July 2010, Volume 1, No.

1
International Journal of Chemical and Environmental Engineering

Separation of Carbon Dioxide Using Selected

Porous Materials: A Review
Baba U.M., Kamarudin K. S. N. and N. Alias
Department of Gas Engineering, Faculty of Chemical and Natural Resources Engineering,
Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor

* Corresponding author;
Tel: + 6055535482, Fax: + 607 5581463
E-mail: sozana@fkkksa.utm.my

Abstr act
The use of porous adsorbents for CO2 capture and separation is presented, highlighting the important advances in their
research over the past decades. These adsorbents find application commercially due to their tunable pore size and shape,
their applicability over wide range of temperatures and pressures. Surface modification using amines is carried out in
order to improve their affinity and selectivity towards CO2. The commercial/industrial applications of these adsorbents in
cyclic adsorption process (PSA, VSA, TSA) are also discussed. Adsorption technology using solid sorbents with high
selectivity and affinity towards CO2 could provide alternative over conventional techniques. Some of these sorbents have
been shown to effectively adsorb CO2 where the gas stream contain vapor or moisture, as such it is possible to eliminate
the dehumidification step. In addition, these materials are synthesized from relatively cheap source and also occur
naturally.

Keywords – separation, porous, solid adsorbent, CO2, adsorption.

1.0 INTRODUCTION
Adsorption and separation of carbon dioxide (CO2)
using porous, solid adsorbents has received tremendous
attention in the past decades mostly in the area of energy
and environment, which include the control of carbon
dioxide emissions. CO2 present in the atmosphere, natural
gas, and exhaust gas of fossil fuels combustion and exist
as by-product from industrial processes. Its concentration
in the atmosphere has risen by more than 30% since the
industrial revolution and has been identified as one of the
main component responsible for the ever increasing
weather disasters. Several options exist to reduce the
emission of CO2, including the substitution of nuclear
power for fossil fuels, increasing the efficiency of fossil
plants, substitution of natural gas for coal, and the
separation and capture of CO2 prior to emission into the
environment [1]-[3]. All of these techniques have the
attractive feature of limiting the amount of CO2 emitted
into the atmosphere but each has economic, technical and
societal limitations.
Absorption using aqueous solutions of alkanolamine
is among the most widely used methods [4]. Other
techniques include membrane separation, and cryogenic
distillation. In spite the efficiency of these processes, their
major drawbacks include the large amount of energy
required for regeneration, equipment corrosion, solvent
degradation in the presence of oxygen and membrane
fouling.
Separation based on solid sorbents might be an
alternative and has been proposed as suitable candidate
due to their highly developed porous structure.
Adsorption using a wide range of solid adsorbents in
adsorption separation process including pressure swing
adsorption (PSA) [5], vacuum swing adsorption (VSA)
[6] and temperature swing adsorption (TSA) [7] is
receiving great attention due to the low energy
requirement, cost advantage, and ease of applicability
over a relatively wide range of temperatures and
pressures. These processes are of particular interest in
bulk gas separation and purification and other chemical
processes. Therefore, development of regenerable
sorbents having high selectivi ty and capacity, high
 Separation of Carbon Dioxide Using Selected Porous Materials: A Review
adsorption/desorption rate for CO2 is crucial for the
success of an adsorption based separation process.
This article reviews the state of art of several types of
porous materials with high capacity for CO2 that find
both industrial and commercial application for CO2
removal and separation from various gas mixtures,
their surface modification (chemical, cationic exchange
and grafting of amine) in order to improve their
capacity and selectivity.
2. ADSORBENTS FOR CO2 SEPARATI ON
Porous adsorbents have attracted much attention
due to the commercial interest in their application in
chemical separation, natural gas purification and
heterogeneous catalysis, as well as scientific interest in
the challenges posed by their synthesis and
characterization procedures. Both natural and synthetic
porous adsorbents are used for the separation of CO2
from various gas mixt ures. Molecular sieve activated
carbon [8] and zeolites [9] are the most widely
investigated. Others include mesoporous materials such
as the MCM-41 [10] and SBA-15 [11], metal organic
frameworks (MOFs) [12], and hydrotalcite-like
compounds (HTlcs) [13]. Pores present in such
materials are classified according to the IUPAC
scheme and may be made of exclusively one pore or a
distribution of pore widths.
Separation by adsorption is based on the selective
accumulation of one or more components of a gas
mixture on a solid surface (adsorbent). When a gaseous
mixture is exposed to an adsorbent for sufficient time,
equilibrium is established between the adsorbate and
the gas phase. The gas phase becomes richer in the less
selectively adsorbed component. The attractive forces
responsible for the adsorption are of the Van der Waals
type. Desorption can be achieved by either increasing
the temperature of the system or by reducing the
adsorbate pressure. The desorption step also
regenerates the adsorbent surface for reuse during the
subsequent adsorption step. Thus, the adsorptive
separation process consists of a cyclic sequence of
adsorption and desorption steps. When desorption is
achieved by increasing the system temperature, the
system is called thermal swing adsorption (TSA).
When desorption is achieved by decreasing the
pressure, the process is called pressure swing
adsorption (PSA). One of the components of a gas is
selectively adsorbed at a higher partial pressure and
desorbed subsequently by lowering the partial pressure.
The change in partial pressure of the gas can be caused
either by decreasing the total pressure, changing the
composition of the gaseous mixture, or by a
combination of both [14].
41
Porous Carbon
Porous carbon, especially activated carbon are very
versatile adsorbents of industrial importance and are used
in a wide range of applications that are concerned mainly
with the removal of undesired species by adsorption.
They also find application in catalysis or catalyst supports
[17]. There are numerous experimental data available in
literature of single and binary mixtures on several porous
carbon including carbon dioxide (CO2), methane (CH4),
nitrogen (N2) and hydrogen (H2) at different ranges of
temperatures and pressures [8], [15]. Van der Vaart et al
[8] reported the single and mixed gas adsorption
equilibrium of CO2/CH4 on a Norit RBI with an
adsorption capacity of 108 mg/g-adsorbent at 21.5 oC.
Himeno et al. [15] presented experimental data obtained
for the adsorption of CO2 and CH4 onto five activated
carbons at temperatures ranging from (273 to 333) K and
pressures up to 6KPa. Maximum adsorption was obtained
in the isotherms of carbon dioxide at 283 K and pressures
> 3.5 Mpa. For all the activated carbons investigated, the
amount of CO2 adsorbed was about twice that of CH4.
Maxorb had the highest CO2 capacity where the order of
adsorption capacity is as follows: Maxsorb > activated
carbon A >Norit R1 Extra > A10 > BPL.
Recently, some rigid and designated inorganic
templates such as SBA-15 and zeolite have been used in
an attempt to synthesize porous carbons with uniform
pore size and large surface area. The general template
synthesis procedure involves the preparation of the carbon
precursor or an inorganic template composite, followed
by carbonization and lastly the removal of the inorganic
template [16]. This method known as replica synthesis
produces materials with very large surface area and pore
volume (Figure 1). Ma et al. [17], [18] reported the
synthesis of a material having large surface area up to
3600 m2/g and 1.5 cm3/g pore volume with almost no
mesoporosity. Zhou et al. [19] used SBA 15 as a template
to synthesize a microporous molecular sieve carbon
nanorods. Tetraethyl orthosilicate (TEOS) of analysis
grade and sucrose were used as silica and source
respectively. The material had a specific surface area of
about 1100 m2/g and pore volume of 1.3 cm3/g and
showed higher affinity for CO2 than the other gases (NH4,
N2 and O2) tested under the same experimental condition.
Fig 1. Schematic, explaining the overall template synthetic procedure for
microporous carbon using zeolite Y as template [16].
Zeolites
Other than porous carbon, zeolites are among the
most widely investigated adsorbents for CO2 separation
 Separation of Carbon Dioxide Using Selected Porous Materials: A Review
(Figure 2). Both natural and synthetic zeolites are
employed for CO2 gas separation and purification. The
adsorption characteristics of any zeolite are dependent
upon the detailed chemical/structural makeup of the
adsorbent [20], [21]. According to Bonenfant et al. [22],
the capacity of CO2 depends mainly on the basicity and
electric field in their cavities as well as the size of both
the pores and the adsorbate molecule. Other factors
include the polarization power, distribution and number of
cations, the Si/Al ratio, and the nature of carbonates
formed at their surface. The thermal treatment and the
resulting level of dehydration may also affect the final
properties of the adsorbent [20]. Many of these factors
have been extensively studied for both synthetic [23] and
natural zeolites [20]. Detail review on these factors can be
found in other literature [22].
Fig 2. Schematic diagram of zeolite 4A [21].
Experimental investigations into the CO2 removal
from CO2/N2 mixture using several types of zeolites
revealed that indeed the cation type as well as the Si/Al
ratio had a profound effect on CO2 adsorption [13].
Among the zeolites investigated, NaY, 13X, ZSM-5 and
5A were found promising. 5A is one of the lowest Si/Al
ration among the zeolites studied and also contained the
Ca2+ cation followed by 13X, NaY and ZSM-5 which
contained the Na+ cation. 5A exhibited the strongest net
cation-quadrapole interaction with about 8 sites per
molecule. Lower Si/Al ratios require more cations to
balance the charge distribution within the structure and
result in high degree of heterogeneity.
Hydrotalcite-like Compounds (HTlcs)
The HTlcs compounds are receiving considerable
attention in recent years due to their wide range of
applications, such as catalyst, ion exchangers, filters,
decolorizing agents, industrial adsorbents. Exchange of
the metal cations, as well as intercalation of the anionic
layer can lead to a wide range of catalytic adsorption
properties with particular stability under wet gas and
high-temperature conditions [13]. Thus such materials are
potentially suitable for high temperature application in
gas separation. Figure 3 shows the structure of HTlcs
where M2+ and M3+ represents di- and tri-valent cation
which, with the –OH molecules, form the layered
structure of the HTlcs. The interlayer spacing is occupied
42
with charge-compensating anions (An-1) and water
molecules [24].
Fig 3. Structure of hydrotalcite compound [24].
Factors influencing CO2 adsorption on these
materials include aluminum content, anion type, water
content as well as the heat treatment temperature. The
effect of these factors on CO2 adsorption at high
temperatures was investigated on several commercially
supplied HTlcs at higher temperatures (300 oC) [25].
Their results revealed that the capacity for CO2 increases
when the amount of aluminum was decreased and that
there is an optimum aluminum content in the HTlcs for
adsorption of CO2. The presence of small amount of water
in the HTlcs also favors the adsorption capacity.
Similarly, under dry and wet feed condition, the capacity
for the wet feed conditions was found to be approximately
10% higher than for the dry feed condition [13].
Adsorption capacities of HTlcs having CO32- and OH-
anion reveal that the HTlcs containing CO32- show higher
adsorption capacities than those containing OH-. The
effect of temperature was carried out at low temperatures
(20 oC) and higher temperatures (200 oC and 300 oC)
where the order of adsorption was given as Q (300 oC)> Q
(20 oC)> Q(200 oC). The reason for this is that HTlcs have
different thermal decomposition behaviors at different
stages of calcinations. The highest capacity obtained for
the HTlcs samples was slightly higher than 0.30 mmol/g.
Metal Organic Frameworks (MOFs).
Metal organic frameworks (MOFs), also known as
coordination polymers are a relatively new class of porous
materials with high diversity and find application in
separation process, catalysis and gas storage [26]. These
materials are formed by coordination bonds from
multidentate ligands to mono- or polynuclear metal
centers and may have extensive open-framework
structures resulting in the inclusion of guest species
(usually solvent) during synthesis. These species can be
removed via desolvation and the resulting empty
framework may maintain structural integrity giving a
porous MOF material with large surface area [27], [28].
The MOF system allows access to the open framework
structures with network topologies and connectivities
(Figure 4) and the possibility of generating unusual large
diameter channels and cavities that are not usually
observed in classical porous materials [29].
 Separation of Carbon Dioxide Using Selected Porous Materials: A Review
(a) (b)
Fig 4. Some of the MOFs used for CO2 separation. (a) MOF-5, (b)
MOF-177 [28].
One of the fascinating property of these MOFs is
their structural flexibility or breathing effect, which allow
them to reversibly modulate their pore size according to
the molecules adsorbed into the pores, including gases
and liquids, while maintaining their crystallinity and thus
their long range order [30]. This phenomenon occurs
primarily with porous solids containing a hybrid organic-
inorganic framework because of the interaction of guest
molecules with the host structure [31]. MIL-53 (Materials
of the Institute Lavoisier), a particular eye catching case,
has attracted a lot of attention due to its large flexibility
and the occurrence of double structural flexibility upon
adsorption of some gases (CO2, H2O, C2H6) [32], [30], but
not ( CH4) [33]. The structure of the MIL-53 contains
hydroxyl groups located at the metal-oxygen-metal links
(μ2-OH) [32]. Upon adsorption of CO2, the material
shows different adsorption mechanism from other MOF
family such as its isostructural vanadium analogue MIL-
47 (V) where the corner sharing μ2-OH groups of MIL-43
are replaced are replaced by μ2-oxo groups in MIL-47
[32].
Studies have shown that MOFs are suitable for high
pressure application requiring mild regeneration
temperature and show higher adsorption capacity as
compared to most common porous materials like zeolites
and activated carbons where high temperature is needed
for regeneration [44]. Llewellyn et al. [30] investigated
the adsorption of CO2 and CH4 on large pore MIL-100
(Cr) and MIL-101 (Cr) at low temperature (300 K) and
relatively high pressures (5 Mpa). In particular, they
reported a CO2 uptake of 40 mmol g-1 or 390 cm3 STP
cm-1 for MIL-101 which they claim to be the highest
amount recorded to date for any MOF at 5 Mpa.
Yazaydm et al. [26] showed that preadsorbing a small
amount of water can significantly increase the selectivity
of the material towards CO2.
Mesoporous Silica
The discovery of the M41S family of ordered
mesoporous silica by scientist at Mobil Oil have attracted
considerable attention with respect to understanding the
formation and synthesis mechanism of novel adsorbents
with tailor made properties [35]. The most common types
of mesoporous silica are MCM-41 [10] and SBA-15 [11].
Figure 5 shows the possible mechanistic pathways for the
43
formation of MCM-41. Unfortunately, pure silica surfaces
do not interact very strongly with CO2 because the
hydroxyl groups are not able to induce strong enough
interactions and further specific adsorption sites are
missing.
Fig 5. Schematic possible mechanictic pathways for the formation of
MCM-41: (1) liquid crystal phase initiated and (2) silicate anion initiated
[35].
Table 1 summarizes the adsorption characterisctic of
different adsorbents. The physicochemical properties of
the adsorbent influence the adsorption of CO2. As such, in
order to enhance the adsorption of the adsorbents, surface
modification is an interesting means to modify the surface
properties and to further increase the gas adsorption
interaction.
Tab. 1 Summary of the adsorption characteristic of adsorbents.
Adsorbent Adsorption characterisctics
Zeolites Depends on basicity and dielectric field
NaY, 13X,
ZSM-5 5A
Porous carbon Able to achieve up to 108 mg/g @ 21.5 oC
Hydrotalcites Suitable for high temperature
Al content, anion type, water content affect CO2
adsorption
Metal organic Adsorption uo to 40 mmol/g @ 5 MPs
framework (MOF)
Mesoporous silica Do not have enough interaction between CO2
and hydroxyl groups.
3. SURFACE MODIFICATION
A lot of research aiming at improving the adsorptive
properties of porous adsorbents by modifying their
surfaces which generally improves their basic character is
currently in progress with several promising results
published in literature. Such modifications include
exchange or substitution of cations within the material
framework, simple chemical treatment of the surface as
well as impregnation/functionalization of the pores. These
modifications usually results in a decrease in surface area
but with increase in capacity and as well as selectivity and
affinity towards the target gas (CO2).
Cationic Substitution in Zeolite
In zeolites, the cation distribution within the
framework is a function of not only the structural and
 Separation of Carbon Dioxide Using Selected Porous Materials: A Review
composition of the framework but also the cationic form
[36]. Investigation into the effect of cationic substitution
in zeolites on several gases including CO2, CH4 and N2
shows that isotherms for CO2 are more favorable than
CH4 and N2 [36], [37]. The preference for CO2 against
other gases is attributed, in addition to the kinetic
screening against methane and nitrogen molecules, to the
fact that carbon dioxide has stronger electrostatic
interaction with the extra framework cation than methane
and nitrogen. The cations introduced can thus neutralize
the acidity and improve the basicity of the framework
which is beneficial for the adsorption of acidic CO2 [36].
It has been shown that at 273 and 303 K and pressures
between 0 to 1 atm, the selectivity of CO2 over CH4 on
Naβ were 22.2-28.8, which is higher than that of Hβ 12.8-
17.8 confirming the strong electrostatic interaction
between CO2 and the extra framework Na+ ions in Naβ
[37]. Adsorption equilibria of N2 and CO2 on fully
exchanged potassium chabazite (KCHA), sodium
chabazite (NACHA) and lithium chabazite (LiCHA)
shows that CO2 is more strongly adsorbed gas than N2.
The loadings of N2 on LiCHA, NaCHA and KCHA were
1.53, 1.25 and 0.87 molecules uc-1 respectively, and 6.37,
5.85 and 4.77 molecules uc-1 for CO2, at 273 K and 103
kPa. These quantities show the high affinity for CO2 and
the effect of cation type on adsorption capacity at low
pressures, where molecule-cation interactions are
dominating.
Cationic Treatment of Hydrotalcite (HTlc)
Recently, the use of potassium promoted Htlcs in
high temperature pressure swing adsorption and CO2
sorbents in sorption enhanced reaction process (SERP)
for the production of high purity hydrogen has been
investigated with higher capacities obtained compared to
the bare HTlcs. Their sorption performances were greatly
enhanced in the presence of vapor [38]. Oliveira et al.
[39] impregnated some commercially supplied HTlcs
having different Mg/Al ratios with potassium (K) and
cesium (Cs). Investigations into the CO2 sorption capacity
of the modified and unmodified HTlcs at 676 K and 0.4
bar in the presence of steam shows that the modified
samples performed much better than the unmodified ones.
Potassium modified (MG30-K) sorbed 0.76 mol/Kg of
CO2, cesium modified (MG70-Cs) sorbed 0.41 Kg/mol,
while the unmodified showed almost the same capacity
(0.4 Kg/mol).
Chemical Modification of Porous Carbon
It has been shown that the adsorption properties of
carbon based sorbents can be improved by simple
chemical modification such as the introduction of
nitrogen functional groups into their structure as well as
introducing alkali metal or alkaline earth on the surface.
Such modification increases the basic character of the
material well as their affinity towards CO2 [40], [41].
Investigation on the effect of CO2 adsorption on
commercially activated carbon, modified with ammonia
44
gases at temperature range of 200-800 oC revealed an
increase in CO2 adsorption capacity from 7 wt.% for the
parent carbon to about 9.6 wt.% for the modified carbon
[40]. These results indicated that surface modification of
activated carbon with ammonia increases its affinity
towards CO2 and thus concluded that the affinity towards
CO2 depends not only on the amount of total nitrogen
incorporated but to specific nitrogen-functionalities.
Young et al. [41] showed that at higher temperatures (300
o
C), the adsorption capacity of carbon based adsorbents
can be improved by chemical modification using
magnesium oxide, making them suitable materials for
high temperature PSA application and SERP.
Functionalization Using Amine
Immobilization of amines onto the surface of porous
solid adsorbents with the aim of improving the adsorption
capacity and selectivity towards the target molecule (CO2)
is another strategy that has been applied to silica based
sorbents [42], zeolites [43], and MOFs, [44]. One
strategy to increase the CO2 adsorption capacity is to
attach amine functional groups (primary or secondary)
onto high surface area support. Immobilization can be
achieved by either grafting or impregnation method. A
high surface area will allow for the grafting of a large
number of active sites per gram of adsorbent, and the
nature of this grafting will determine the amount of CO2
adsorbed and the energy required for regeneration. In
MOFs, functionalization of the pores is achieved by the
use of linker bearing the desired constituent [44] such as
2-aminoterephthalic acid, 1,4-benzenecarboxylic acid and
1,4-dicarboxylic-2amino-benzene [29],[45]. Two
approaches have been reported for introducing amine
functionalities into the pores MOFs by either introducing
prior to synthesis, an organic functional group directly by
replacement of a proton of the aromatic ring by amine to
produce an MOF with functionality within its framework
or post synthesis grafting of amino groups on the
accessible Lewis acid sites [44].
4.0 CYCLIC ADSORPTION PROCESS
Studies on CO2 capture using PSA, VSA and TSA
can be found in literature with different ranges of
temperature, pressure, design, cycles and other operating
parameters [46], [47]. Gomez et al. [48] carried out both
simulation and experimental investigation to determine
the optimal conditions for obtaining high purity product
from a flue gas stream comprising CO2 and N2 in the
presence of inerts using zeolite 13X. They showed that
increasing the feed flow rate resulted in decrease in the
purity of N2 in the product stream, while the product
recovery increases slightly. Increasing the cycle time
resulted in an increase in purity but with slight decrease in
recovery. Further, an optimum cycle time is obtainable at
about 30 s. They showed that an increase in the inert
component results in the decrease in product purity. Since
inerts dilute the mixture, it is expected that an increase in
 Separation of Carbon Dioxide Using Selected Porous Materials: A Review
inerts that is not adsorbed or weakly adsorbed, would
result in a decrease in product purity.
In order to minimize the bed size and maximize the
utilization of sorbents, layered beds containing different
sorbents are increasingly being used for multicomponent
separation in cyclic adsorption process [49]. The concept
involves the use of an initial layer of a weakly adsorbing
sorbent which is followed by a strongly adsorbing sorbent
having a smaller working capacity thereby minimizing the
use of each sorbent and hence the size of the adsorber
[49]. However, the advantages of using a single layer
include lower maintenance cost, no requirement of
screens to prevent adsorbents from admixture and overall
lower vessel cost.
5. CONCLUSION
From the literature, potential adsorbents having large
capacity to for CO2 capture and storage, their surface
modification to further improve on their performance
were discussed. Capacity and selectivity values reported
in literature were obtained from pure components. In the
industrial practice, the gas feed to be separated will also
contain several impurities. Although, the presences of
small amount of water have already been shown to
enhance their capacity for CO2, the presence of other
impurities (SOx and NOx) may further reduce the
adsorption capacity and may even result in a gradual
degradation of the adsorbent. Therefore, for practical
application, it is necessary to design adsorbents that will
simultaneously adsorb these impurities without adversely
affecting the capacity of the adsorbent material and the
overall performance of the system.
ACKNOWLEDGMENT
The authors acknowledge the financial support
from Fundamental Research Grant Scheme and
Universiti Teknologi Malaysia, Skudai, Johor
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