Sorption of Carbon Dioxide, Methane,
and Nitrogen on Zeolite-F: Equilibrium
Adsorption Study
Mihir R. Belani, Rajesh S. Somani, and Hari C. Bajaj
Inorganic Materials and Catalysis Division, Central Salt and Marine Chemicals Research Institute, Council of Scientific and
Industrial Research, (CSIR - CSMCRI), Bhavnagar, Gujarat 364002, India; hcbajaj@csmcri.org (for correspondence)
Published online 00 Month 2017 in Wiley Online Library (wileyonlinelibrary.com). DOI 10.1002/ep.12524
Carbon dioxide is a major contributor in greenhouse gases.
Unswerving increase of CO2 in atmosphere, due to growing
industries and automobile field, is a wakeup call to the world
as excess of CO2 will affect humans in many ways among
which greenhouse effect dominated the most. In the present
work potassium based zeolite-F was synthesized by hydrother-
mal method as reported by International Zeolite Association.
Synthesized zeolite-F was characterized with powder X-Ray
diffraction analysis, FT-IR spectroscopy, scanning electron
microscopy, thermo gravimetric analysis and BET surface
area measurement. The equilibrium adsorption capacities of
pure gases CO2, N2, and CH4 were measured at 273, 288, and
303 K up to 850 mmHg. Although zeolite-F possesses low CO2
adsorption capacity (43.6cc/g) at 303 K, the selectivity towards
N2 and CH4 reflects its potential as an efficient CO2 adsorbent.
The selectivity of CO2 over N2 in zeolite-F was 38 at 303 K and
850 mmHg pressure, whereas selectivity for CO2 over CH4 was
30. Thus, zeolite-F has shown potential for selective CO2
adsorption from its gas mixture with N2 and CH4. V C 2017 Ameri-
can Institute of Chemical Engineers Environ Prog, 00: 000–000, 2017
Keywords: zeolite-F, carbon dioxide, methane, nitrogen,
adsorption
INTRODUCTION
Increase in the atmospheric CO2 concentration (407.7
ppm, May, 2016 [1]) has gained interest among researchers
worldwide to put their efforts on reduction of CO2 emis-
sions. Fossil fuel based power plants, vehicles, hydrogen,
and ammonia production and residential buildings are
among those sources, which generate CO2 in larger propor-
tions. CO2 capture and sequestration may be termed as first
step in order to achieve optimum level of CO2 concentration
back. CO2 capture technologies such as absorption, adsorp-
tion, and membrane separation are useful. Absorption is
more of energy consuming while membrane separation
requires use of hazardous reagents as initiators. Therefore,
adsorption is considered to be more useful than other two
discussed techniques. The well-known potential adsorbents
reported for CO2 separation are activated carbon [2,3], graph-
ite/graphene-based adsorbents [4,5], zeolites [6,7], silica
based adsorbents [8], MOFs [9], carbon nanotubes [10], and
nanoporous silica-based molecular basket [11].
C 2017 American Institute of Chemical Engineers
V IZA [18]. Accordingly, 9.26 g potassium hydroxide (AR, 85%,
Environmental Progress & Sustainable Energy (Vol.00, No.00) DOI 10.1002/ep
Zeolites, a class of porous crystalline aluminosilicates, con-
structed of an episodic array of TO4 tetrahedral (T 5 Si or Al),
which are widely used in separation applications mainly
because of their unique molecular sieving property for liquid
and gaseous molecules [12,13]. The presence of aluminum
atoms in silica based molecular sieve materials introduce nega-
tive framework charges that are compensated by exchangeable
cations in the pore space (often alkali cations) and these struc-
tural characteristics of zeolites enable them to adsorb a wide
variety of gas molecules, including modern world’s antagonist
CO2. Today there are over 250 unique zeolite topologies
indexed by the International Zeolite Association (IZA). Zeolite
is a conventional adsorbent that is useful in capturing CO2 due
to its pore structure and high surface area. Brown et al. studied
CO2 adsorption on SSZ-13 [14], wherein Cu-SSZ-13 showed
significantly higher CO2 adsorption (89 cc/g), its modified
Cu-form showed slight lower CO2 adsorption (84 cc/g).
Dangi et al. [15] reported the CO2 adsorption (59 cc/g) at 303 K
on zeolite-L. Chatti R. et al. [16] have reported breakthrough
study on modified Na-X zeolite with 24 mg/g CO2 adsorption.
Lei Wu et al. [17] reported amino-modified MIL-68(In) with
enhanced hydrogen and CO2 sorption enthalpy. Among the
modifiers used, 2-amino-terephthalic acid showed 53 cc/g CO2
adsorption at 273 K. Particularly studies reported by Brown
and Dangi et al. motivated us to pursue CO2 adsorption on
zeolite-F. Zeolite-F showed comparable volumetric equilibri-
um adsorption capacity of CO2 (64 cc/g) at 273 K (Table 1)
with those adsorbents reported in the literature.
In continuation of our work on potassium based zeolites
[15], in this communication we focused on zeolite-F, having
formula K10(Al10Si10O40)• wH2O (w 5 8). It was synthesized
from the batch composition 5.26 K2O: Al2O3: 3 Si02:
94.5 H2O [18] that have been hardly studied for gas adsorp-
tion [19,20]. In this study, we used zeolite-F for adsorption of
CO2, CH4, and N2. Zeolite-F was synthesized in our laborato-
ry using known protocol [18]. Its structure resembles with
the naturally occurring Edingtonite type zeolite. Unit cell
data shows that zeolite-F contains tetragonal phase. It also
contains edge length of a 5 6.9 and c 5 6.4 Å [21].
MATERIALS AND METHODS
Synthesis of Zeolite-F
Zeolite-F was synthesized using method recommended by
Month 2017 1
Table 1. Comparison of CO2 adsorption capacity of various adsorbents reported in the literature.

CO2 adsorption
Adsorbent Modification capacity (cm3/g) Conditions References
SSZ-13 H-form 89 298 K, 760 mmHg [14]
SSZ-13 Cu-form 84 298 K, 760 mmHg [14]
K-L Cation exchange 59 303 K, 760 mmHg [15]
Na-X Monoethanolamine (MEA) 25 348 K, 760 mmHg [16]
MIL-68 2-Aminoterephthalic acid 53 273 K, 760 mmHg [17]
Terephthalic acid/amino 50 273 K, 760 mmHg
terephthalic acid
35 298 K, 760 mmHg
Zeolite-13X As such 04 Relative humidity study [6]
Silica APTES-grafting 47 298 K, 760 mmHg [29]
b-zeolite As such 39 303 K, 760mmHg [30]
b-zeolite MEA 17 303 K, 760 mmHg [30]

Rankem, India) is added to 20 mL distilled water under stirring.

After KOH gets dissolved in water it is divided in to two parts.
In part-1, 0.719 g Aluminium wire (99.9%, Sigma Aldrich) was
added and refluxed for 5 h. In part-2, fumed silica (Cab-O-Sil)
was added and then stirred for 5 h. Both the solutions were fil-
tered and stored in plastic bottles. Afterwards both the solu-
tions were mixed and gel formation takes place. Mechanical
stirring at 1000 rpm was applied for 5 min. Crystallization of
gel was accomplished at 958C 96 h in a closed system. The
required product (zeolite –F) was recovered by centrifugation
and washed with distilled water till the filtrate pH was 8 to 9.

Characterization of Zeolite-F
The powder X-ray diffraction (PXRD) patterns of synthe-
sized samples were recorded with a PANalytical (model:
Empyrean X’PERT-PRO XRD) with CuKa radiation
(k 5 1.5406 Å) on an advance X-ray powder diffractometer.
PXRD patterns were collected using scan step time 20, 40,
60, and 80 s for each step size (2 h) considering as 0.0130,
and 2h ranging from 5 to 508. Thermogravimetric analyzer
(NETZSCH TG 209F1 Libra TGA209F1D-0105-L) was used for
the investigation of thermal stability of the synthesized
zeolite-F under the argon atmosphere at the heating rate of
108C min21 from 30 to 8008C. Microscopic images of zeolite-
F samples were collected using FE-SEM JEOL JSM 7100F.
The surface area measurement of the zeolite-F samples
was carried out using static volumetric gas adsorption analyz-
er system (Model-ASAP 2020, Micromeritics) by obtaining N2
adsorption/desorption isotherms at 77 K. Prior to the adsorp-
tion measurement the sample was degassed overnight under
vacuum (5 3 1026 mmHg) at 623 K.
Equilibrium Adsorption Measurements
Zeolite samples being hydrophilic in nature were dried at
383 K for 10 h in an oven. Prior to adsorption measurements, the
samples were out gassed by heating up to 623 K, at a heating rate
of 1 K min21 under vacuum (5 3 1023 mmHg) for 5 h using a
degassing system. CO2, N2, and CH4 adsorption isotherms were
measured at 273, 288, and 303 K using a static volumetric system
(Model-ASAP-2020, Micromeritics, Figure 1). Adsorption tempera-
ture was maintained by circulating water from a constant temper-
ature water bath (Julabo F25, Seelbach, Germany). Adsorption
capacity, as the volume of gas adsorbed per gram of adsorbent,
was measured at 278, 288, and 303 K up to 850 mmHg.
Figure 1. Volumetric CO2 adsorption unit (ASAP-2020,
Micromeritics). [Color figure can be viewed at wileyonline-
library.com]
synthesized material having a good agreement in the peak
positions with those of the zeolite-F [18] (Figure 2b) JCPDS
data file no. 00-038-0216. Effect of variation of scan step time
on the XRD pattern is shown in Figure 3, which confirms
that higher scan step time gives more precise data. If the
scan step time is reduced, it may give erroneous results
while analyzing the data [22]. By increasing scan step time,
we observed high increment in intensity at 2h 5 138, which
corresponds to (001) plane, from this one can say that it is
the case of preferential orientation [23].
Thermogravimetric Analysis
The thermogravimetric and differential thermal profile for
zeolite-F is shown in Figure 4. The weight loss, in the tempera-
ture range of 50–2608C can be attributed to adsorbed water loss.
The observed weight loss was 10 wt % only. After removal of
water zeolite-F structure remained almost stable upto 8008C that
confirms that zeolite-F is thermally stable adsorbent.

RESULTS AND DISCUSSION FTIR Spectroscopy

The FTIR spectrum of zeolite-F is shown in Figure 5. The
Powder X-Ray Diffraction deformation and mixed vibration of silicon aluminum lattice
The PXRD pattern for zeolite-F is shown in Figure 2a. The absorption peaks in the range 760–440 cm21 are observed.
diffraction pattern indicates well crystalline nature of The strong infrared absorption band at 1010 cm21 is

2 Month 2017 Environmental Progress & Sustainable Energy (Vol.00, No.00) DOI 10.1002/ep

Figure 2. (a) PXRD pattern of zeolite-F and (b) Comparison
of XRD patterns of Zeolite-F (1) reported [15] and (2) Labora-
tory synthesized sample. [Color figure can be viewed at
wileyonlinelibrary.com]
Figure 3. Effect of scan time on PXRD pattern of zeolite-F.
[Color figure can be viewed at wileyonlinelibrary.com]
assigned to vibration of (Al, Si) – O bonds. The absorption
bands in the range 3607–3460 cm21 are vibration of AOH
bond. The vibrations in the region 1657 cm21 can be
assigned to the presence of zeolitic water. Most intense
band, assigned to antisymmetric O-T-O stretching vibration,
lies in the 1200–950 cm21 range.
Scanning Electron Microscopy
SEM images of zeolite-F showed assembly of cotton-
candy-like [24] morphology (Figures 6a–6d) in contrast to the
reported prism like morphology [25]. This may be due to the
difference in synthesis protocol and conditions.
Environmental Progress & Sustainable Energy (Vol.00, No.00) DOI 10.1002/ep
Figure 4. TGA and DTA profiles of zeolite-F. [Color figure
can be viewed at wileyonlinelibrary.com]
Figure 5. IR spectrum of zeolite-F.
N2 Adsorption-Desorption Isotherm
The N2 adsorption-desorption isotherm of zeolite-F mea-
sured at 77 K for powder sample is shown in Figure 7. The
isotherm reveals slow uptake up to p/p0 5 0.6 and then gives
continuous increase in uptake till relative pressure reached
p/p0 5 0.9. After that, it increased drastically till the satura-
tion. The BET and Langmuir surface area of powder zeolite-
F, was calculated from N2 adsorption-desorption data at 77 K
using BET and Langmuir equations, and were found to be 54
and 78 m2/g, respectively, with total pore volume of 0.14
cm3/g at p/p0 5 0.97. The N2-isotherm can be classified as
Type-III, which indicates adsorption on non-porous/macro-
porous solid with weak adsorption of nitrogen. The t-plot
method was adopted for micropore analysis to obtain micro-
pore volume, micropore surface area, and external surface
area. These values were found to be 0.002 cm3/g, 4.47 m2/g,
and 48.05 m2/g, respectively. Higher value of external sur-
face area as compared with micropore surface area is a proof
of less entrapment of N2 in the pores of zeolite-F. The t-plot
curve was well fitted to linear, as shown in Figure 8.
Differential Pore Volume and Surface Area Distribution
Differential pore volume was calculated using Barret-
Joyner-Halenda (BJH) model and the Horvath-Kawazaoe
(HK) method. The BJH model is used for calculation of the
pore size distributions (PSD) in the mesoporous range and a
Month 2017 3
Figure 6. SEM images of zeolite-F at different magnifications. (a) 33300, (b) 38500, (c) 313,000, and (d) 323,000.

Figure 7. N2 adsorption-desorption isotherms of zeolite-F at

77 K. [Color figure can be viewed at wileyonlinelibrary. Figure 8. The t-plot for zeolite-F.
com]

respectively. It is observed that at a given pressure, adsorp-

small part of a microporous range [26]. The HK model is
developed for Slit-like micropores [27]. It is priggishly used
to determine the microporous materials. The comparison of
PSD obtained using BJH and HK models is shown in Figure
9. PSD observed by BJH method shows comparatively high
pore volume at 2.5 nm. Same phenomenon was observed by
HK model, which depict 5–10 nm pores are present in zeo-
lite F.
CO2 Adsorption
The adsorption isotherms of CO2, N2, and CH4 measured
at three different temperatures, that is, 273, 288, and 303 K
of zeolite-F up to 850 mmHg is shown in Figures 10–12,
tion capacity increases with the decrease in temperature.
This can be understood simply on the basis of the kinetic
energy of adsorbate molecules, which is proportional to the
temperature. Increasing temperature makes adsorbate mole-
cules energized enough to desorb from the surface. The
adsorption isotherms (Figures 9–11) of different gases clearly
indicates the adsorption capacity of CO2 is much higher than
those of all other gases studied; and the order of adsorption
capacity is CO2  CH4 > N2. Main highlight of the present
study (Table 2) is the higher adsorption of CO2 at low pres-
sure (51 cc/g at 15 mmHg and 65 cc/g at 850 mmHg pres-
sure). It revealed that very high CO2 adsorption take place at
very low absolute pressure (15 mmHg) and the adsorbent

4 Month 2017 Environmental Progress & Sustainable Energy (Vol.00, No.00) DOI 10.1002/ep
 Figure 11. N2 adsorption on zeolite-F at different tempera-
Figure 9. PSD of synthsized zeolite-F obtained by BJH and
tures. [Color figure can be viewed at wileyonlinelibrary.
HK models. [Color figure can be viewed at wileyonlineli-
com]
brary.com]

Figure 12. CH4 adsorption on zeolite-F at different tempera-

Figure 10. CO2 adsorption on zeolite-F at different tempera- tures. [Color figure can be viewed at wileyonlinelibrary.
tures (Inset image shows 80–85% saturation by CO2 at very com]
low absolute pressure). [Color figure can be viewed at
wileyonlinelibrary.com]

Table 2. Adsorption capacity of CO2 on zeolite-F at 15 and

get saturated up to 80–85% (inset image in Figure 10). Favor- 850 mmHg at 273, 288, and 303 K.
ably, lower uptake for CH4 and N2 were observed at all the
three temperatures at 850 mmHg. These results revealed that CO2 adsorption
zeolite-F can auspiciously adsorb CO2 over CH4 and N2. The capacity (cm3/g)
higher uptake of CO2 was due to its higher quadrupole Temperature 15 mmHg 850 mmHg
moment (13.4 3 10240 C m2) and polarizability (26.3 3
10225 cm3) compared with CH4 (0 C m2 and 26.0 3 10225 273 K 51 65
cm3) and N2 (4.7 3 10240 C m2 and 17.6 3 10225 cm3) [28]. 288 K 39 55
The higher uptake of methane over nitrogen may be due to 303 K 31 44
the higher polarizability of methane than nitrogen. Notable
higher selectivity for CO2 in comparison to methane and
nitrogen gas {CH4 (CO2/CH4 530).and N2 (CO2/N2 5 38)} is
one of the key advancement from this study. The selectivity The equilibrium selectivity (Table 3) of a gas “M” over gas
of the above gases at three different temperatures for zeolite- “N” was calculated using Eq. 1.
F is calculated from equilibrium adsorption capacities (Table
2). It is observed that with an increase in adsorption temper- qM
a5 (1)
ature the selectivity of CO2 and CH4 over nitrogen increases qN
due to comparative poor electrostatic interactions between
nitrogen and zeolite-F at higher temperature. The selectivity where, qM and qN are the quantity (cc/g) of M and N
was found to be CO2/N2 > CO2/CH4. adsorbed, respectively.

Environmental Progress & Sustainable Energy (Vol.00, No.00) DOI 10.1002/ep Month 2017 5
Table 3. Equilibrium adsorption selectivity of CO2/N2, CO2/
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