Chemical Engineering Journal 351 (2018) 356–363

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Chemical Engineering Journal

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Competing adsorption of toluene and water on various zeolites T

⁎
Markus Kraus, Ulf Trommler, Frank Holzer, Frank-Dieter Kopinke, Ulf Roland
Helmholtz Centre for Environmental Research – UFZ, Department of Environmental Engineering, Permoserstr. 15, 04318 Leipzig, Germany

H I GH L IG H T S G R A P H I C A L A B S T R A C T

• Single and competing adsorption of

toluene and water were studied.
Separate and competing adsorption of water and toluene were studied for a wide variety of zeolites.

• Awithwidedifferent
variety of adsorber materials
hydrophobicities was
investigated.
• The sorption behavior varied from al-
most non-competing to water-driven
desorption.
• Strong variations were observed even
for the same zeolite type.
• Rules for selection of most appropriate
adsorbers were derived.

A R T I C LE I N FO A B S T R A C T

Keywords: Decontamination of air or other gas streams loaded with low VOC concentrations is a prevalent task for ad-
Adsorption sorption using zeolites. Emphasizing the importance of adsorber selection, several zeolites varying in type, Si/Al
Competing adsorption ratio and provider were tested for toluene as representative organic target compound and water as adsorbate
Water both in single and competing adsorption studies. In some cases, the toluene breakthrough is mainly caused by
Toluene
water-driven desorption. It was shown that for adsorption capacity, kinetics and competition behavior not only
Zeolites
type and Si/Al ratio of the zeolite are important but also producer-specific parameters such as crystallinity,
binder type and content which are usually not explicitly documented. This study offers a basis for the selection of
adsorber materials for treatment of gas streams with significant water contents.

1. Introduction activated carbon adsorbers to adsorption-wheel technologies adapted

Volatile organic compounds (VOC) such as organic solvents are
prevalent air pollutants originating from many industrial processes but
also from stock breeding or remediation of soil and groundwater. In
many cases, the sources of contamination are diffuse which results in
large contaminated air streams with relatively low and often fluctuating
VOC concentrations. Adsorption methods for cleaning of VOC-con-
taining gas streams have been established for many years [1–5]. De-
pending on the specific process conditions and the relevant hazardous
pollutants, the technical realization ranges from simple one-way
for different scales and flow rates. For quasi-continuous operation,
combined adsorption/regeneration techniques have been developed
[4,6–9]. In the field of air cleaning in the industrial context, the
treatment of large air streams with VOC concentrations below 1000
ppmv is an ongoing challenge with broad economic and environmental
relevance [10,11]. The large variety of applications can be illustrated
by examples from production of various chemicals such as paints
[12,13] and from paint finishing systems but also from livestock
breeding [14,15], upgrading of natural gas [16–18] or even in air
conditioning processes in buildings or cars [2,19–21]. In all these cases,

⁎
Corresponding author.
E-mail address: ulf.roland@ufz.de (U. Roland).

https://doi.org/10.1016/j.cej.2018.06.128
Received 23 March 2018; Received in revised form 18 June 2018; Accepted 19 June 2018
Available online 20 June 2018
1385-8947/ © 2018 Published by Elsevier B.V.
M. Kraus et al. Chemical Engineering Journal 351 (2018) 356–363

Table 1
Overview of investigated materials, providers and selected properties.
Zeolite type Commercial name or specification Company Pellet form and size [mm] [33] Si/Al ratio BETN2 [m2/g]

NaXa Köstrolith 13 BFK CWK1 spheres: 1.6 to 2.5 1.17 766

NaX Zeosorb 13X Süd-Chemie2 spheres: 1.6 to 2.5 < 1.5b 702
NaX SYLOBEAD MS C 544 Grace3 spheres: 1.6 to 2.5 < 1.5 708
NaX 13X Tricat Zeolites4 spheres: 2 to 3 < 1.5b 379
NaX Köstrolith NaMSX K2 CWK1 spheres: 1.6 to 2.5 < 1.18 732
NaY LiLSX Tricat Zeolites4 spheres: 1.6 to 2.5 1.5 … 5b 870
NaY SP 562 Grace3 spheres: 1.6 to 2.5 5 782
NaY NaYK CWK1 spheres: 1.6 to 2.5 2.5 695
NaY Köstrolith UK8 CWK1 spheres: 2.5 to 3.5 ≥15 490
US-Y HiSiV 1000 UOP5 sticks: Ø = 1.5, l to 3 < 20 423
US-Y Z700 ZeoChem6 spheres: 1 to 2.5 28 517
US-Y DaY C13 Degussa7 sticks: Ø = 3, l to 6 100 608
3A Zeosorb 3A Süd-Chemie2 spheres: 1.6 to 2.5 1b 23
4A SYLOBEAD® MS 514 Grace3 spheres: 1.6 to 2.5 1b 23
5A Köstrolith 5AK CWK1 spheres: 1.6 to 2.5 1b 587
5A Köstrolith 5ABF CWK1 spheres: 1.6 to 2.5 1b 651
5A SYLOBEAD® MS C 522 Grace3 spheres: 1.6 to 2.5 1b 581
ZSM-5 Z400 ZeoChem6 spheres: 1 to 2.5 200 273
ZSM-5 HiSiv3000 UOP5 sticks: Ø = 1.5, l to 3 > 20 370
ZSM-5 Köstrolith UZ8 CWK1 spheres: 2.5 to 3.5 > 50 316
ZSM-5 FeBEA 25 Süd-Chemie2 sticks: 1.6 to 2.5 20 … 25 439
ZSM-5 ZEOcat FM-8 Zeochem6 broken pieces < 3.2 15 ± 3 550

a
Without binder.
b
Per definition.
1
CWK Chemiewerk Bad Köstritz, Bad Köstritz, Germany.
2
Süd-Chemie München (now Clariant), Germany.
3
Grace GmbH & Co KG, Worms, Germany.
4
Tricat Zeolites GmbH (now Clariant), Bitterfeld, Germany.
5
UOP M.S. S.r.I, Reggio Galabria, Italy.
6
ZeoChem, Uetikom, Switzerland.
7
Degussa AG (now Evonik Degussa GmbH), Essen, Germany.

specific and optimized clean-up methods are required and, with respect
to the technical principle, adsorption techniques are mainly used.
Among the adsorber materials, activated carbons (AC) from various
sources are, without any doubt, the most established, well characterized
and also relatively cheap materials [22,23]. They are predestinated for
the adsorption of hydrophobic organic compounds which closely in-
teract with the large inner surface. Co-adsorption of hydrocarbons can
lead to a strong interference when comparing the results with single-
component adsorption. Gironi et al. described this competing behavior
on the basis of a Langmuir model for methyl tert-butyl ether and cy-
clohexane adsorbed on activated carbon [24]. Based on the individual
isotherms the simulation allows predicting the competitive adsorption
[25,26]. In contrast, in the present study a hydrophobic hydrocarbon is
studied together with water characterized by a multilayer adsorption
behavior.
The application of activated carbons is limited for processes were
adsorption is combined with thermal regeneration in oxygen-containing
gas streams, namely air. Therefore, depending on the type of con-
tamination and the process context, a wide range of non-carbonaceous
adsorbents are commercially available and even more are under in-
vestigation [27]. Especially, zeolites as a material class with a large
variety of the relevant properties (e.g., pore size and shape, hydro-
phobicity) have been employed for VOC adsorption. Among them,
faujasites of type Y are favourable for organic compounds especially for
low pollutant concentrations due to their large specific surface area,
sorption capacity and shape of the adsorption isotherm [28–30]. Many
binder-containing and binder-free zeolite materials are commercially
available and partially characterized with respect to the adsorption
properties for relevant hydrocarbons. However, the data basis for the
practically most relevant application conditions, i.e. for humid gas
streams, is limited. This is especially true for ambient air as carrier gas.
At ambient temperature (T = 23 °C), a typical relative humidity (rh) of
60% corresponds to a water content of about 12.3 g m−3 or 1.66 vol-%.
Therefore, a competitive adsorption of the target compounds, ha-
zardous VOC, and water molecules has to be considered in order to
evaluate the potential of zeolite materials for off-gas cleaning purposes.
Thus, zeolites which are appropriate for VOC adsorption in dry air may
be inefficient under real-case conditions in humid air. A key parameter
of the zeolites in this context is their surface polarity because the
contaminants are usually relatively hydrophobic whereas water
strongly interacts with hydrophilic materials. The polarity and there-
fore the affinity towards hydrophobic and hydrophilic molecules cor-
relates with the Si/Al atomic ratio, alternatively expressed as modulus
(SiO2/Al2O3 ratio), of the zeolite framework. Additionally, binder ma-
terials can influence the sorption properties of zeolites. While single
compound adsorption on zeolites has often been investigated up to
now, data on adsorption of gas mixtures containing water are scarce in
the literature [31,32].
For applications in adsorption technology and heterogeneous cata-
lysis, a wide variety of zeolites differing in structural type, modulus,
type of cation compensating the negative charge of Al in the zeolite
framework and binder have been designed. Only a part of them are
commercially available. For off-gas cleaning issues, only a handful of
zeolites are widely used and in many cases there is a lack of knowledge
with respect to competition adsorption properties of these materials.
Therefore, the present study was carried out with 22 different
zeolites under well-defined experimental conditions in order to reduce
the gap of knowledge in this field. Toluene was chosen as a re-
presentative VOC for off-gas cleaning due to its high relevance in
practice. The hydrocarbon and water were adsorbed both separately
and simultaneously in order to characterize the competitive adsorption.
The experiments were made in a packed-bed reactor employing gran-
ular zeolite materials.

357
M. Kraus et al.
Fig. 1. Schematic presentation of the experimental procedures during zeolite pre-treatment and adsorption studies.
Fig. 2. Co-adsorption of toluene and water on zeolite HiSiv1000 where the
maximum amount of adsorbed toluene is only slightly influenced by simulta-
neous water adsorption.
2. Materials and methods
2.1. Packed-bed materials
Separate and simultaneous adsorption of toluene and water both
from the gas phase was investigated for a number of zeolites with
varying hydrophobicities. An overview of all tested substances is given
in Table 1. All materials are commercially available products.
2.2. Experimental setup
Prior to adsorption experiments, the samples were equilibrated in
humid air (T ≈ 22 °C, about 60% rh) for about 24 h. For the adsorption
tests, about 1–3 g of the zeolite materials were placed in a quartz glass
tube (packed-bed reactor, inner diameter 10 mm) between two layers of
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Chemical Engineering Journal 351 (2018) 356–363
quartz glass wool. For realizing a defined temperature, the quartz tube
was placed in a tube furnace type MTF 10/15/131 from Carbolite
(Neuhausen, Germany). The temperature within the zeolite bed was
measured by a thermocouple type K combined with a multimeter type
V840 from Voltkraft (Wollerau, Switzerland).
Pure nitrogen (purity > 99.999%, from Linde) was used as carrier
gas. Gas flow controllers type GFC 17 and mass flow meters GFM series
38 (both from Analyt, Müllheim, Germany) were applied to realize and
measure a constant gas flow. Toluene (p.a.) as model VOC was provided
by Merck (Darmstadt). Before starting the adsorption experiments, the
tube was purged with N2 (404 mL min−1) at 400 °C for 2 h to remove
water from the zeolite samples. The moisture content of the purge gas
was measured in the inlet and outlet streams by gas humidity sensors
type HygroPalm2 from ROTRONIC AG (Ettlingen, Switzerland). From
these data, the dry mass of the zeolites (overview given in Table 1) was
calculated on the basis of the initial mass of the water-containing
sample.
The zeolite was loaded at T = 22 °C (uncertainty ± 1 K) with water
and/or toluene by a nitrogen stream with a total flow rate of
404 mL min−1. Thereof, 400 mL min−1 streamed through a tempera-
ture-controlled gas humidification device in order to maintain a pre-
defined dew point of 15 °C corresponding to a gas humidity of about
64% rh (12.5 g Nm−3, Tnorm = 20 °C) at ambient temperature (22 °C).
In the same manner, a small fraction of the nitrogen stream
(4 mL min−1) was saturated with toluene leading to a total concentra-
tion of 216 ppmv (corresponding to 827 mg Nm−3). The adsorption was
carried out until the concentrations in inlet and outlet flows were the
same. The experimental setup and experimental steps are schematically
shown in Fig. 1. The relative accuracy of the determined adsorbed
amount of toluene and/or water was about ± 3% in total, resulting
from the measurement uncertainties of the equipment.
The toluene concentrations in the inlet flow and the effluent from
the reactor were quantified by NDIR analysis after calibration for this
hydrocarbon using two devices type NDIR-Optik from Saxon Junkalor
(Dessau, Germany). For a representative number of samples, the
amount of toluene adsorbed on the zeolite was verified by CO2 analysis
after total oxidation of the hydrocarbon in air (employing a CuO cat-
alyst and a type C-MAT D-03GTE from Ströhlein Instruments,
M. Kraus et al.
Fig. 3. Competing adsorption of toluene and water on zeolite 13X (Süd-
Chemie) with a progressive water front leading to desorption of toluene by
replacement.
Germany). The results were in good agreement for both methods.
The breakthrough was defined according to the following criterion
based on the inlet and equilibrium concentrations: cout,breakthrough/
cin = cout,breakthrough/cout,equilibrium = 0.02.
Fig. 4. Estimation of adsorption capacities of various zeolites by separate adsorption of toluene and water under equilibrium conditions (at 22 °C, pH2O = 1.66 kPa,
ptoluene = 0.02 kPa).
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Chemical Engineering Journal 351 (2018) 356–363
3. Results and discussion
3.1. Types of adsorption behavior
For every zeolite, breakthrough curves for pure water, pure toluene
and for simultaneous adsorption of both substances were measured. In
principle, the apparent kinetics of the adsorption is strongly dependent
on experimental parameters such as gas flow rate, pellet form and size
and cannot, therefore, be simply scale-transferred [34]. However,
general conclusions can be derived when investigating the zeolite ma-
terials under uniform conditions. Generally, two different adsorption
characteristics can be distinguished: more or less undisturbed co-ad-
sorption and strong competitive adsorption. While in the case of pre-
ferential co-adsorption water and toluene are adsorbed at different
sites, in the case of competitive adsorption the two adsorbates compete
for at least one common adsorption site.
In Fig. 2, the adsorption of toluene and water on zeolite HiSiv1000
is exemplarily shown demonstrating the co-adsorption case. Here, ad-
sorbed toluene molecules were practically not affected by water mo-
lecules. The areas between the inflow and effluent curves represent the
amount of adsorbed toluene and water in the zeolite bed.
The adsorption of the two substances on zeolite 13X (from Süd-
Chemie) as shown in Fig. 3 is characteristic for competing adsorption.
Initially, both toluene and water were completely adsorbed in the
zeolite bed. However, it has to be considered that the spatial distribu-
tion of both adsorbates within the bed differs markedly which was not
reflected by the current effluent concentrations. The toluene con-
centration rose to a maximum value being about two times higher than
that of the inlet flow. Subsequently, the hydrocarbon concentration
started to decrease until after about 30 min the inflow content was
reached. Desorption of toluene was driven by the progress of water
M. Kraus et al.
Fig. 5. Amount of adsorbed water during simultaneous toluene adsorption until the first detection of water in the effluent and in equilibrium state, respectively (at
22 °C, pH2O = 1.66 kPa, ptoluene = 0.02 kPa).
adsorption along the bed length. Adsorbed toluene molecules were re-
placed by water molecules and re-adsorbed in the next dry and non-
toluene-saturated zone of the packed bed. In a continuous process, the
water adsorption front within the packed bed then reached this zone
and the replacement of toluene started again. The replacement me-
chanism temporarily leads to a higher concentration of toluene in the
effluent. In agreement with this interpretation, the maximum of the
toluene concentration at approximately 1.1 h correlates with the ap-
pearance of water in the outlet gas stream of the packed bed.
This competing behavior of organic components and water as ad-
sorbates has been also observed in literature [33,35]. In particular,
Azambre et al. reported such a behavior for different faujasites and
explained it by the relevance of acidic sites [36].
A representative selection of breakthrough curves is given in a
“Supplementary material” part of this publication.
3.2. Adsorption of single components
In addition to simultaneous co-adsorption of toluene and water,
adsorption of the single components was investigated for all zeolites.
The experimental results are summarized in Fig. 4. The adsorbed con-
tent qadsorbate (in wt.%) is referred to the dry mass of the adsorber. The
measured values represent one point of the adsorption isotherm at 22 °C
for partial pressures of pH2O = 1.66 kPa (typical ambient conditions)
and ptoluene = 0.02 kPa (representative concentration for trace con-
tamination).
Due to steric reasons (kinetic and critical diameters of a toluene
molecule are 5.58 Å and 6.7 Å, respectively) [37,38], the adsorption of
toluene is negligible for all type A zeolites (KA, NaA, CaA with pore
diameters of about 3, 4 and 5 Å) whereas water is able to enter the pores
[39,40]. The other zeolites and especially faujasites are suitable for
both water and toluene adsorption. As expected, the water adsorption
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Chemical Engineering Journal 351 (2018) 356–363
capacity decreases with increasing Si/Al ratios (Si/Al: 13X < NaY <
USY) of the faujasite zeolites. In general, the ratio between toluene and
water adsorption capacities correlates with the hydrophobicity re-
presented by the modulus. However, there are large differences espe-
cially for toluene adsorption in detail in spite of almost the same Si/Al
ratio. Possibly, this can be due to different binders and production
conditions used.
3.3. Adsorption under competing conditions
The results obtained for a purge gas loaded with both water and
toluene represent the adsorption behavior under competing conditions.
In Fig. 5, the amount of adsorbed water until the first detection of
gas humidity in the outlet gas stream (detection limit about
0.1 mg min−1) and the corresponding value for equilibrium conditions,
i.e. coinciding concentrations in the inlet and the outlet gas stream, are
shown. While the first value is dependent on the experimental condi-
tions (a kinetic parameter) and therefore, strictly speaking, only com-
parable within one series of experiments, the latter represents a mate-
rial-specific value (a thermodynamic parameter) for the water
adsorption under the present competing conditions.
As already discussed for single-component adsorption, the water
equilibrium adsorption capacity varied considerably between the zeo-
lite types and within the same zeolite group; but even more deviations
were found for the breakthrough capacity until the first water detection
in the effluent (from almost 0% to 80% of the equilibrium capacity).
The latter fact is important for many adsorption tasks when not only the
sorption capacity but also the residual water content in the effluent is
relevant.
In Fig. 6, the toluene adsorption until the first detection of the hy-
drocarbon in the outlet gas stream (detection limit 0.05 mg min−1 and
breakthrough criterion of 2% related to the inlet and equilibrium
M. Kraus et al.
Fig. 6. Amount of adsorbed toluene during simultaneous water adsorption until the first detection of toluene in the effluent and in equilibrium state, respectively (at
22 °C, pH2O = 1.66 kPa, ptoluene = 0.02 kPa).
concentrations, respectively) and the amount of adsorbed toluene under
equilibrium conditions of practically equal inlet and outlet concentra-
tions are shown during simultaneous toluene and water adsorption.
These results are especially relevant for the evaluation of the materials
with respect to the removal of organic contaminants from humid air
streams or gas flows in general.
As expected, the ultra-stable hydrophobic zeolites with high Si/Al
ratio are especially efficient for adsorptive elimination of toluene from
humid air streams. Nevertheless, even within this class of zeolites the
adsorbed quantities vary from 4 to 10 wt-%. This overview given in
Fig. 6 clearly shows the necessity of a material screening under the
conditions characteristic for the addressed application in gas cleaning.
Although the ratio of zeolite loadings until first adsorbate break-
through and until saturation depends on the experimental conditions,
the presented values give an indication for the character of competing
adsorption of water and organics. Especially for the zeolite types NaX
and NaY, a toluene replacement was detected leading to higher inter-
mediate hydrocarbon concentrations in comparison to the data for
equilibrium loading. For some of these zeolites, namely for NaYK
(CWK) and SP 562 (Grace), the replacement of toluene by water was
almost complete within the accuracy of detection. Due to this strong
selectivity, these zeolites could also be used for water-driven recovery
(see Fig. 3) of valuable, thermally sensitive chemicals.
In order to illustrate the effect of competing adsorption, the shift of
maximum adsorption due to the addition of a second compound, water
or toluene, is shown in Fig. 7. For clarity, the corresponding data are
given as relative values with respect to the maximum single-component
adsorption capacity. Especially for zeolite types 13X and NaY (not ultra-
stable), the dramatic reduction of the adsorbable amount of toluene is
illustrated. Except of the zeolite Z700 from Zeochem, a strong reduction
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Chemical Engineering Journal 351 (2018) 356–363
of this value of about 30% was also found for ultra-stable faujasite
zeolites in spite of their hydrophobicity. For Z700, even a small increase
of the adsorption capacity was measured but the relevance of this effect
has to be further proved. The strong influence of co-adsorption of water
can be generally explained by the strong affinity of most zeolites to this
polar molecule.
The effect of competing adsorption is much lower when considering
water adsorption. For most zeolites, such as all type A zeolites and
faujasites of type 13X, a displacement effect by toluene is not sig-
nificant. While a complete replacement of the toluene was measured for
some zeolites due to water adsorption, the maximum reduction of water
adsorption due to addition of toluene was lower than 40% for zeolite
UK8. This behavior is not surprising taking into account the stronger
bonding of water to the zeolites under most experimental conditions.
However, for practical application, i.e. drying of gas streams, the co-
adsorption of in most cases relatively low concentrations of hydro-
carbons is usually not relevant or does not markedly influence the
performance of such materials as drying agents.
4. Conclusions
The results on separate and competitive adsorption of water and of
toluene as model substance for organic air contaminants provide
practical guidelines for the selection of adsorber materials. For humid
gas streams, two main adsorption modes can be distinguished: one with
relatively low interference (co-adsorption) and another one with a
strong replacement of pre-adsorbed species taking place (competing
adsorption). In the second case, the recovery of organic adsorbates by
water-driven desorption at low temperatures is achievable which is
especially relevant for thermally labile substances.
M. Kraus et al.
Fig. 7. Variation of toluene and water adsorption capacities for various zeolites due to competing adsorption of the second component (at 22 °C, pH2O = 1.66 kPa,
ptoluene = 0.02 kPa).
Toluene is a good representative for a variety of contaminants/hy-
drocarbons, which are characterized by a comparable polarity (sig-
nificantly lower than that of the competing substance water with large
dipole moment), non-specific (so-called ‘hydrophobic’) interactions
with the adsorber materials and a low miscibility with water. For such
compounds (including trichloroethylene), the results of the present
study can be transferred in a qualitative manner. In contrast, for water-
miscible compounds such as alcohols the conclusions of the present
study on competing adsorption cannot be applied.
In addition to general rules related to pore size distribution and
affinity towards non-polar organic molecules (stronger for hydrophobic
zeolites with large Si/Al ratio, namely ultra-stable Y zeolites), the
commercially available products differ in a wide range with respect to
the adsorption properties. Therefore, a systematic pre-screening even
for the same zeolite types differing in the way of production, crystal-
linity or the type and amount of added binder component is strongly
advised for designing and further optimizing the gas treatment systems.
A main conclusion for the practical application of adsorption for gas
cleaning is that, especially for the most relevant VOC, already low
water concentrations in the gas stream reduce the adsorption capacity
of many materials drastically. The results of the screening tests provide
a more detailed insight into potentials and limitations of selective ad-
sorption of VOC on zeolites. They are especially crucial for the opti-
mization of processes for decontamination of gas streams containing
organic pollutants.
Acknowledgment
The authors thank the Deutsche Bundesstiftung Umwelt [Project
23750/02] for financial support and all zeolite producers given in
Table 1 for providing the applied zeolite samples.
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Chemical Engineering Journal 351 (2018) 356–363
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in the
online version, at http://dx.doi.org/10.1016/j.cej.2018.06.128.
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