicon (SiSiC) manu-
factured by “Erbicol SA” with a total porosity of 0.88, a pore number
of 10 ppi and an element height of 25 mm. The second sponge type
was provided as a prototype by “Johann Jacob Letschert Sohn” and
is made of silicate ceramics with a porosity of 0.91 and a pore
number of approximately 10 ppi. The elements have a height of
100 mm. An element with a cone-shaped bottom (90◦ cone angle)
as drainage enhancer was also provided. The third sponge type was
manufactured by “Vesuvius, Becker & Piscantor, Grossalmeroder
Schmelztiegelwerke” and is made of oxidic bounded silicon car-
bide (OBSiC) with a porosity of 0.85 and 10 ppi at 50 mm element
height. Photographs of all sponge types are shown in Fig. 1.
The geometrical characteristics of the sponges were determined
according to Grosse et al. [30,31]. In Table 1 the nominal porosity
corresponding to the total porosity value, the outer porosity and
the geometrical surface area of the sponges are given. The outer
porosity is defined as the ratio of the outer void volume to the total
element volume and is the relevant porosity concerning hydro-
dynamics. Furthermore, element and packing height used in this
study are given in Table 1. The silicate sponge element with the
cone-shaped bottom had a height of 125 mm.
As the sponge elements are of limited height, stacking of ele-
ments is necessary. The influence of the number of intersections
on the operating range proved to be of minor importance [9]. Up
to 15 elements are stacked for the packing heights used in this
study. For cleaning and drying they were removed from the column
between the experiments, which lead to a random arrangement of
packing elements in the column (denoted as “random” further on).
This procedure was checked against a procedure, where the pack-
ing remained in the column for cleaning and drying at the highest
gas load (denoted as “non-random” further on).
2.2. Experimental setup
The experimental setup is shown in Fig. 2. A DN 100 glass column
with an actual internal diameter of 102 mm was used. The packing
height for the different sponge types was chosen as given in Table 1.
The circumferential surface of the packing was wrapped in Teflon
foil in order to avoid bypass and to fit properly in the column. All
experiments were carried out near ambient conditions and started
with dry packing. The temperatures of the gas and liquid streams
were measured as well as the pressure inside the column and the
differential pressure drop over the packing.
The liquid flow is circulated through the column with a gear
pump and distributed above the packing with a pipe distributor
of approximately 1000 drip points/m2 with a diameter of 1 mm. A
siphon at the liquid outlet of the column avoids gas breakthrough at
the column bottom. The liquid flow was measured with an Endress
& Hauser Promass 80E coriolis mass flow meter. For the absorption
measurements liquid samples were taken from the storage tank
and analysed by acidimetric titration. For the desorption measure-
ments, first deionised water was circulated through the column to
wet the packing. Then CO2 -saturated water was fed to the column.
Liquid samples were taken plunged in caustic soda solution and
then analysed with acidimetric titration. Sample collection was car-
ried out from the storage tank and directly under the packing with
a drainage trough over the whole column diameter.
The main gas flow is taken from the pressurized air supply, regu-
lated by a mass flow controller and saturated with water at 25 ◦ C in a
heated packed column with ceramic cylinder rings. For the absorp-
tion measurements, a gas flow of CO2 is added to the main gas flow
and mixed in a static gas mixer. The concentration of CO2 in the total
gas flow is set by the ratio of both flows. As indicated schematically
in Fig. 2, the gas flow enters the column through a gas distributor,
 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39 31

Table 1
Overview of the characteristics of the sponge elements used in this study.

Manufacturer Material Nominal porosity ppi Element height (mm) Packing height (mm) Outer porosity Specific surface area (m2 /m3 )
a
Erbicol SiSiC 0.88 10 25 375 0.86 470a
Letschert silicate 0.91 10 100/125 200 + 125 0.88b 700b
Vesuvius OBSiC 0.85 10 50 350 0.77 500
a
Data from Grosse et al. [31].
b
Data from Grosse and Kind [9].

i.e. a pipe with the bottom quadrant cut out (50 mm × 13 mm). The
concentration of the gas phase is measured just before and after the
packing, where samples were taken from the column and analyzed
with FT-IR spectrometry. This should avoid to measure concentra-
tions influenced by entrance and exit effects due to absorption or
desorption outside the packing.
2.3. Data evaluation
For data evaluation, the HTU–NTU-concept was applied as given
below. The properties of the gases and the liquids were used as
recommended by Hoffmann et al. [17]. For the phase equilibrium,
Henry’s law can be used (Eq. (1)), as the molar fractions of CO2
are always above 0.01% and below 1%. Thus the molar load (mol
CO2 /mol carrier gas or liquid) is approximately equal to the molar
fraction (mol CO2 /mol total). The molar load is used here instead of
the molar fraction for simplification of all balances.
Y∗ Y He
K= = ∗ = (1)
X X p
where K is the equilibrium constant, He (bar) is the Henry coeffi-
cient, p (bar) is the pressure, X (mol/mol) is the molar load of CO2
for the liquid side, Y (mol/mol) is the molar load of CO2 for the gas
side, X* (mol/mol) is the equilibrium molar load of CO2 for the liq-
uid side and Y* (mol/mol) is the equilibrium molar load of CO2 for
the gas side.
The HTU–NTU-concept based on the gas side mass balances and
kinetics leads to Eq. (2) [17].
 G,out
NG dY
H = HTUOG · NTUOG = · (2)
kOG · aeff · AC · mG Y∗ − Y
    G,in  
HTUOG NTUOG
where H (m) is the packing height, HTUOG (m) is the height of an
overall transfer unit for the gas side, NTUOG is the number of overall
transfer units for the gas side, NG (mol/s) is the molar flow rate of
the gas, kOG (m/s) is the overall mass transfer coefficient for the
gas side, aeff (m2 /m3 ) is the effective interfacial area, AC (m2 ) is the
column cross sectional area and mG (mol/m3 ) is the molar density
of the gas. The specific effective interfacial area aeff is assumed to
be constant over the column height.
For the absorption of CO2 in caustic soda solution, the reaction
between CO2 and the OH− ions takes place in the film and is irre-
versible under the condition of OH− concentrations bigger than
0.1 mol/l [32]. Then the concentration of CO2 in the bulk liquid is
zero. Therefore the NTUOG can be calculated from the measured
gas concentrations under the assumption that the equilibrium gas
concentration is zero, too.
The volumetric overall mass transfer coefficient kOG aeff is cal-
culated from the HTUOG of the sponge packing. The reaction is
assumed to be of pseudo-first order and very fast, as long as there
are sufficient OH− ions at the interface [33]. This was shown by
Danckwerts and Kennedy [32] for the absorption of CO2 in caustic
soda solutions with concentrations bigger than 0.1 mol/l. The liq-
uid side mass transfer is enhanced by the reaction. In this case, the
enhancement factor E can be set equal to the Hatta number Ha [34],
Eq. (3).

DL · kR · cNaOH
E ≈ Ha = , for Ha > 2 (3)
kL
where E is the enhancement factor, Ha is the Hatta number,
DL (m2 /s) is the diffusion coefficient for CO2 in the liquid phase,
kR (m3 /mol/s) is the reaction constant, cNaOH (mol/m3 ) is the
concentration of the caustic soda solution and kL (m/s) is the mass
transfer coefficient for the liquid side. kR is taken from [33] and DL
is taken from [35].
This was confirmed for the conditions used in this work by
Weimer and Schaber [27]. Hence, the overall mass transfer coef-
ficient can be written as in Eq. (4).
1 1 K · mG
= +
kOG · aeff kG · aeff E · kL · aeff · mL

1 1 K · mG
= + ·  (4)
kG · aeff aeff DL · kR · cNaOH · mL

Fig. 2. Experimental setup for the determination of mass transfer coefficients and
effective interfacial area.
where kG (m/s) is the mass transfer coefficient for the gas side and
mL (mol/m3 ) is the molar density of the liquid.
If the gas side mass transfer resistance is negligible, i.e. the gas
side mass transfer coefficient kG is larger than 0.01 m/s, as shown
32 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39
by Weimer and Schaber [27] for our experimental conditions, the
effective interfacial area can be calculated directly from the mea-
sured overall volumetric mass transfer coefficient (kOG aeff )meas
using Eq. (5).
K · mG
aeff ≈ (kOG · aeff )meas ·  (5)
DL · kR · cNaOH · mL
The validity of the assumption of a negligible gas side mass transfer
resistance is verified by using different concentrations of caus-
tic soda solutions. If the values for the effective interfacial area
calculated according to Eq. (5) show a decrease with increasing
concentration of the caustic soda solution at the same operating
conditions, the gas side mass transfer resistance is not negligible.
A second possibility to evaluate the data measured at different
concentrations of the caustic soda solution is the so called “Danck-
werts plot” [26], which takes the influence of the gas side mass
transfer coefficient into account and allows the determination of
both the effective interfacial area and the gas side mass transfer
coefficient. In this plot, 1/(kOG aeff ) is plotted versus the last term in
Eq. (4) for measurements at different concentrations. The regres-
sion line of the measured data then exhibits a slope of 1/aeff and an
intercept of 1/(kG aeff ). This evaluation method is very sensitive to
errors in measurements, but can be used in addition to the other
method to determine the order of magnitude of the gas side mass
transfer coefficient and therefore also to justify the assumption of
a negligible gas side mass transfer resistance.
For the liquid side mass transfer coefficient the procedure is
comparable. The desorption of carbon dioxide from water into
air is used as test system. The HTU–NTU-model can be evaluated
both for a gas and a liquid side overall mass transfer coefficient,
see Eq. (2). The gas side NTUOG for the assumption of both straight
equilibrium line and straight operating line can be approximated
as shown in Eq. (6) [36]. The equilibrium concentration Y* is calcu-
lated with Eq. (1). In this case the overall mass transfer coefficient
is given by Eq. (7). Here it is also possible to neglect the gas side
mass transfer resistance as discussed before. For the liquid side,
the HTU–NTU-concept leads to Eq. (8).
 G,out
dY
NTUOG =
G,in
Y∗ − Y
Yout − Yin

(Y ∗ − Y )out
= · ln
(Y ∗ ∗
− Y )out − (Y − Y )in (Y ∗ − Y )in
1 1 K · mG
= +
kOG · aeff kG · aeff kL · aeff · mL
 L,out
NL dX
H = HTUOL · NTUOL = · (8)
kOL · aeff · AC · mL L,in
X∗ − X
where HTUOL (m) is the height of an overall transfer unit for the
liquid side, NTUOL is the number of overall transfer units for the
liquid side, NL (mol/s) is the molar flow rate of the liquid and
kOL (m/s) is the overall mass transfer coefficient for the liquid side.
For the calculation of the NTUOL it is assumed that CO2 is a spar-
ingly soluble gas and thus the equilibrium concentration X* is equal
to zero. As in this case the gas side mass transfer is negligible, the
overall mass transfer coefficient for the liquid side equals the liquid
side mass transfer coefficient. The justification of these assump-
tions has already been proven by Bornhuetter and Mersmann [28].
2.4. Experimental procedure, reproducibility and consistency
First proper wetting of the sponge packing was ensured for all
experiments by circulating liquid at the desired feed rate through
the column for approximately 30–45 min. For the absorption exper-
iments, the gas load was then added and after reaching steady state
gas samples were taken. Caustic soda solutions of 0.1 mol/l up to
1.1 mol/l were used with 4–6 different concentrations. The concen-
tration of the liquid was measured before and after the experiment
and proved to be constant, as the amount of CO2 absorbed was
comparably small. In addition to that, the absorption in the column
outside the packing would also lead to a change in the concen-
tration of the caustic soda solution. Therefore the mass of CO2
absorbed with time calculated from the gas side concentrations
always shows less absorbance than calculated from the liquid side
concentrations. Thus a consistency check with mass balances was
not possible. For the data evaluation under neglect of the gas side
mass transfer resistance, no influence of the caustic soda solution
concentration could be found. The assumption of a negligible gas
side mass transfer resistance was therefore justified.
Reproducibility was tested by 10 independent absorption mea-
surements at similar concentrations of caustic soda solution
cNaOH ≈ 0.97 mol/l at constant liquid load, BL = 14.7 m3 /m2 /h and gas
load F = 0.34 Pa0.5 without removal of the packing from the column
between the experiments (non-random arrangement). The exper-
iments showed a standard deviation of 5% for 1/(kOG aeff ) while
the concentration-term varied with a standard deviation of 3%.
If only the four experiments were taken into account where the
concentration-term in Eq. (4) varied with a standard deviation of
0.4% a standard deviation of 2% was reached.
For the desorption experiments deionised water was used for
the wetting of the sponge packing and the gas load was already
added. Then the liquid feed was changed to the CO2 -saturated
water and, after reaching steady state, gas and liquid samples were
taken. The mass balance for CO2 was used as a consistency check.
Only those measurements with less than 25% difference between
the mass desorbed from the liquid side and the mass absorbed on
the gas side are presented here. Reasons for the inaccuracy of about
one third of the measurements for sponges are discussed later on.
Reproducibility was tested in 5 measurements for one combina-
tion of gas and liquid load (BL = 8.9 m3 /m2 /h and F = 0.51 Pa0.5 ) and
the standard deviation for kL aeff was found to be at about 15% for
the calculations from kOL and 10% for the calculation from kOG . The
mean value of all 10 coefficients determined had a standard devi-
ation of 13%. The values determined from kOL were mostly higher
than the values determined from kOG . In the following sections, the
(6) mean values of the calculations from kOL and kOG are presented.
Reference measurements were performed with a Mellapak 250Y
to evaluate the measurement methods. The effective interfacial
areas determined under neglect of the gas side mass transfer coef-
(7)
ficient from the absorption measurements showed a clear decrease
with increasing concentration of the caustic soda solution, which
contradicted the assumption of a negligible gas side mass transfer
resistance. Therefore the effective interfacial area was calculated
from the Danckwerts plot. As shown in Table 2, the results were
in good agreement with the correlation of Weimer and Schaber
[27]. These authors used potassium hydroxide solutions for absorp-
tion to avoid the described effect, as they neglected the gas side
mass transfer coefficient and used Eq. (5) for data evaluation. The
gas side mass transfer coefficients observed for the Mellapak 250Y
must therefore be in the same order of magnitude as in the work
of Weimer and Schaber.
Spiegel and Meier [37] measured gas side mass transfer coeffi-
cients with test systems for distillation. The values obtained from
our measurements are in the range of the values measured by
Spiegel and Meier, although they also measure significantly higher
values depending on the operating conditions. Due to the different
test systems used it is expected that the values obtained can only
be compared to a limited extend. For the liquid side Laso et al. [38]
measured mass transfer coefficient for the desorption of oxygen.
 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39 33

Table 2
Overview of the validation data for the Mellapak 250Y and the values taken from literature.

BL (m3 /m2 /h) F (Pa0.5 ) aeff (m2 /m3 ) aeff,Lit a (m2 /m3 ) kG (m/s) kG,Lit b (m/s) kL aeff (1/s) kL aeff,Lit c (1/s)

8.9 0.34 152 – 0.0048 – 0.012

0.0044
14.8 0.34 217 203 0.0030 0.023 0.017
–0.0063
20.2 0.34 – 205 – 0.024 0.021

8.9 0.68 123 – 0.0165 0.018 0.012

0.0092
14.8 0.68 212 215 0.0050 0.023 0.017
–0.0127
20.2 0.68 222 217 0.0056 0.039 0.021

8.9 1.02 192 – 0.0048 0.024 0.012

0.0158
14.8 1.02 238 223 0.0035 0.066 0.017
–0.0206
20.2 1.02 204 224 0.0061 0.037 0.021
a
Correlation of Weimer and Schaber [27].
b
Range of values from Spiegel and Meier [36].
c
Laso et al. [37] converted for CO2 .

These values had to be converted for carbon dioxide and were then
found to be in the same order of magnitude, although our val-
ues are up to two times as high as the values by Laso et al. For
all mass transfer coefficients it is thus expected that the order of
magnitude of the measured data is in accordance to the literature
values.
3. Experimental results and discussion
Experiments were performed at different liquid and gas loads
for the different sponge samples. The liquid loads BL and the gas
loads F were chosen in accordance to the operating range observed
in previous work [9]. In the following sections the focus is set on the
measurements with the SiSiC sponges. For the other sponge types,
only comparative experiments were carried out. For the compari-
son with correlations from literature mainly the proportionalities
were considered.
the available area is wetted, which however is not reached at the
highest liquid load.
It is obvious that the two data evaluation methods are only in
partial agreement with each other. For the data evaluation accord-
ing to Danckwerts plot, the highest and the lowest liquid load lead
to comparable results for the effective interfacial area to the values
obtained from the data evaluation “kG neglected”. The other liq-
uid loads lead to significantly higher values. At the same time, the
calculated gas side mass transfer coefficients were by far lower than
expected, as will be discussed in Section 3.3. The assumption of a
negligible gas side mass transfer resistance was justified by the fact,
that for the evaluation “kG neglected” no decrease in the effective
interfacial area could be observed with increasing concentration

3.1. Measured effective interfacial area

The absorption experiments for the SiSiC packing with random

arrangement were evaluated with both methods described in Sec-
tion 2.3. The results for the evaluation after the Danckwerts plot
(denoted “Danckwerts”) and under the assumption of a negligi-
ble gas side mass transfer resistance (denoted “kG neglected”) are
depicted in Fig. 3 as a function of the gas load for different liq-
uid loads. For the data evaluation according to Danckwerts plot,
single data points at low concentrations were omitted in order to
obtain a positive intercept for the regression line. Namely, at low
concentrations the measurements become less reliable due to mea-
surement errors and the fact that the amount of carbon dioxide
absorbed might change the concentration during the experiment.
Examples for the Danckwerts plot can be found in Fig. 5 and in [39].
The obtained coefficients of determination are often lower than for
the evaluation of all possible data points and lie in the range of
R2 = 0.5–0.97. For the evaluation under neglect of the gas side mass
transfer resistance, the error bars indicate the standard deviation
of the measurements at 5 different concentrations. The standard
deviations reach up to 50% of the mean value at the lowest liquid
load and between 15 and 30% at the higher liquid loads. The abso-
lute values of the standard deviation are comparable for all liquid
loads.
The data obtained from Danckwerts plot showed an increase in
the effective interfacial area with increasing liquid load except for
the highest liquid load. The same trend is visible in the data eval-
uation under neglect of the gas side mass transfer resistance. Here
also the highest liquid load follows the trend. Thus better wetting
Fig. 3. Results for the effective interfacial area at different liquid loads as a function
is achieved at higher liquid loads, although it does not exceed 30%
of the gas load from the experiments with random packing arrangement. Determi-
of the total specific geometric surface area ageo of the sponge struc- nation according to Danckwerts plot (a). Determination under the assumption of a
ture. For the evaluation according to Danckwerts plot, over 50% of negligible gas side mass transfer resistance (b). Lines added as visual guidance.
34 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39
Fig. 4. Results for the effective interfacial area of the other sponge types ((a) OBSiC
and (b) silicate) at different liquid loads as a function of the gas load for the mea-
surements with random packing arrangement. Data evaluation under neglect of the
gas side mass transfer resistance. Lines added as visual guidance.
of the caustic soda solution. Therefore the gas side mass transfer
coefficient should be in the range of kG > 0.01 m/s, as can be eas-
ily calculated from Eq. (4) for the range of concentrations used in
this study, which was already performed by Weimer and Schaber
[27]. This was not in very good agreement with the data evaluated
according to Danckwerts plot, as will be discussed in the section
dealing with mass transfer coefficients. Thus a thorough evaluation
of the measurement method seems necessary and will be discussed
in the following section.
For the other packing types, only measurements with random
packing arrangement were carried out. The results under neglect of
the gas side mass transfer resistance are shown in Fig. 4. There less
influence of the liquid load was observed for the OBSiC sponges.
For the silicate sponges with cone-shaped bottom an inversion
of the influence of the liquid load was found. In these sponges
the drainage is enhanced and therefore the flow at the bottom of
the sponge packing cannot be compared with the other sponge
types. The data for the OBSiC sponges lead mostly to a nega-
tive intercept when the Danckwerts plot was applied and could
therefore only partly be compared with the values presented in
Fig. 4. The estimated effective areas at the lowest liquid load
were in the range of 200 m2 /m3 approximately and thus slightly
higher than calculated under neglect of the gas side mass transfer
resistance. For the silicate samples, the inversion of the influence
of the liquid load was also present in the Danckwerts plot. The
effective area values found for the lower liquid load were in the
range of 250 m2 /m3 and for the higher liquid load in the range
of 120 m2 /m3 .
Fig. 5. Examples for the regression line according to the Danckwerts plot (a). Influ-
ence of an increasing effective interfacial area with increasing concentration on the
linear regression (b).
The geometric surface area of all sponge types used in this
study cannot be properly wetted despite the radial distribution
of the liquid with approximately 1000 drip points/m2 and thus
the effective surface area is not as high as could be desirable
for applications in separation columns. This observation indicates
that the flow pattern of the liquid flow through the sponge is a
rivulet flow where only parts of the available geometric surface
area are used. Thus even a good distribution of liquid over the
packing cannot improve the wetting of the structure. Compared
with the correlations from literature, both higher and lower val-
ues could be expected from the calculated values. An increase
with increasing liquid load is predicted by some correlations, as
well as a slight increase with increasing gas load. This corre-
sponds well with the data obtained for the SiSiC, but nor for the
other sponge types. Nevertheless, no correlation could fit the data
properly.
One further reason for the observed variation in the effective
interfacial area might be caused in axial liquid maldistribution over
the packing height. Indications for this fact were found in a previ-
ous study on the hydrodynamics of the sponge samples used in this
work [9]. A significantly higher static holdup at the lower end of
the packing was observed. Such liquid maldistribution leads to an
inhomogeneous effective interfacial area over the packing height.
For the calculation of the HTU–NTU-model, the assumption of a
constant specific effective interfacial area over the packing height
was necessary in order to solve the integral. Liquid maldistribu-
tion thus leads to less reliable results evaluated with this model.
As liquid maldistribution seems to be a general problem caused by
 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39
the structure of the sponges the results have to be considered with
care.
3.2. Applicability of the measurement methods for sponges
As the data evaluation under neglect of the gas side mass transfer
coefficient showed high standard deviations and the Danckwerts
plot often lead to a negative intercept a discussion on the appli-
cability of the recommended test systems to ceramic sponges is
necessary. In general, the measured values scatter very much for
the different concentrations when the random packing arrange-
ment was chosen. An example for a Danckwerts plot is given in
Fig. 5(a). Due to the fact that the absolute value of the intercept is
very small, a negative intercept occurs easily if the measured data
varies with a varying effective surface area. As the sponges were
removed from the column between the measurements, it is well
possible that the wetted area is different each time the packing has
been newly inserted into the column, as the arrangement of the
sponge elements with respect to each other and the inlet and outlet
configuration of the column might be of significant influence. The
sponge at the top of the packing acts as a second liquid distributor
with different design for different sponge elements. Furthermore
the configuration of the intersections changes as well. In Fig. 5(b)
it is shown, how an increasing effective interfacial area, as might
be caused by a concentration dependent contact angle, leads to a
negative intercept.
As mentioned in Section 2.1, additional experiments were car-
ried out at the highest liquid load and evaluated with both methods.
In order to control the arrangement of the sponges they were
not removed from the column between all experiments (“non-
random”). It was observed that the coefficients of determination in
the Danckwerts plot were higher than for the measurements with
removal of the packing. Values between 0.93 and 0.99 were reached
for the different gas loads. At the same time, all regression lines
showed a negative intercept. This could be due to an influence of
the concentration of the caustic soda solution on the contact angle
and thus on the wetting of the structure, which was thus inves-
tigated. For the SiSiC sponges a plate made of the same material
was provided by the manufacturer. On this plate the contact angle
could easily be measured. It was verified with a measurement on a
broadened strut end on a sponge element that the contact angles
measured were comparable. All contact angles were averaged from
four to six measurements. The contact angle of water on the sponge
surface was found to be (H2 O) = 20.79◦ . For the caustic soda solu-
tion, a decrease of the contact angle with increasing concentration
cNaOH was found as given in Eq. (9), while the surface tension of the
caustic soda solution was found to be approximately constant, as
confirmed in literature [40].
(NaOH) = 15.29◦ − 9.47◦ · cNaOH (mol/l)
+ 5.369◦ · (cNaOH )2 ((mol/l) )
2
− 1.13◦ · (cNaOH )3 ((mol/l) )
3 matter how the packing is arrangend. Neglecting the gas side mass
where  (◦ )
is the contact angle.
Therefore, a model based data correction was performed.
Among the numerous correlations from literature predicting the
effective surface area the correlation of Shi and Mersmann [41]
not only predicts the influence of the surface tension but also the
influence of the contact angle on the effective surface area. The
proportionality predicted is given in Eq. (10).
C of variation. A careful choice of experimental conditions is nec-
aeff =
1 − 0.93 · cos 
The corrected inverse volumetric mass transfer coefficient
(1/kOG · aceff ) is then calculated according to Eq. (11). The contact
35
Fig. 6. Results for the effective interfacial area at the highest liquid load as a function
of the gas load for the different measurements and evaluation types. Lines added as
visual guidance.
angle of water is set as a reference.
1 1 aeff
= ·
kOG · aceff (kOG · aeff )meas aceff
1 1 − 0.93 · cos (H2 O)
= · (11)
(kOG · aeff )meas 1 − 0.93 · cos (NaOH)
In addition to that, a selection of measurements with random
and non-random arrangement of the packing was evaluated with
the Danckwerts plot (denoted as “selection”). The range of con-
centrations used in this selection was restricted, as mainly the
measurements at the highest and lowest concentrations were
omitted. Therefore the influence of the concentration on the contact
angle causing a different wetting could be minimized.
A comparison of the different evaluation methods and the dif-
ferent packing arrangements at the highest liquid load is depicted
in Fig. 6. The data evaluation after correction of the contact angle
(denoted as “corrected”) leads to lower absolute values, as the
reference value is set at a higher contact angle and thus a lower
effective interfacial area due to less wetted surface of the sponge.
For the non-random arrangement the correction led to significantly
lower standard deviations, which clearly proves the influence of the
contact angle and thus the concentration on the effective interfa-
cial area. Nevertheless the intercept in the Danckwerts plot for the
corrected data of the non-random arrangement was still negative.
For the selection and the evaluation according to the Danckw-
erts plot the effect of the correction is less obvious. In general, the
uncorrected values all lead to the same range of data values. Com-
paring the results with random and non-random arrangment under
neglect of the gas side resistance, the values with non-random
arrangement are higher, but both curves lie within the standard
deviation of each other. This indicates that measurements with at
least five different concentrations lead to comparable results, no
(9)
transfer resistance leads in any case to curves with a clear influence
of the gas load. The evaluation according to the Danckwerts plot
leads to greater variations with the gas load. As the selection also
contains the values measured with random arrangement, the
difference between this curve and the pure random arrangement
is comparably small.
In general, all results obtained with the different data evalua-
tions and the different measurement methods show a broad range
(10) essary in order to produce reliable results. The experiments with
random and non-random arrangement of the packing showed that
the wetting of the structure depends on the actual arrangement
of packing elements in the column and therefore reliable results
36 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39

require a proper analysis of the wetting situation. Results with ran-

dom arrangement should lead to a more realistic range of possible
interfacial areas when transferred to other sponge packings. At the
same time the contact angle between the liquid and the sponge
surface can depend significantly on the concentration of the caus-
tic soda solution. This effect should therefore be verified for each
material used in a study. The results for the sponges made of SiSiC
obtained under neglect of the gas side mass transfer resistance
seem in total more consistent than those from Danckwerts plot,
as the influence of the liquid load is clearly visible.

3.3. Measured mass transfer coefficients

As already discussed in Section 3.1 dealing with the results

of the effective interfacial area the determination of the gas side
mass transfer coefficients is highly uncertain due to the regres-
sion lines leading to negative intercepts. Results will therefore only
be presented for the SiSiC samples, where a detailed study of the
measurement parameters was possible and the abundance of mea-
sured values enabled a selection of proper data or an exclusion of
data points for evaluation. Although the absolute values cannot be
considered reliable, the results based on these measurements pro-
vide an idea about the order of magnitude of the mass transfer
coefficient.
The study on the influence of the concentration of the caustic
soda solution suggests for the gas side mass transfer coefficient
values in the range of kG > 0.01 m/s, as already mentioned in Sec-
tion 3.1. In addition to that, the evaluation of the measured data
with the Danckwerts plot gives values for the gas side mass trans-
fer coefficient, which are depicted in Fig. 7. The results obtained
for the three lower liquid loads do not correspond to the order of
magnitude expected for the gas side mass transfer coefficient. At
Fig. 7. Results for the gas side mass transfer coefficient at different liquid loads as
the lowest liquid load, the values tend to be higher than for the a function of the gas load for the measurements with random packing arrangement
other two medium liquid loads. For those two, the effective inter- corresponding to the effective interfacial area in Fig. 3(a). Results for the differ-
facial area calculated from Danckwerts plot was significantly higher ent measurement types at the highest liquid load corresponding to the effective
than under neglect of the gas side mass transfer resistance, which interfacial areas in Fig. 6. Data evaluation for both diagrams with Danckwerts plot.
Coefficients of determination in the range of R2 = 0.5–0.97. Lines added as visual
is in theoretical agreement to the lower mass transfer coefficients. guidance.
An increase of the gas side mass transfer coefficient with increasing
gas load as expected from correlations for state-of-the-art column
internals found in literature was not observed. could be observed with increasing liquid or gas load. The range of
For the highest liquid load three different data evaluations were the measured values is in good agreement with those measured for
possible, as already discussed in Section 3.2. Here the data with ran- conventional column internals, as for example by Hofmann et al.
dom arrangement and the selection are in the same range, which [17]. For the silicate sponges mass transfer coefficients in the same
also corresponds to the range expected from the data evaluation range were observed, while the values for OBSiC sponges were in
for the effective interfacial area under neglect of the gas side mass the range of 0.0004 m/s < kL < 0.0007 m/s. For all sponge types no
transfer resistance and data from literature for example as mea- significant influence of the gas and liquid load could be confirmed.
sured by Hoffmann et al. [17] for Pall rings. In this study, the
experimentally determined gas side mass transfer coefficients were
approximately constant with a slight decrease with increasing gas
load towards flooding. Additionally an influence of the liquid load
on the gas side mass transfer coefficient was observed. This could
not be confirmed in this work.
The selection shows the expected increase with increasing gas
load, while the data with random arrangement seems to vary
arbitrarily. The correction of the selected data with the contact
angle leads to values up to one order of magnitude lower, as was
also observed for the effective interfacial area. These results agree
with the uncorrected values at lower liquid loads. For the other
sponge types the data evaluation leads to results in the range of
0.002 m/s < kG < 0.013 m/s. A consistent influence of gas or liquid
load over the different sponge types was not observed.
For the liquid side mass transfer coefficients, the desorption
experiments had to be evaluated. These experiments were often
inconsistent; therefore only for some combinations of gas and liq-
Fig. 8. Results for the liquid side mass transfer coefficient at different gas loads as
uid load results are presented in Fig. 8. In general, no trend of a function of the liquid load using the effective interfacial area determined under
increase or decrease of the liquid side mass transfer coefficient neglect of the gas side mass transfer resistance. Reproducibility within ±15%.
 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39 37

Therefore the data is in contrast with the correlations for state-of- factors (Eqs. (14) and (15)). The variation of k L in relation to kL at
the-art column internals found in literature. fG = fL = 1 was exemplified as shown in Fig. 10.
For the sponges made from SiSiC and OBSiC, the collection of
 Xin − Xout
liquid below the packing in the desorption experiments was par- Xout = Xin − (12)
fL
ticularly difficult to realize. Thus the liquid concentration could in
some cases not be determined with sufficient accuracy. This led to  Yout − Yin
Yout = Yin + (13)
the large deviations in the mass balances between gas and liquid fG
side. A possible explanation for this effect will be discussed in the
  fL · NL X
following section. H = HTUOL · NTUOL =  ·a · ln in (14)
kOL eff · AC · mL Xout

3.4. Stream splitting in rivulet flow
Due to the fact that the liquid tends to flow in rivulets through
the sponge structure and the gas might therefore tend to channel, a
representative sample collection is challenging. As Fig. 9 illustrates,
rivulets and channelling might lead to a splitting of streams, where
parts of the streams pass the packing without contact to the other
phase and thus without mass transfer. The split fraction of the molar
flow in contact to the other phase is denoted as f.
The measured data at the inlet of the streams should be reli-
able concerning sample collection, as no stream splitting has yet
occurred. At the outlet of the streams the situation might be more
difficult to judge. As the values at the outlet of the streams always
differ significantly from the values at the inlet, the sample taken
must have had contact with the other phase. Whether the sam-
ple is taken from the remixed streams (Yout or Xout ) or from a split
stream in direct contact to the other phase (Y out or X out ), which
has a higher concentration in the gas phase and a lower concentra-
tion in the liquid phase compared with the remixed streams for the
desorption experiments, is not easy to verify.
The dependence of the calculated values for the mass trans-
fer coefficient on the split factors fL and fG for both evaluated
HTU–NTU-concepts was thus investigated. First the relations
between the concentrations of the remixed stream and the split
stream were evaluated (Eqs. (12) and (13)). Then the new values
for the HTU–NTU-concept were calculated depending on the split
 
H = HTUOG · NTUOG
 − Yin
fG · NG Yout
=  · ∗
kOG · aeff · AC · mG (Y − Y )out − (Y ∗ − Y )in

 (Y ∗ − Y  )
· ln out
(15)
(Y ∗ − Y )in
As can be seen in Fig. 10 a split of the gas stream has no influence
on the calculated values from the liquid side overall model and only
at very low split factors – and thus a high amount of gas passing
without contact to the liquid – a significant influence on the gas
side overall model. The split factor of the liquid side is of much
more importance and has nearly the same influence on the gas and
liquid side overall models. A splitting of the liquid stream might
thus significantly change the values for the measured liquid side
mass transfer coefficients.
As gas as well as liquid stream might split at the same time,
the concentrations measured may not correspond to each other
and to the total molar flow of the phase. Then the mass balance
for the transfer component over the packing is no longer fulfilled
when calculated with the measured values, and the measurement
is inconsistent. It is not possible to judge whether the gas or the
liquid side concentration might be incorrect – or even both concen-
trations, thus whether Yout or Y out for the gas side or Xout or X out
for the liquid side respectively is measured. Therefore inconsistent
measurements were excluded from the presented data.
The model presented here for the stream splitting is the sim-
plest one imaginable, but already leads to a significant influence
on the measured values. In addition to that, two rivulets might
rejoin, so that the wetting over the packing might become worse.
Such behaviour was observed by Calvo et al. [6], who investigated
the liquid distribution over the sponge packing under different
hydrodynamic conditions. The presence of axial liquid maldistri-
bution as observed in the previous work [9] with a significantly

Fig. 10. Influence of the split factors of gas fG (curves for fL = 1) and liquid streams fL
(curves for fG = 1) on the calculated values of k L for both HTU–NTU-models related to
the value without stream splitting kL . OG, overall model for the gas side; OL, overall
Fig. 9. Scheme of the stream splitting over the packing. model for the liquid side; mean, mean value of both models.
38 J. Grosse, M. Kind / Chemical Engineering and Processing 55 (2012) 29–39
higher holdup at the lower end of the packing is also of impor-
tance and might further influence the results. Measurements of
residence time distribution for the liquid phase with injection of
a salt tracer and conductivity measurements at the liquid outlet
were also performed [39] and suggest a strong dependency on the
sponge type.
4. Conclusions
In the present study effective interfacial areas and mass transfer
coefficients for ceramic sponges were determined experimentally.
The measurement procedures were evaluated concerning repro-
ducibility and consistency of the measured data and found to
be reliable for the purpose. Nevertheless the data measured for
ceramic sponges scattered significantly for all parameters and
sponge types. Therefore the obtained results must be interpreted
with great care. Different evaluation methods were tested for the
effective interfacial area and the influence of the wetting of the sur-
face by caustic soda solution of different concentrations was taken
into account by a model based correction.
For all sponge types a general agreement in the data obtained
for the effective interfacial area by the different evaluation methods
was observed. The assumption of a negligible gas side mass transfer
resistance led to lower effective surface areas and in case of very
low mass transfer coefficients, a significantly higher surface area
was obtained by the Danckwerts plot than under neglect of the gas
side mass transfer coefficient. The measured effective interfacial
area is in all cases considerably lower than the geometric surface
area of the sponge samples. For the mass transfer coefficients values
comparable to the expected range were measured. A comparison
with prediction of correlations from literature was found to be of
less relevance, as the findings of this study were mostly in contrast
with the proportionalities of the correlations from literature.
Owing to the fact that performed experiments indicate a rather
poor wetting and liquid maldistribution over the packing, a possible
application of the ceramic sponges as an efficient alternative to
established structured packings is doubtful.
Acknowledgements
The authors thank the German Research Foundation (Deutsche
Forschungsgemeinschaft) for the financial support of Research Unit
583 “Solid Sponges - Application of Monolithic Network Structures
in Process Engineering”, Johann Jacob Letschert Sohn, Germany,
for the provision of the silicate sponge prototypes, as well as
Daniel Haigis, Tobias Beierlein, Barbara Ostmann, Sarah Übele and
Johannes Schanz for their contributions.
Appendix A. Nomenclature
AC column cross-sectional area (m2 )
aeff effective interfacial area (m2 /m3 )
ageo specific geometric surface area of the sponge structure
(m2 /m3 )
BL liquid load (m3 /m2 /h)
cNaOH concentration of NaOH in the liquid (mol/m3 )
D diffusion coefficient (m2 /s)
E enhancement factor
√ liquid–solid mass transfer by carbon nanofibers on solid foam as catalyst sup-
F gas load (F = uG · G ) (Pa0.5 )
f split fraction of the molar flow (mol/mol)
H height of the packing (m)
Ha Hatta number
He Henry constant (bar)
HTU height of a transfer unit (m)
k mass transfer coefficient (m/s)
kR reaction constant (m3 /mol/s)
K equilibrium constant
N molar flow rate of the carrier stream (mol/s)
NTU number of transfer units
p pressure (bar)
R2 coefficient of determination
X molar load liquid side (mol CO2 /mol carrier liquid)
Y molar load gas side (mol CO2 /mol carrier gas)
Greek letters
 contact angle (◦ )
m molar density (mol/m3 )
Indices
c corrected
G gas
in at the inlet of the stream
L liquid
meas measured
O overall
out at the outlet of the stream
* equilibrium
 of the split stream
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