Chemical Engineering Communications

ISSN: 0098-6445 (Print) 1563-5201 (Online) Journal homepage: https://www.tandfonline.com/loi/gcec20

Piperazine impregnation on Zeolite 13X as a novel

adsorbent for CO2 capture: experimental and
modeling

Fatemeh Fashi, Ahad Ghaemi & Amir Hossein Behroozi

To cite this article: Fatemeh Fashi, Ahad Ghaemi & Amir Hossein Behroozi (2020): Piperazine
impregnation on Zeolite 13X as a novel adsorbent for CO2 capture: experimental and modeling,
Chemical Engineering Communications, DOI: 10.1080/00986445.2020.1746657

To link to this article: https://doi.org/10.1080/00986445.2020.1746657

Published online: 06 Apr 2020.

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CHEMICAL ENGINEERING COMMUNICATIONS
https://doi.org/10.1080/00986445.2020.1746657

Piperazine impregnation on Zeolite 13X as a novel adsorbent for CO2

capture: experimental and modeling
Fatemeh Fashia, Ahad Ghaemib , and Amir Hossein Behroozib
a
Chemical Engineering Department, Faculty of Energy, Kermanshah University of Technology, Kermanshah, Iran; bSchool of Chemical,
Petroleum and Gas Engineering, Iran University of Science and Technology, Tehran, Iran

ABSTRACT KEYWORDS
Zeolite 13X was modified using a piperazine solution for CO2 adsorption purposes. The Adsorption; CO2 capture;
operating parameters including temperature, pressure, piperazine concentration, adsorbent modeling; modified Zeolite
amount, and particle size are investigated experimentally to examine adsorption capacity. 13X; piperazine
The maximum adsorption capacity was obtained at temperature of 25
C, pressure of 8 bar,
piperazine concentration 2 wt.%, adsorbent amount of 1 g, and particle size of 200 mm. The
adsorption capacity for Zeolite 13X is increased from 193.844 to 242.084 mg g1 after modi-
fication. The empirical isotherm data are more consistent with Freundlich model. The best
adsorption kinetic model was Elovich model. The thermodynamic parameters represent the
spontaneous and exothermic of the process.

Introduction 2019). The amine-modified adsorbents have three

A batch of new adsorbents used to adsorb CO2 is
known as amine-modified adsorbents. In these
adsorbents, amine materials are deposited on
porous solid supports or the adsorbent structure
is modified with the amine. Amine-modified
adsorbents were created to enhance basic func-
tionality and improve some of the properties of
the solid adsorbents and consequently fix the
defects of amine solutions (Fashi et al. 2019;
Taheri et al. 2019). Amine-modified adsorbents
have the advantages of amine solutions, except
that these types of adsorbents are affordable and
able to lessen the energy consumption needed to
regeneration, increase the adsorption capacity,
and CO2 selectivity. They also cause less corro-
sion and less environmental pollution (Fashi
et al. 2019; Saeidi et al. 2018; Wang et al. 2019).
The important issues in these adsorbents are
the kinetic and adsorption mechanism, reactions,
and eventually the mass transfer rate and adsorp-
tion capacity (Karbalaei Mohammad et al. 2018;
Khajeh and Ghaemi 2020; Mohammad et al.
categories of amine impregnated, amine grafted,
and combine the first and second batches (Taheri
et al. 2019).
 The first group is prepared by physically loading
the amine on a porous solid support. The amine
is mixed with the support by the help of a solv-
ent, and then the additional solvent is evapo-
rated. There is no chemical reaction between the
amine groups and the support.
 In the second group, the amines of the sillane
group are bonded to the porous solid support
with covalent bonding. In this method, the rela-
tionship between support and amine is much
stronger than the first one.
 The third group is produced by polymerization
in the place of amino-polymers with porous
solid support (Meconi et al. 2019; Mittal 2013;
Ramezanipour Penchah et al. 2019).
The impregnation technique has been
employed more because of the advantages of easy
preparation, less corrosion, and high amine

CONTACT Ahad Ghaemi aghaemi@iust.ac.ir School of Chemical, Petroleum and Gas Engineering, Iran University of Science and Technology,
Tehran, Iran.
ß 2020 Taylor & Francis Group, LLC
2 F. FASHI ET AL.

Table 1. A summary of some studies on CO2 adsorption capacity using modified Zeolites.
Amine
concentration Adsorption
Researcher Year Support Amine (wt%) T (K) P (bar) capacity (mgg1) References
Jadhav et al. 2007 Zeolite 13X MEAa 10 303 0.15 1.0 Jadhav et al. (2007)
Son et al. 2008 KIT-6 PEIb 500 348 0.05 1.95 Son et al. (2008)
Fisher et al. 2009 b-Zeolite TEPAc 38 303 0.10 2.08 Fisher et al. (2009)
Chatti et al. 2009 Zeolite 13X MEA 348 1 0.45 Chatti et al. (2009)
IPAd 348 1 0.51
Su et al. 2010 Zeolite Y60 TEPA 50 333 0.15 4.27 Su et al. (2010)
Babaei et al. 2017 Zeolite NaY TEPA 10 348 1 2.11 Babaei et al. (2017)
DEAe 10 348 1 1.77
2-MAEf 10 348 1 1.94
a
Monoethanolamine.
b
Polyethylene impregnated.
c
Tetraethylenepentamine.
d
Isopropanolamine.
e
Diethanolamine.
f
2-(Methylamineo) ethanol.

adsorption capacity. The impregnation allows
more flexibility in the number of variables such
as amount and kind of impregnating compounds,
physico-chemical properties of supports, and co-
solvents addition. Polyethyleneimine (PEI)
(Sakwa-Novak et al. 2015), tetraethylenepent-
amine (TEPA) (Chen et al. 2009; Zeng and Bai
2014), and other alkylamines such as diethylentri-
amine, triethylenetetramine, and pentaethylene-
hexamine (Gibson et al. 2015; Sanz et al. 2015)
are the most common impregnating agents that
have been employed for the CO2 capture. Amine
adsorbents can be physically placed on different
supports (Taheri et al. 2019). One of these sup-
ports is Zeolite 13X. Zeolite is a mineral that
mainly consists of aluminosilicate and is in the
form of a crystalline network that contains oxy-
gen, aluminum, or silice. These materials are very
regular pores crystals of aluminosilicate. Zeolite
can be used for CO2 adsorption by presenting
the aluminum in the structure of silicate. The
adsorption kinetic of Zeolites is very desirable for
this purpose. In most cases, Zeolites will reach
the final adsorption capacity within minutes. The
most important reason for the interest of the
Zeolites category is that their properties, such as
porosity and structure or chemical composition,
affect their adsorption performance. Also,
Zeolites are included in the list of high-grade
adsorbents due to their abundant in the environ-
ment, thermal stability, regular pores, their ability
to adsorb and replace aluminum, low prices, and
biological features (Choi et al. 2009; Khajeh
Amiri et al. 2019; Sayari et al. 2011).
Su et al. modified a kind of commercial Zeolite
named Y60 with TEPA to study the features of
CO2 adsorption/desorption from the gas flows.
The nature of the Y60 surface has altered by
modifying with TEPA that will significantly
increase the adsorption capacity. The water vapor
after medication affected the CO2 adsorption cap-
acity and the capacity of 4.27 mmol g1 was
obtained at water vapor of 7%. The CO2 adsorp-
tion of Y60 is physical interaction mechanism
but after modification with TEPA, it was mainly
converted to chemical interaction mechanism (Su
et al. 2010).
Lee et al. modified a type of synthesis Zeolite
called Y8 with amines MEA, IPA, and TEPA
using the impregnation method to evaluate the
adsorption capacity of CO2 in an 80 l air cham-
ber. Based on the obtained results, the Y8
adsorption capacity was increased after modifica-
tion and the highest adsorption rate was higher
than 158 mg g1. Also, for all types of studied
amines, the order of adsorption capacity was
TEPA > MEA > IPA (Lee et al. 2013).
Bansiwal et al. investigated the CO2 adsorption
using functionalized adsorbents with MEA, DEA,
IPA, AMP, and EDAN amines on Zeolite 13X as
support at temperatures of 30, 55, and 75
C. The
adsorption capacity of these adsorbents was eval-
uated by a continuous stream in a filled bed
reactor and a stream of similar amounts of 15%
CO2 and N2 residue. The results showed that
after amine addition, the Zeolite adsorption
capacity increased significantly (Bansiwal
et al. 2014).

Babaei et al. modified a new type of synthesis
Zeolite called NaY by impregnation method to
study the effects of the adsorbent surface chang-
ing for CO2 adsorption using TEPA, DEA, and
2-MAE amines. The CO2 adsorption capacity was
measured by the volumetric method at 25 and
75
C and the adsorption capacity enhanced by
rising temperature. Before modification, the
adsorption capacity for Zeolite NaY was 82.8
and 73.51 mg g1 at the temperature of 25 and
75
C, respectively. Also, the CO2 adsorption
capacity on TEPA-NaY, DEA-NaY, and 2-
MAE-NaY adsorbents was measured as 60.63,
65.21, and 72.93 mg g1 at 25
C, and 92.9, 78,
and 85.42 mg g1 at 75
C, respectively. The
results proved that the nature of the NaY sur-
face changes with amines after modification
and a high potential for adsorption of CO2
under high temperatures was concluded for
amine-modified adsorbent (Babaei et al. 2017).
Some studies on the CO2 adsorption capacity
using modified Zeolites are present in Table 1.
Generally, physical impregnation is performed
using wet-impregnation method with an amine–-
solvent mixture and after that, the evaporation of
solvent has occurred. The mesoporous silicas
such as MCM-41, MCM-48, SBA-15, SBA-16,
and KIT-6 are the most common materials used
for this method because of their large pore vol-
ume and surface area. Also, the most common
used amines for this purpose are PEI, DETA,
DIPA, AMPD, TEA, PEHA, TEPA, MEA, AMP,
DEA, and EDA (Mart
ın et al. 2016).
Dindi et al. examined the effects of polyethyle-
nimine (PEI) impregnation on the CO2 capture
performance of an activated fly ash material.
Their results showed an enhancement in the sur-
face area from 11 to 270 m2 g1 by activating the
fly ash and the highest adsorption capacity of
26 mg g1 was obtained at 70
C and 25% PEI-
600 sorbent (Dindi et al. 2017). Numaguchi et al.
synthesized a new polyamine as an amine-
impregnated solid sorbent by screening the amine
compounds. Based on their results, the sorbent
was completely regenerable even at low tempera-
ture conditions (Numaguchi et al. 2017). Singo
et al. impregnated a sodalite zeolite-like metal
organic framework (sod-ZMOF) with chitosan
for CO2 capture. The maximum adsorption
CHEMICAL ENGINEERING COMMUNICATIONS 3
capacity for Sod-ZMOF-chitosan was 978 mg g1
at a temperature of 25
C, flow rate of
25 ml min1, and a pressure of 1 bar (Singo
et al. 2017).
In the last decade, a new species of Zeolites
have been developed by researchers and its prop-
erties have been investigated. Among the various
types of these Zeolites, Zeolite 13X is one of the
most common X-Zeolite species, and has been
widely studied for CO2 separation. In the current
study, Zeolite 13X was modified with piperazine
(Pz) by the impregnation method to increase the
adsorption intensity. Kinetic, isotherm, and its
thermodynamic were studied to investigate the
behavior of CO2 adsorption. Also, the influences
of different operating conditions such as tem-
perature, pressure, adsorbent’s amount, particle
size, and Pz concentration on the adsorption pro-
cess were evaluated.
Theory
Possible reaction mechanism
The amine-modified adsorbents in the CO2
adsorption contain the chemical reactions occur-
ring between the amine and CO2. In this reac-
tion, carbamate species are produced according
to the following reactions:
2RNH2 þ CO2 ! RNHCOO þ RNH3 þ (1)
RNHCOO þ H2 O ! RNH2 þ HCO3  (2)
An increase in the adsorption capacity of
amine-modified materials can be related to the
chemical interaction in the support pores. In fact,
a hybrid adsorption and adsorption mechanism
occurs in this type of modified adsorbent (Chatti
et al. 2009).
Experimental
Set-up
A batch reactor with a 3 cm inner radius, 9 cm
long, 254.34 cm3 internal volume, and stainless
steel material is used in the experimental set-up.
The environment was completely isolated for the
reactor using proper door and gas waste was
almost eliminated throughout the processing
time. The reactor chamber consists of a cell
4 F. FASHI ET AL.
Figure 1. The schematic view of the experimental set-up.
where the adsorbent was placed inside it. During
the process, the temperature and internal pres-
sure were displayed using a panel. All tests were
conducted with Zeolite 13X and modified Zeolite
13X. Materials were weighted by a digital scale
and shifted to the reactor cell and the cell was
finally placed inside the reactor. Before the pro-
cess starts, the pressure and temperature were
adapted. First, pure CO2 gas was entered into the
reactor chamber to regulate the initial CO2 pres-
sure using a connected valve and a pressure
gauge. By adjusting the pressure and temperature
at the desired points, adsorption runs for an hour
and storing 3600 data of temperature, pressure,
and time were done. This process was repeated
for various stages. The experimental set-up is
presented schematically in Fig. 1.
Materials
In this study, Granolas Zeolite 13X was supplied
by Sigma-Aldrich Company. Piperazine anhyd-
rous and methanol with a molecular weights of
86.14 and 46.07 g mol1 were prepared from
Merck chemical company, respectively. Also,
Well gas Sdn. Bhd was supplied a high pure CO2
gas with 99.999% purity.
Method of adsorbent modification
First, the distilled water was used to wash the
granolas Zeolite 13X and then it is dried in an
oven for 12 h at 100
C. The obtained product
was impregnated with 1, 2, 3, and 4 wt% Pz con-
centrations. For 1 wt% sample, 1 g and 99 g of the
Pz and methanol, respectively, were mixed using
a stirrer for 15 min. After that, the mixture was
stirred for 2 h at 35
C by adding the Zeolite 13X
with the amount of 5 g. A mercuric thermometer
was used to control the mixture temperature. The
final mixture was filtered, washed with methanol,
and dried in the oven at 60
C for 12 h to elimin-
ate methanol wholly. The preparation steps were
repeated for preparation concentrations of 2, 3,
and 4 wt%, by dissolving 2, 3, and 4 g of Pz in
the 98, 97, and 96 g of methanol, respectively. It
should be noted that the impregnation process
was performed at dry conditions and the effects
of humidity on the adsorbent was not investi-
gated in the current study.
Experimental measurement and conditions
The current study was carried out in the experi-
mental scale and a batch reactor. The influences
of operating conditions such as temperature (T),
pressure (P), amount of adsorbent (m), particle
size (d), and Pz concentration (CPz) to obtain
CO2 maximum adsorption using modified Zeolite
13X were investigated. The experiments were per-
formed under different temperatures of 25, 45,
65, and 85
C; pressures of 2, 4, 6, and 8 bar; par-
ticle sizes of 200, 300, 500 and 800 mm; the
adsorbent amount of 0.5, 1, 1.5, and 2 g; and Pz
concentration of 1, 2, 3 and 4 wt%. The effects of
each parameter were examined by considering
the other parameter constant.
The “adsorption capacity” and “adsorption
percentage” in the CO2 treatment process are cal-
culated through the following equations (Saeidi
et al. 2018):

Figure 2. XRD pattern of Zeolite 13X before and after modification with Pz solution.
ðPi  Pe ÞVMCO2
qe ¼  1000
RTm
Pi  Pe
Adsorption ð%Þ ¼  100
Pi
Results and discussion
Adsorbent characteristics
N2 adsorption and desorption, X-ray diffraction
(XRD), and Fourier Transform Infrared spectros-
copy (FTIR) techniques were utilized to charac-
terize the materials. The XRD analysis was
carried out in the range of 2h between 5
and
60
for composition and crystalline adsorbent
structure and identifying its phase. XRD device
STOE STADI-MP Germany model with Cu Ka
radiation, 40 kV voltage, and flow of 30 Ma was
used to perform the analysis. The phase analysis
was also carried out with X’ Pert High Score
Pluse software. The resulting pattern of XRD for
Zeolite 13X and modified Zeolite 13X is depicted
in Fig. 2. X-ray results showed that Zeolite 13X
has a major phase of amorphous with a structural
formula Na2Al2Si2 408.8, 6.7 H2O, and a silica
quarts substrate with a SiO2 structural formula.
The cavity peaks of the Zeolite 13X sample are
cubic with the crystallographic parameters
a ¼ 24.6760 Å, b ¼ 24.6760 Å, c ¼ 24.6760 Å and it
fits perfectly with the standard sample (JCPDS
PDF NO.00-043-0168) and no peak that shows
that the impurities were not detected. High and
CHEMICAL ENGINEERING COMMUNICATIONS 5
sharp peaks show the crystalline structure and
(3)
high crystallinity of Zeolite 13X. After modifica-
tion with Pz, there is no change in the X-ray pat-
(4)
tern of Zeolite 13X. The modification with amine
has no effects on the crystallinity and structure of
Zeolite 13X and the main peaks remain
unchanged but the capacity of the peaks has
dropped. This is due to the relative filling of the
pores and reduce the structural order of pores in
the structure of the material and this confirms
that the Pz has been successfully loaded onto the
support (Jadhav et al. 2007).
The functional groups in the adsorbent were
specified using FTIR device model Spectrum Rx1
manufactured by Perkin Elemer Company. Fig. 3
presents the FTIR spectrum for Zeolite 13X and
modified Zeolite 13X samples in a range of
400–4000 cm1, respectively. According to Figure
3, the broad and wide band of 3478 cm1 is con-
cerned with the stretches of O–H molecules of
water, the peak at 1644 cm1 is associated to
bending bond of water molecules, the peak at
977 cm1 is related to asymmetric stretch bonds
like T–O where T can be Si or Al. Also, the peak
at 752 cm1 is relevant to the external asymmet-
ric stretch bond of Si–O–Si, peaks of 672, 562,
and 464 cm1 are relevant to internal tetrahedron
stretch bond, six-member rings bond, and bend-
ing of T–O bond, respectively. After modifica-
tion, two new peaks in the wavenumbers range
of 2925 and 1444 cm1 are added to the FTIR
6 F. FASHI ET AL.
Figure 3. FTIR spectrum of Zeolite 13X before and after modification with Pz solution.
spectrum of Zeolite 13X which are related to
stretch bond of C–H and deformation vibration
stretch of CH2, respectively that indicates the
loading of Pz on the Zeolite 13X surface
(Gunasekaran and Anita 2008).
An automated gas sorption system was used to
perform the N2 desorption and adsorption at 77 K
and 7–22 kPa for the adsorption temperature of
and pressure, respectively (Micromeritics, Model
ASAP 2020, USA). This analysis of the studied
materials is represented in Figs. 4 and 5. Before
this analysis, the samples were heated to 120
C to
eliminate the water vapor, CO2, and other mole-
cules that may fill the materials’ volume. Using the
BET method, the pores’ volume and specific sur-
face area were measured. Table 2 shows the struc-
tural properties of the prepared adsorbents. As can
be seen for the modified Zeolite 13X, the values of
properties were decreased due to the entrance of
Pz particle into the Zeolite pores but its adsorption
capacity was increased because of its functionaliza-
tion with Pz leads to more reaction with CO2.
As it has resulted from Table 2, the values of
all the parameters have reduced after modifica-
tion; this shows that the Pz is filled and loaded
into the Zeolite 13X pores. The surface modifica-
tion shortens the pore space that causes the vari-
ation of pores’ specific volume and the specific
surface area (Kishor and Ghoshal 2017).
Effects of operating conditions
Based on response surface methodology (RSM)
results, the optimum conditions were obtained
1 g, 200 mm, 2 wt%, 25
C, and 8 bar for the
adsorbent’s amount, particle size, Pz concentra-
tion, temperature, and pressure, respectively. But
the aim of current study is considering the vari-
ation of one parameter, whereas the other param-
eters are kept fixed to examine the variation
trend of CO2 adsorption capacity experimentally.
Amount of adsorbent
The experiments were conducted at various
adsorbent amounts to evaluate the effects of
Zeolite 13X amount on the CO2 adsorption cap-
acity. As can be seen in Figs. 6 and 7, the adsorp-
tion capacity increases by decreasing the
adsorbent’s amount when other parameters are
kept fixed. Because of higher adsorbent surface
exposing to CO2 at lower adsorbent amounts,
CO2 gas diffuses into the more adsorbent surfaces
per mass unit, so adsorption capacity enhances.
In the experiments with a high amount of adsorb-
ent, by accumulating on the surface, CO2 diffusion
into the other layers is prevented. Also, at higher
adsorbent’s amount, the amount of pressure drop
is high and the adsorption capacity and the mass
ratio of adsorbate to adsorbent reduces. Although
the pressure was not in its optimum value but the
optimum value of adsorbent’s amount is obtained
1 g agreed with RSM results.
Mesh size
In this section, the particle size impacts on the
CO2 adsorption capacity are investigated while
other parameters are constant (25
C, 5 bar, and
1 g for the temperature, pressure, and adsorbent’s
 CHEMICAL ENGINEERING COMMUNICATIONS 7

Figure 4. N2 adsorption and desorption diagram for Zeolite 13X.

Figure 5. N2 adsorption and desorption diagram for modified Zeolite 13X.

Table 2. BET analysis for Zeolite 13X before and after modifi- gas leads to an increase in the mass transfer rate
cation with Pz solution. and the adsorption intensity. Although the post-
Adsorbent
combustion occurred around 1 bar but in the cur-
Parameters Modified Zeolite 13X Zeolite 13X
rent study, the pressure of 5 bar was used because
SBETa (m2/g) 16.576 23.524
Vtb (cm3/g) 0.259 0.424 the effects of each parameter were more distin-
Vpc (cm3/g) 0.071 0.086 guishable relative to 1 bar.
Pore sized (nm) 1.20 1.28
Micro-pore areae (m2/g) 26.180 37.516
The average pore diameterf (mn) 0.561 0.665 Pz concentration
a
Obtained by BET measurement.
b
The total hole Volume.MP-plot method.
The experiments were performed under various
c
Calculated by the BJH (desorption) method using N2 adsorp- Pz concentrations to examine its effects on the
tion isotherm.
d
Calculated by the BJH (desorption) method using N2 adsorp- adsorption capacity. The other conditions such as
e
tion isotherm. the particle size, adsorbent’s amount, pressure,
Obtained by the t-plot method.
f
Obtained by the MP-plot method and temperature were fixed at 200 mm, 1 g, 5 bar,
and 25
C, respectively. The results of adsorption
amount, respectively). The particle size is pre- capacity at equilibrium state and by time vari-
pared in meshes with 200, 300, 500, and 800 mm ation are shown in Figs. 10 and 11, respectively.
by crushing granolas Zeolite 13X and moving it At low Pz concentrations, the adsorption is per-
from the mesh strainer. As it was concluded formed chemically and physically and the
from Figs. 8 and 9, enhancement of the particle unoccupied surfaces for CO2 to penetrate
size causes a decrease in the CO2 adsorption cap- through the support are high. But at high Pz con-
acity due to the contact surface reduction. In centrations, collecting the Pz molecules on the
addition, the reduction of the particle size causes surface leads to lessening the adsorption capacity
the adsorbent surface to be more exposed to the of Pz, and consequently, the adsorption
8 F. FASHI ET AL.

Figure 6. Effects of Zeolite 13X amount on equilibrium CO2 adsorption capacity at temperature of 25
C, pressure of 5 bar, and
particle size of 200 mm.

Figure 7. Variation of CO2 adsorption capacity under various Zeolite 13X amounts at temperature of 25
C, pressure of 5 bar, and
particle size of 200 mm.

Figure 8. Effects of particle size on equilibrium CO2 adsorption capacity at temperature of 25
C, pressure of 5 bar, and adsorbent
amount of 1 g.

mechanism using the support prohibits. Temperature

Moreover, enhancing the Pz concentration
causes the pores to fill, thus the surface and
adsorption capacity decrease. Finally, at 2 wt%
as Pz concentration, the adsorption process is
conducted chemically by Pz. In addition, Fig.
12 shows the 3D graph for the effects of Pz
concentration on the CO2 adsorption capacity
using Zeolite 13X.
The effects of temperature on the CO2 adsorption
rate are investigated at 5 bar, 1 g, and 2 wt% for
the pressure, adsorbent’s amount, Pz concentra-
tion, respectively. As shown in Fig. 13, by
increasing the temperature, the gas adsorption
capacity decreases. Due to the exothermic reac-
tion in this study, the amount of removed CO2
decreases by increasing the temperature. It has
 CHEMICAL ENGINEERING COMMUNICATIONS 9

Figure 9. Variation of CO2 adsorption capacity under various mesh sizes at temperature of 25
C, pressure of 5 bar, and adsorbent
amount of 1 g.

Figure 10. Effects of Pz concentration on equilibrium CO2 adsorption capacity at temperature of 25
C, pressure of 5 bar, adsorbent
amount of 1 g, particle size of 200 mm.

Figure 11. Variation of CO2 adsorption capacity under various Pz concentrations (wt%) at temperature of 25
C, pressure of 5 bar,
adsorbent amount of 1 g, and particle size of 200 mm.

resulted that the adsorption capacity increases
from 130.456 to 148.725 mg g1 after modifica-
tion. A comparison of the CO2 adsorption cap-
acity for Zeolite 13X and modified Zeolite 13X at
different temperatures has been shown in Fig. 14.
This figure confirms that the adsorption capaci-
ties for the modified adsorbent are more than the
unmodified one at all temperatures. The 3D
graph for temperature effects on the CO2 adsorp-
tion capacity using modified Zeolite 13X is
shown in Fig. 15 for better understanding. As it
is clear in this figure, the CO2 adsorption cap-
acity reduces by increasing the temperature from
25 to 85
C as time elapses.
Pressure
The effects of pressure on the CO2 adsorption
capacity are shown in Fig. 16. As can be
observed, the percentage of removed CO2 enhan-
ces as the pressure increases, thus it indicates
10 F. FASHI ET AL.
Figure 12. 3D graph for piperazine concentration effects on CO2 adsorption capacity at temperature of 25
C, pressure of 5 bar,
adsorbent amount of 1 g, and particle size of 200 mm.
Figure 13. Variation of CO2 adsorption capacity using Zeolite 13X under various temperatures at pressure of 5 bar, adsorbent
amount of 1 g, and Pz concentration of 2 wt%.
that the positive impact of pressure on the
adsorption efficiency. Also, the chance of the gas
particles colliding with the surface of adsorbent
increases by enhancing the pressure. A compari-
son of the CO2 adsorption capacity for Zeolite
13X and modified Zeolite 13X at different pres-
sures is shown in Fig. 17. It shows that the modi-
fied Zeolite 13X has a higher adsorption rate
than the unmodified one. By modifying the
adsorbent, the adsorption capacity increases from
193.844 to 242.084 mg g1. Fig. 18 indicates a 3D
graph to present the pressure effects on CO2
adsorption capacity using modified Zeolite 13X.
As can be seen, the capacity is improved by
enhancing the pressure from 2 to 8 bar dur-
ing time.
Thermodynamic
Thermodynamics parameters include enthalpy
change (DH
), Gibbs free energy change (DG
),
and entropy change (DS
). These properties can
be computed by Equations (6) and (7)
DS
DH

Ln kd ¼  (6)
R RT
The value of standard Gibbs free energy is cal-
culated from equation below
DG
¼ DH
 TDS
(7)
As shown in Fig. 19, by plotting variations of
Ln(Kd) versus 1/T, a straight line is observed. By
computing the slope and the line intercept, DH

and DS
can be obtained, respectively. Fig. 20
shows the variation of CO2 adsorption percentage
versus temperature for modified Zeolite 13X. Table
3 shows the results of thermodynamic parameters
for modified Zeolite 13X at the pressure of 5 bar
(Rashidi et al. 2016; Tan et al. 2014).
The experimental tests were conducted at tem-
peratures of 298.15, 318.15, 338.15, and 358.15 K
and constant pressure of 5 bar. DH
has a value
with a minus sign which indicates an exothermic
adsorption process, and the adsorption rate
decreases by enhancing the temperature. The
negative value for DS
depicts that the irregular-
ity of the adsorption process reduces and this
 CHEMICAL ENGINEERING COMMUNICATIONS 11

Figure 14. Comparison of CO2 adsorption capacities for Zeolite 13X and modified Zeolite 13X at different temperatures; at pres-
sure of 5 bar, adsorbent amount of 1 g, and Pz concentration of 2 wt%.

Figure 15. 3D graph for temperature effects on CO2 adsorption capacity using modified Zeolite 13X at pressure of 5 bar, adsorbent
amount of 1 g, and Pz concentration of 2 wt%.

Figure 16. Variation of CO2 adsorption capacity using modified Zeolite 13X for various pressures at temperature of 25
C, adsorb-
ent amount of 1 g, and Pz concentration of 2 wt%.

shows that the specific adsorbent sites were filled
by the adsorbate molecules and also the adsorbate
molecules regularization. The enthalpy change
was assumed constant to investigate the DG
val-
ues at various temperatures. Its values are also
negative at all temperatures which present the
spontaneous adsorption process. Also as shown,
the DG
values are reduced by increasing the
temperature evidencing more adsorption capacity
at lower temperatures (Cui et al. 2010; Rashidi
et al. 2016).
Isotherm model
Adsorption data were analyzed by Langmuir,
Freundlich, and D–R isotherm models to a better
12 F. FASHI ET AL.

Figure 17. Comparison of CO2 adsorption capacities for Zeolite 13X and modified Zeolite 13X under various pressures; at tempera-
ture of 25
C, adsorbent amount of 1 g, and Pz concentration of 2 wt%.

Figure 18. 3D graph for pressure effects on CO2 adsorption capacity using modified Zeolite 13X under various pressures; at tem-
perature of 25
C, adsorbent amount of 1 g, and Pz concentration of 2 wt%.

Figure 19. Plot of Ln Kd vs. 1/T for CO2 adsorption using modified Zeolite 13X.

understanding of the adsorption mechanism of
CO2 molecules on the modified Zeolite 13X sur-
face with Pz. The isotherm parameters are deter-
mined under various pressures and at the
temperature of 25
C using the non-linear
method. This is a test and error method using an
optimization procedure to maximize the coeffi-
cient of determination (R2) between experimental
and predicted data (Ho 2006). The correlation
coefficient more and closer to 1 determines the
best model that has the highest compliance
with experimental data. Based on the equilib-
rium data and models presented in Table 4,
process behavior was studied with each model
which are explained in detail in the following
(see Fig. 21).

Figure 20. Variation of CO2 adsorption percentage with temperature using modified Zeolite 13X.
Table 3. Thermodynamics parameters of CO2 adsorption by
modified Zeolite 13X at pressure of 5 bar.
DG
(kJ mol1)
DH
DS

(kJ mol1) (kJ mol-1 K1) 298.15 318.15 338.15
140.340 0.334 40.681 33.996 27.310
From the R2 values, the most appropriate models
are Freundlich > Langmuir > D–R that Langmuir
and Freundlich models are well-coordinated and
only D–R model is weak. As can be seen in Table
4, the largest amount of R2 (¼0.9891) belongs to
the Freundlich model which verifies that this iso-
therm model is more proper than others. In the
Freundlich isotherm model, first, the stronger con-
nectivity places were occupied and then other places
by reduced energy (Adamson and Gast 1997;
Freundlich 1907; Langmuir 1916). In the Freundlich
model, there are constants “n” and “KF”, where n is
the utility index of the adsorption and indicates the
capacity of adsorption and KF represents the adsorp-
tion capacity. In this work, for modified Zeolite
13X, the values of n and 1/n are 1.531 and 0.653,
respectively which shows that the adsorption system
is acceptable and favorable. The value of mean
adsorption energy (E) in the D–R model indicates
the chemical or physical nature of the adsorption
process. As shown in Table 4, E value for modified
Zeolite 13X is less than 8 kJ/mol indicating that the
adsorption process is physical and much heat is not
generated (Aljeboree et al. 2017; Amrhar et al. 2015;
Ben-Mansour et al. 2016; Gadipelli and Guo 2015;
Monazam et al. 2013; Zheng et al. 2009).
Kinetics models
The kinetic behavior of the CO2 adsorption pro-
cess of modified Zeolite 13X was investigated by
CHEMICAL ENGINEERING COMMUNICATIONS 13
five kinetic models presented in Table 5. The kin-
etic parameters’ values were determined at four
different temperatures and pressure of 5 bar for
358.15
modified Zeolite 13X to determine the best kin-
20.625
etic model. On the other hand, using the non-lin-
ear form of the adsorption kinetic equations and
using data from Table 5 at 25
C, comparing kin-
etic adsorption models with experimental data is
performed in Fig. 22.
Based on the R2 values in Table 5, the weak-
ness of the first order and rate controlling model
is clear while the Elovich and second order mod-
els are suitable for empirical data of modified
Zeolite 13X. In particular, the first order model
can represent reversible interactions between
adsorbent and adsorbate. In contrast, the second
order model assumes that the interaction between
adsorbate and adsorbent was caused by a strong
gas connection to the adsorbent surface and used
when adsorption process involves chemical inter-
action. Elowich model is suitable to describe sys-
tems with heterogeneous adsorption surfaces, in
particular, adsorption of gases on solid surfaces
€
(Ammendola et al. 2017; Bulut et al. 2008; Ozacar
and Şengil 2005). According to the diagrams and
the comparison correlation coefficients for modi-
fied adsorbent, the Elovich model with R2 value
of 0.9953 is better than other models. Following
this model in this process is due to the heteroge-
neous adsorption mechanism of CO2 for modi-
fied Zeolite 13X. This means that uniform
surface of adsorbent is not available to adsorb
CO2 and active sites are not constant during
adsorption. Therefore, it is suggested that the
CO2 adsorption on modified Zeolite 13X can be
attributed to both chemical and physical
14 F. FASHI ET AL.

Table 4. Parameters of isotherm models of CO2 adsorption using modified Zeolite 13X at temperature of 25
C.
Isotherm models Nonlinear form Eq. number Parameters Modified Zeolite 13X
Langmuir 1916 qm 515.398
qe ¼ qm KL PCO2 =1 þ KL PCO2 (8) KL 0.120
R2 0.9869
Freundlich 1907 KF 66.201
qe ¼ KF PCO2 1=n (9) n 1.531
R2 0.9891
Dubinin-Radushkevich 1947 qm 245.382
qe ¼ qs exp ðKDR e2 Þ (10) KDR 0.901
E 0.745
R2 0.9663

Figure 21. Isotherm modeling of CO2 adsorption using modified Zeolite 13X at temperature of 25
C.

Table 5. Parameters of kinetic models of CO2 adsorption using modified Zeolite 13X at pressure of 5 bar.
Temperature (K)
Kinetic model Nonlinear form Eq. number Parameter 298.15 318.15 338.15 358.15
First order (Ho and Mckay 1999) qt ¼ qe :ð1  exp ðk1 :tÞÞ (11) qe 139.489 84.091 69.763 46.003
K1 0.00886 0.0080 0.00089 0.0194
R2 0.9158 0.8846 0.9608 0.8253
Second order (Ho and Mckay 1999) qt ¼ k2 :qe 2 ð1þk2t :qe :tÞ (12) qe 146.353 88.753 87.646 47.800
K2 0.0001 0.00014 0.00001 0.0005
R2 0.9764 0.9564 0.9672 0.8809
Ritchie second order (Ritche 1977) qt ¼ b: log ða:bÞ þ b: log ðtÞ (13) qe 146.353 88.753 87.646 47.80
k2 0.0147 0.0128 0.00094 0.2414
R2 0.9764 0.9564 0.9672 0.8809
Elovich (Ritche 1977) qt ¼ qe  ð1þK
qe
2 :tÞ
(14) a 0.785 0.468 0.001 7.708
b 14.148 9.409 15.819 4.257
R2 0.9953 0.9875 0.9467 0.8568
Rate controlling (Weber and Morris 1963) qt ¼ kid :t0:5 (15) Kid 3.109 1.877 1.231 1.041
R2 0.805 0.8450 0.993 0.8071

Figure 22. Kinetic modeling of CO2 adsorption using modified Zeolite 13X at pressure of 5 bar.

adsorption (Adelodun et al. 2017). On the other
hand, the results of the second order kinetic
model show that the obtained qe value of this
model is closer to the experimental qe and after
the Elovich model, the second order model is
consistent with experimental data. Considering
that adsorbent has been modified by Pz that is
chemical adsorbent, the second order model
shows well the chemical interactions in the modi-
fied adsorbent.
Conclusion
In this study, experimental study and modeling
of CO2 adsorption were performed using Zeolite
13X and modified Zeolite 13X with Pz solution.
Also, the effects of various parameters such as
temperature, pressure, amount of adsorbent, par-
ticle size, and Pz concentration on the adsorption
capacity were investigated by changing one par-
ameter and other fixed conditions. By isotherm,
kinetic, and thermodynamic modeling, the com-
parison between predicted and empirical data,
the adsorption process behavior was found to be
close to the ideal model. In addition, by increas-
ing the pressure and decreasing the temperature,
the adsorption amount increases. From the RSM
results, the highest amount of CO2 adsorption
was obtained at temperature of 25
C and pres-
sure of 8 bar for 1 g of adsorbent with particle
size of 200 mm and Pz concentration of 2 wt%.
The empirical isotherm data of the modified
Zeolite 13X was more consistent with the
Freundlich model. The best adsorption kinetic
model was determined by the Elovich model and
the results of thermodynamic modeling represent
the spontaneous and exothermic adsorption reac-
tion. Thus, the modified Zeolite 13X with Pz is a
new and good adsorbent to remove CO2 from air
and natural gas.
Nomenclature
KL angmuir constant, bar-1
kF Freundlich constant, cm3 g1 bar1/n
kf rate constant of pseudo-first order adsorp-
tion, min1
ks rate constant of the pseudo-second order kinet-
ics, g mg1 min1
CHEMICAL ENGINEERING COMMUNICATIONS 15
k2 reaction rate constant of Ritchie second order
equation, min1
kid intraparticle diffusion rate con-
stant, mg g1 min1
MCO2 molar mass of carbon dioxide, g mol1
m mass of adsorbent, g
N total number of experiments required
n number of variables
Pi initial pressure, bar
Pe equilibrium pressure, bar
qe equilibrium adsorption capacity, mg g1
qm maximum CO2 adsorption capacity, mg g1
qt amount of adsorbed CO2 at time t
R universal gas constant, 8.314 J mol1 K1
R2 correlation coefficient
RL dimensionless constant
T temperature of the reactor, K
t reaction time, min
V volume of the reactor occupied by the CO2
gas, mL
W grams of adsorbent, g
Greek letters
a initial adsorption rate, mg g1 min1
b desorption constant, g mg1
k D–R constant, mol2 J2
x Polanyi potential (equivalent to RT ln(1/1 þ P))
DH
enthalpy change, kJ mol1
DS
entropy change, kJ mol1 K1
DG
Gibbs free energy change, kJ mol1
ORCID
Ahad Ghaemi http://orcid.org/0000-0003-0390-4083
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