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Journal of CO2 Utilization 13 (2016) 1–16

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Journal of CO2 Utilization


journal homepage: www.elsevier.com/locate/jcou

Review article

An overview of activated carbons utilization for the post-combustion


carbon dioxide capture
Nor Adilla Rashidi, Suzana Yusup*
Biomass Processing Laboratory, Centre of Biofuel and Biochemical Research, Chemical Engineering Department, Universiti Teknologi PETRONAS, Bandar Seri
Iskandar, 32610 Tronoh, Perak, Malaysia

A R T I C L E I N F O A B S T R A C T

Article history: The increase of carbon dioxide (CO2) concentration in the ambient air has become the key factor in the
Received 10 August 2015 pace of temperature rise, and accordingly, is a primary contributor towards global warming scenario. In
Received in revised form 20 October 2015 view of this, the quick mitigation efforts associated with capturing CO2 from fossil fuel combustion
Accepted 9 November 2015
source must be implemented to alleviate environmental catastrophic events in future. Therefore, the
Available online 28 November 2015
purpose of this paper was to review the role and performances of activated carbon in capturing
anthropogenic CO2 flue gas prior to emission to air. Throughout this paper, the activated carbons which
Keywords:
were proposed to be a separation medium for CO2 capture are evaluated in terms of equilibrium
Activated carbon
Adsorption
adsorption capacity as well as the surface modification. The utilization of the activated carbons instead of
CO2 removal current state-of-art technology, which is the chemical absorption is promising as it avoids higher energy
Greenhouse gases penalty encountered in regeneration process and the consumption of corrosive chemical such as aqueous
amine-based solvent. In addition, the investigation on the potential of activated carbons for post-
combustion CO2 capture is expected to confer scientists with critical information related to the future
direction of the activated carbons in an industrial application, and as an alternative to conventional
amine scrubbing process.
ã 2015 Elsevier Ltd. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
2. Potential of activated carbons as CO2 separators . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.1. Physically-activated carbons for CO2 capture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.2. Chemically-activated carbons for CO2 capture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.3. General discussions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
3. Surface modifications of activated carbons for CO2 capture . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
3.1. Nitrogen-modified activated carbons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.2. Metal oxides-modified activated carbons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
4. Way forwards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
5. Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Acknowledgement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13

1. Introduction

The increasing of carbon dioxide (CO2) concentration in the


atmosphere is viewed as a serious problem to all people around the
world. In 2014, the CO2 concentrations in ambient air approached
* Corresponding author. Fax: +60 5 368 8205. 400 part per million (ppm) and it increased by 120 ppm from the
E-mail address: drsuzana_yusuf@petronas.com.my (S. Yusup). CO2 concentrations in the pre-industrial time [1]. With regard to

http://dx.doi.org/10.1016/j.jcou.2015.11.002
2212-9820/ ã 2015 Elsevier Ltd. All rights reserved.
2 N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16

this continual increased of CO2 emission from fossil fuels such as amine-functional group, CO2 absorption will take place through a
oil, coal, and natural gas combustions that cater diverse purposes chemical reaction mechanism, owing to acid-base ionic species in
such as electricity generation, transportation, and industrial sector, the solution [17]. Upon equilibrium, a rich-CO2 solution will be
deteriorations of both environmental and ecosystem conditions regenerated in a stripper column at high temperature around 100–
are likely to happen. In addition, with the never-ending emission of 140  C, in order to release the bonded CO2 molecules from the
CO2 gas to the surrounding, the Kyoto Protocol had been enforced absorbent [14,15,18]. Whilst purified CO2 is compressed and
in 2005 in which its core objective is to reduce the greenhouse gas sequestered, the regenerated amine-based solvent will be cooled
concentrations primarily CO2, methane (CH4), and nitrous oxide and recycled to the absorption column [16,18]. The schematic
(NOx) in the atmosphere to a minimum level, by which diagram of the amine scrubbing process is illustrated in Fig. 2.
catastrophic impacts towards the ecosystem can be evaded. In Despite the good performance of absorption technology in
line with this policy, it has been reported that the CO2 emissions capturing CO2 which can be up to 98% efficiency [20], heavy
from industrialized countries must be reduced to lesser than 6% by consumption of amine-based solvent contributes towards equip-
2012 [2]. With regard to this, Malaysia affirms to take appropriate ment corrosion, and hence, requires special materials for
initiatives to decrease the level of CO2 concentrations by 40% in equipment construction which can withstand corrosivity of these
2020, with respect to its concentration level in 2005. In order to chemicals [21,22]. Moreover, the corrosivity and generation of
realize the vision, proper mitigation techniques must be chemically-unstable compounds during the heating process are
addressed. In Malaysia, power plant sector has released significant difficult to handle than solid adsorbents [20]. In addition, a higher
amount of CO2 pollutants, and in 2010, the total CO2 emission from energy input is imposed during solvent regeneration process due
this sector almost reached 47.63 million tons, and thus accounted to stronger chemical interaction between CO2 and basic amine
for 52.29% of the total CO2 emission [3]. Since electricity generation solvent [22,23]. Yu et al. [24] reported that the total energy
is the prevailing contributor of CO2 emission in Malaysia, the CO2 consumption for solvent regeneration has accounted for 60% of the
capture should be implemented starting from this source. The total energy consumption. Besides, it is reported that heat input to
present technology for CO2 capture which is broadly adopted in the remove one ton CO2 consumes about 2.5 to 3.6 GJ [16]. Further-
industry nowadays is the post-combustion system, whereby the more, with regards to high volatility of these amine compounds,
flue gas separation takes place after the combustion process of there is a possibility that a minor portion of these chemicals will be
fossil fuel. The benefits of this process include ease in retrofitting evaporated and released to ambient along with cleaner flue gas,
the existing power plants and flexibility of the process, whereby and accordingly impacts the ecosystem. Moreover, another
the power plant is still capable to operate even if there are concern in utilizing the chemical absorption process is due to
malfunctions in the capturing system [4]. The conditions of flue gas amine degradation, either through oxidative degradation or
streams from the coal and natural gas combustion are summarized thermal degradation. The oxidative degradation causes the amine
in Table 1, and the simplified diagram of the post-combustion compounds to fragment into toxic derivatives such as organic acid,
carbon capture is shown in Fig. 1. In post-combustion CO2 capture, ammonia, and amide, whilst the thermal degradation that usually
the temperature of the flue gases will cool down and the gas takes place in a stripping column tends to produce large molecular
streams will undergo a pre-treatment scheme prior to capturing weight of the amine-chain products. The potential of the amine
system. The purpose of pre-treatment system or known as gas compounds to degrade and accumulate in solvent phase will result
cleaning is mostly to reduce the concentration of impurities in the in poor CO2 absorption capacity and kinetic rate, and thus
flue gas such as nitrogen oxide, sulphur oxide, water vapour, and necessitates a frequent injection of fresh absorbent and contrib-
particulate matter [5]. In addition, Chen et al. [6] reported that utes to higher operating cost [19].
typical temperature for the flue gas in post-combustion system is Due to the shortcomings of conventional amine scrubbing
between 50 and 150  C. process in CO2 removal from flue gas, solid adsorption process is
By far, chemical absorption with amine-based or ammonia- proposed as an alternative to the current technology. The
based absorbent receives the greatest attention due to its high adsorption scheme is said to offer miscellaneous advantages
process efficiency, and thus, is widely performed by industrialists. including high adsorption capacity at ambient conditions, low
This process that commonly utilizes alkanolamine-functional regeneration cost, long-term stability, fast kinetics, evading in
groups such as monoethanolamine (MEA) will react with CO2 moisture removal from flue gas, and ease in terms of handling [25–
from the flue gas in an absorber column at temperature between 27]. In addition, adsorption system is attractive since it can reduce
40 and 60  C and at ambient pressure [14,15]. During this stage, flue the total energy consumption in regeneration process, owing to
gas is introduced at the bottom part of the absorber unit whilst 20– lower heat capacity of adsorbent as compared to water, as well as
30% MEA solution is added from the top [16]. By utilizing the skipping the water evaporation stage [28]. This technology
involves two stages which are CO2 adsorption onto the material
surfaces in an adsorption column via physical (physisorption) or
Table 1
Summary of flue gas conditions in post-combustion technology [10–13].
chemical (chemisorption) bonding. Upon equilibrium, solid
adsorbents will be regenerated through a pressure swing (PSA)
Components Coal-fired flue gasa Natural gas-fired flue gas or thermal swing (TSA) process, so that the adsorbed CO2
N2 (vol%) 70–80 73–80 molecules can be discharged from the carbon surfaces and the
CO2 (vol%) 11–15 3–8 adsorbents can be reused for the next adsorption cycle [23,29]. In
H2O (vol%) 5–12 7–14.6
TSA system, regeneration process is performed by increasing the
O2 (vol%) 3–6 4.45–15
SO2 (ppm) 200–4000 <10 operating temperature, whilst PSA is a process where the CO2
SO3 (ppm) 0–20 – molecule is desorbed from carbon surface upon pressure reduction
NOx (ppm) 200–800 50–70 [30]. The flow diagram of the adsorption process for CO2 removal
CO (ppm) 50–<100 5–300
from flue gas is shown in Fig. 3.
Hg/As (ppb) 1–7 –
Particulate matters (g/m3) 5–20 –
In considering the adsorption technology as an alternative to
Pressure (bar) 1 1 amine scrubbing process, there are a few guidelines that must be
CO2 partial pressure (bar) 0.12–0.15 0.05–0.1 abided by researchers so that effectual separation process is
a attained. Accordingly, the selection of adsorbent should satisfy the
Before flue gas treatment—FGD and deNOx.
following features which include high adsorption capacity, high
N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16 3

Fig. 1. Simplified block diagram of post-combustion CO2 capture [5,7–9].

Fig. 2. Schematic diagram of amine scrubbing process; reprinted with permission from [19], Copyright 2015 American Chemical Society.

CO2/N2 selectivity, high surface area, fast kinetic, mild desorption physisorbent materials such as the activated carbon and zeolites
conditions, good tolerant towards moistures and impurities, high is attractive since they are safe for local environmental and
in mechanical strength, stable in multi-cycle adsorption and relatively inexpensive to the manufacturers [35]. Comparing these
minimal in operational cost [5,31]. In post-combustion capture, two adsorbents, the activated carbon is deemed as a superior
since the operating temperatures are low, appropriate solid adsorbent for CO2 separation from flue gas stream, due to its
adsorbents that can be applied are usually limited to activated hydrophobicity properties that will prevent an additional step for
carbon and zeolites, as both of these adsorbents belong to lower- moisture removal prior to CO2 adsorption. Ling et al. [32] reported
temperature adsorption application, aside from their extensive that performance of Zeolites 13X in capturing CO2 is reduced in
usage in industrial processes [32–34]. Besides, utilizing presence of water vapour, due to potential of water vapour
4 N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16

Therefore, the purpose of this review paper is to discuss and


revise the recent performance of the activated carbons in CO2
removal (2011-present), with respect to adsorption capacity and
surface modification. Thereby, a great understanding and knowl-
edge related to CO2 adsorption process with the activated carbon as
separation medium is valuable for the up-scaling process and for
implementation in actual industrial applications.

2. Potential of activated carbons as CO2 separators

The activated carbons have been widely acknowledged as


promising adsorbents in capturing CO2 in post-combustion
conditions, which is at atmospheric pressure and moderate
temperatures. In producing activated carbons, any carbonaceous
materials can be converted to activated carbons as long as they
possess high carbon content and low in ash, significant volatiles
matter as evolution of volatiles during thermal heating will assist
in creating the pore formation, and originated from non-expensive
resources must be taken into consideration [41–43]. Besides, raw
precursors must be easily activated, and to have a lower
degradation rate in order to preserve their physiochemical
characteristics [44]. Therefore, selection of appropriate raw
materials prior to the activated carbon production is crucial since
composition of the material structure such as carbon, nitrogen,
oxygen, hydrogen, and sulphur will influence the physiochemical
properties of the synthesized activated carbons. Recently in 2013,
Rashidi et al. [45] showed that types of raw precursors are amongst
the significant variables towards CO2 adsorptive properties of
activated carbons, through the analysis of signal-to-noise ratio. In
addition, origins of these precursors play a substantial role in
properties of the carbon products. Olivares-Marín et al. [46] who
studied the influence of different origins of carpet wastes (pre- and
post-consumer) as the precursors proved that these wastes are
varied in terms of chemical compositions, and hence will affect the
properties of the synthesized activated carbons. The presence of
high volatile matters in pre-consumer waste was observed to form
lower carbon yields (13.31 wt%), compared to post-consumer
waste that is notably higher in inorganic material. The lower yield
was expected for pre-consumer waste, as it has significant
amounts of volatiles (81.33–99.60 wt%), and upon thermal
carbonization process at 450  C, these volatiles will be released
as gas compounds, and thus yield lower products. Moreover, it has
been reported that during devolatilization stage, both mass loss
and shrinkage of precursors occur due to the release of moisture
contents through convection and diffusion, and causes rearrange-
Fig. 3. Process flow diagram of CO2 adsorption; Reproduced with permission from ment of the material structures [47,48]. Meanwhile, high produc-
[5], Copyright 2013 Elsevier.
tion yield of post-consumer waste that ranges between 49 and
52 wt% is attributed to their high incombustible ash content.
adsorption onto the sodium cations in zeolites structures, and thus
Accordingly, the post-consumer waste obtained from street and
reduces the potential for CO2 sorption. With regard to this, flue gas
residential area has poor BET surface area which is between
should be in a dry state prior to adsorption by zeolites and the
326 and 466 m2/g and lower CO2 adsorption capacity than the pre-
drying cost can reach up to $10USD per ton of captured CO2 [36].
consumer waste, in which its surface area exceeds 1200 m2/g with
Meanwhile, the activated carbons are excellent as they own
predominant micropores and CO2 adsorption capacity of 13.8 wt%
valuable properties such as superior CO2 adsorption capacity,
[46]. Apart from the nature of precursors, operating conditions for
reversibility and stable in adsorption–desorption cycles, high
the activated carbon production are crucial in developing suitable
resistivity to alkaline and acidic conditions, good porosity network
activated carbon for gas phase application. There are two types of
that assist in adsorption process and gas diffusion into interior side
activation, which are physical and chemical activation which will
of activated carbon, ease in modification in terms of surface
be described in the following sub-section.
chemistry and physiochemical characteristics via pre- or post-
modification method, aside from their low cost [37–39]. Being a
2.1. Physically-activated carbons for CO2 capture
physisorbent material, the activated carbon has relatively lower
heat of adsorption than zeolites, and subsequently the regenera-
The activated carbon produced via physical activation is
tion step can be performed without imposing higher energy
manufactured through two separate stages, which are carboniza-
penalty [38,40]. It is reported that the heat of CO2 adsorption of the
tion under inert environment (pyrolysis) and followed by
activated carbon at 25  C and 1 bar is 3 kJ/mole while zeolites are
activation process in the presence of oxidants such as air, CO2,
10 times higher, which is about 30 kJ/mole [15].
and steam [49–53]. In conventional physical activation, an initial
N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16 5

stage which is material carbonization under inert gas such as needs to acquire additional steam generator as well as a metering
nitrogen (N2) is intended to eliminate both volatile matters and pump, as is needed in the steam activation process [67].
impurities, and to yield carbon-enriched samples (char). The Nevertheless, conventional physical activation that undergoes
carbonization process often occurs at temperature below 800  C, twofold stages has its limitations which are higher energy penalty
which is considered sufficient for a complete devolatilization due to dual thermal-cooling routes and longer time to complete
process, and to hold at the specified desired temperature for a the process [68]. In addition, the elevated temperature for the
certain period of time and is subsequently cooled to ambient. activation process that can reach up to 1000  C is inappropriate
Afterwards, the produced char will undergo activation process in since it leads to reduction in the carbon yield, and thus, do not meet
presence of oxidizing gas at temperature between 800 and 1000  C the industrial specifications which should be within 20–40 wt%
[49,51,52]. The previous work that focuses on the physically- [68]. Therefore, in order to circumvent the appalling circum-
activated carbons for CO2 capture at 1 bar is tabulated in Table 2. stances, alternatives to the current practice of physical activation
Based on recent publications regarding the physically-activated should be established. In 2014, Rashidi et al. [54,69,70] showed
carbons for CO2 capture (2011 to present), it shows that extensive that single-step CO2 activation with an absence in preliminary
work has been performed using CO2 activation, either by single- or carbonization step is able to circumvent the existing drawback of
dual-stage activation technique. The endothermic reactions longer operational hours, and minimize gas and energy consump-
between carbonaceous materials and oxidizing gases are simpli- tion. Besides, the synthesized activated carbons obtained from this
fied in Eqs. (1)–(2) [60,61]. single activation route is competent in adsorbing substantial
amounts of CO2 (1.79 mmol/g) [54]. In the single activation
C þ CO2 ! 2CO DH ¼ þ 173kJ=mole ð1Þ
method, CO2 oxidants serve dual functions, which is as a purging
gas to flush out moisture and volatiles that are released during the
thermal process, and to allow the chemical reaction with carbon to
C þ H2 O ! CO þ H2 DH ¼ þ 132 kJ=mole ð2Þ form porosity [69]. From industrial perspective, the one-stage
The selection of CO2 as activation agent instead of steam is due to physical activation in producing the activated carbons is the
its potential to form narrow micropores which suits the CO2 simplest and cheapest method and able to circumvent the
adsorption, whereas steam is prone to mesopores formation upon limitations of current state-of-art physical activation [70].
the activation process [61,62]. The difference in pore structures of Similarly, single-stage CO2 activation had been performed by
the activated carbon is related to high reactivity of steam, and González et al. [55] with olive stone and almond shell as the
accordingly, the activation process using steam as an activating starting materials. They agreed that single-step physical activation
agent can be performed at low temperature and operational time with the absence of carbonization step will minimize both the
[63,64]. Besides, steam that has high reactivity rate is explained by operation and installation cost, aside from excellent surface areas
its lower molecular size as compared to CO2 molecule, in which it and pore characteristics [55].
permits faster diffusion to pore network and access to micropores Plaza et al. [60] have applied the single-stage technology for the
(width d < 2 nm) that leads to micropores widening to mesopores production of activated carbons, but with diluted oxygen (3-21%
(2 nm < d < 50 nm) and macropores (d > 50 nm) [65]. Hence, for gas O2, balanced with N2) as the activation agent. The utilization of O2
adsorption, CO2 activation is suitable as it tends to formulate as oxidizer is considered inexpensive, since O2 gas is readily
microporous activated carbon that highly suits the adsorption available and can be obtained from air or flue gas that has excess O2
process of small CO2 molecules. Besides, Wei et al. [66] proved the gas which is not consumed in the combustion process [60,71].
significances of narrower micropores (d  0.55 nm) for the CO2 Nevertheless, owing to exothermic reaction between O2 and
adsorption at lower pressure, since the pore sizes offer ample carbon material as shown in Eq. (3)–(4), the activation process
spaces for CO2 molecules to adjust themselves in the pore walls. using O2 gas is difficult to control due to its higher reactivity, and
Moreover, CO2 activation is considered inexpensive and simple, as thus, justifies the limited research work on O2 activation in
the CO2 flow can be easily regulated from gas cylinder without the literatures [60,71]. Moreover, due to excessive combustion in O2

Table 2
Recent physically-activated carbon productions for purified CO2 capture at atmospheric pressure (year 2011–2015).

Precursors Carbonization process (under N2) Activation process Max. surface area Adsorption Ref.
(m2/g) capacity
(mmol/g)

Flow rate Temp. Holding time Types of Flow rate Temp. Heating rate Holding time 25  C 100  C
(mL/min) ( C) (min) oxidant (mL/min) ( C) ( C/min) (min)
Coconut – – – CO2 150 900 20 45 371 1.8 0.4 [54]
shell
Almond – – – CO2 100 750 10 240 862 2.7 0.9 [55]
shell
Olive stone – – – CO2 100 800 10 360 1215 3.1 0.8 [55]
Coconut – – – CO2 140 800  (N2) 210 1327 3.9 – [56]
shell
Coffee 50 600 n/a CO2 10 700 25 (N2) n/a 593 2.4 – [57]
residue
Nut shell 500 600 60 CO2 500 900 n/a 60 573 3.48 – [58]
Cotton n/a 600 n/a CO2 n/a 800 n/a n/a 610 2.30a 0.5b [59]
stalk
Almond – – – O2 (3%) 100 650 n/a 83 557 2.1 0.7 [60]
shell
Olive stone – – – O2 (3%) 100 650 n/a 110 697 2.0 0.6 [60]
a
At 20  C.
b
At 120  C.
6 N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16

atmosphere, burning process will not only occur in the internal 2.2. Chemically-activated carbons for CO2 capture
pore structures but towards the exterior particles as well.
Therefore, it leads to higher carbon burn-off and reduces the In contrast to physical activation, chemical activation involves
surface area [71,72]. To circumvent the limitations of O2 as the impregnation of raw precursors with a dehydrating agent prior to
activating agent, Plaza et al. [60] proposed to perform O2 activation carbonization/activation process. The dehydration agents that are
at low temperatures (preferably <650  C) and low operational usually used include alkaline, acidic, and salt mediums such as
times in order to avoid excessive combustion, and to use diluted O2 potassium hydroxide (KOH), sodium hydroxide (NaOH), zinc
and balanced inert N2 stream rather than using purified O2 gas. chloride (ZnCl2), phosphoric acid (H3PO4), etc. The recent work
Their findings showed that single O2 activation produced activated that utilizes the chemically-activated carbons for the CO2
carbon with maximum adsorption capacities of 2.09 and adsorption is presented in Table 3.
0.74 mmol/g at 25 and 100  C, respectively [60]. By comparing The extensive laboratory-scale studies in chemical activation
the CO2 adsorptive properties of dual-step activated carbon with for activated carbon production are triggered by the lower energy
single-step activated carbon, it shows that the latter activation consumption, as the activation temperature is between 600 and
method is promising as it produces activated carbon with 800  C, and shorter operational time that will contribute to high
comparable CO2 adsorption capacity, and hence signifies the carbon yield. Moreover, this chemical activation method is done in
effectiveness of the oxidants as a purging gas and a reactant to form a single stage, whereby both carbonization and activation process
porosity. are performed simultaneously with assistance of chemical
activator, which will generate porosity through dehydration and
C þ O2 ! CO2 DH ¼ 395kJ=mole ð3Þ
oxidation reactions [93–95]. Though, chemically-activated carbons
need to undergo an intense washing process in order to remove
residual chemicals and impurities from the carbon structures, and
1
C þ O2 ! CO DH ¼ 111 kJ=mole ð4Þ thus lead to secondary pollution problems, caused by the
2 corrosiveness of dehydrating chemical agents and inefficiency in
Besides, another drawback encountered while utilizing CO2 chemical recovery during the washing stage [96]. Besides, longer
from supplied gas tanks is related to an emission of excess CO2 gas operating time is anticipated to completely recover the activating
that does not take part in activation reaction to the atmosphere. chemicals from carbon structures. Though chemical activation is
Accordingly, Sulaiman et al. [73] proposed to utilize CO2 gases well-documented as a single-step process, there are numerous
emitted from calcination process of calcium carbonate (CaCO3), as studies of two-stage chemical activation in which the dehydrating
shown in Eq. (5) as the activator. In their work, CaCO3 and oil chemicals mix with synthesized char, instead of raw precursors as
palm shell are properly arranged in a tubular furnace in order in one-stage activation [94]. Cao et al. [97] reported that in some
to study a synergistic effect of the simultaneous calcination circumstances, mixing the activating agent with raw precursors is
and activation reactions. The variables of interest in this inadequate to develop activated carbon with high surface area, due
experimental work include the temperature (850–1000  C), to the difficulty in penetration of the activator towards interior
addition of CaCO3 (15–45 g), as well as operating time (0–10 h). structures. Meanwhile, in case of previously carbonized material
The findings showed that as the operating temperature increased, (char) that has some pores developed during carbonization
the time needed to achieve saturated CO2 emission from the process, well-developed porosity will be produced, as the pores
carbonate waste was shorter, whilst large amounts of carbonate in char structures permit easy diffusion for the activators to react
released more CO2 gas and thus, favour the subsequent activation with carbons and hence, generate abundant pores with high
stage. The produced activated carbon by CO2 activation obtained surface area [97]. Nevertheless, dual-stage chemical activation
from the emitted CO2 in calcination process is more economically process is considered akin to the conventional physical activation,
beneficial, as it involves minimal operating cost, aside from the and thus, cannot compensate the weaknesses of the physically
capability of these carbon materials in adsorbing CO2 up to technique which are higher energy and time consumption, along
0.713 mmol/g. with additional effluent treatment problems. In addition, El-
Hendawy et al. [98] agreed that one-stage activation scheme with
CaCO3 ! CO2 þ CaO ð5Þ
respect to thermal treatment is significant for the process to be cost
In addition, utilizing CO2 as an activation agent is favourable in effective.
producing the activated carbon intended for post-combustion Moreover, the chemical activation can be accomplished by
CO2 adsorption. This is due to the saturated activated carbons either solid–solid physical mixing or wet impregnation (soaking)
with CO2 during the adsorption step will need to undergo a process [99–102]. In physical mixing, dried solid activator in
regeneration process in order to release the adsorbed CO2 powder form is mixed with raw precursors or char based on the
molecule, and to tolerate multi-cycle use of carbon materials desired mass ratio at room temperature. Meanwhile, wet
rather than replacing with fresh adsorbent in each cycle. impregnation involves a mixing process between the solution of
Accordingly, the released CO2 gas in the regeneration process chemical agent and raw precursors/char at specified ratio and
can be stored, recycled, and reused for industrial activated carbon impregnation temperature. Upon completion of stirring, the
production via CO2 activation. produced slurry is dried prior to heat treatment under an inert
Nevertheless, the benefit of physical activation instead of atmosphere [100,101]. Yet, the drying step which is often at 110  C
chemical activation is correlated with high purity of the synthe- can be an additional parameter to be explored. Lillo-Ródenas et al.
sized carbon materials. Therefore, a washing stage after comple- [99] studied the influence of drying time upon completion of NaOH
tion of the activation process can be omitted. The high purity of the impregnation, from 0 h (wet sample) to 31 h. The result showed
end product is due to the absence of chemicals during the that an increment in drying time will produce activated carbon
preparation stage, and hence, it is considered as an environmental- with lower micropore volume, due to formation of alkaline
friendly approach. Owing to this advantage, physical activation is carbonates that may obstruct the performance of NaOH as the
said to be widely adopted in industries due to its process simplicity, activating agent. However, influence of the drying time after the
desirable physical characteristics, and well-developed micropores impregnation step is still scarce in the literature.
in the carbon structures [74]. Besides, solid–solid mixing is revealed to formulate activated
carbon with lower surface area and pore volume, compared to
N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16 7

synthesized activated carbons via pre-impregnation route. Chen (353 m2/g). The improvement in surface area and porosity for
et al. [102] explained that poor porosity development of material grinded activators is due to better surface contact between the
produced via physically-mix scheme is caused by difficulty of activators and carbonaceous precursors, which is favourable for
activators (in this case is K2CO3) to penetrate into the carbon pore development.
structures, and thus reduce the pore development. In contrast, wet Referring to the recent work on activated carbon production for
impregnation method is able to fabricate better activated carbon CO2 capture in Table 3, it shows the wider utilization of potassium
since K2CO3 can infiltrate into the carbon precursors, therefore, has hydroxide (KOH) as chemical agents. Cao et al. [97] explained that
high reaction degree to assist in pore expansion. However, various extensive utilization of KOH as activator is due to its lower energy
results on the methods of mixing the activators with carbonaceous requirement as compared to water vapour, aside from imposing
sample rely on the types of activating agent used in the process. An the least environmental impact when compared to other chemical
opposite finding was observed by Andrés et al. [92] who observed activators such as ZnCl2 and H3PO4. During KOH activation,
that solid–solid mixing with NaOH as activating agent produced intercalation of metallic potassium (K) into the carbon structures
better activated carbon with respect to CO2 adsorption capacity, will widen the space between the carbon atomic layers. Therefore,
which can reach up to 3.8 wt%, instead of 1.7 wt% which was the pore volumes of the synthesized activated carbon are enhanced
attained by the wet-impregnated sample. Therefore, a thorough [104,105]. Upon the washing process, the metallic potassium will
analysis on the effect of mixing method should be conducted, as be detached from the carbon matrix and leave a free interlayer
production of high quality activated carbon via solid–solid mixing space that contributes to porosity [106,107]. Being a strong base,
is preferred, since these carbon materials can be synthesized in Sudaryanto et al. [108] proposed that KOH can act as a catalyst to
shorter operational time and with lesser work than the impregna- promote the oxidation process, in which the carbons are oxidized
tion system. While considering physical mixing of activators with and to widen the pore width. Simultaneous and consecutive
precursors, size of activators should be considered as well. Ros et al. reactions that occur during KOH activation are divided into three
[103] proved that the size of activators has a considerable role in regions. The first region corresponds to the temperature range of
producing superior carbon materials, as mixing powdered NaOH 80–250  C and the possible mechanisms are stated in Eqs. (6)–(8).
with precursors will generate BET surface area of 689 m2/g, twice Between 250  C and 680  C, KOH activation proceed to the
than the surface area obtained for granular-sized activator formation of potassium carbonates (K2CO3) as shown in Eq. (9).

Table 3
Recent chemically-synthesized activated carbon productions in 2011-2015 for CO2 capture at atmospheric pressures.

Precursor Process Carbonization Activation process Max. surface Adsorption capacity Ref.
step area (m2/g) (mmol/g)

Temp. ( C) Time Activator IRa (wt/ Temp. Heating rate Time Flow rate 0  C 25  C 50  C 75  C
(h) wt) ( C) ( C/min) (hr) (mL/min)
Wood 1 – – H3PO4 2:1 450 4 1 n/a 1889 – 2.9b – – [75]
Palm stone 1 – – H3PO4 2:1c 450 1 2 80 1320 3.1 – – – [76]
(48%)
Palm stone 1 – – ZnCl2 2:1c 500 1 2 80 924 2.7 – – – [76]
(48%)
Rice husk 1 – – ZnCl2 1:1 500 10 1 100 927 – 1.3b – 0.5 [77]
Bagasse 1 – – ZnCl2 1:1 500 10 1 100 923 – 1.7b – 0.6 [77]
Fly ash 1 – – KOH 5:1 700 5 2 n/a 161 – 0.6 – – [78]
Sawdust 1 – – KOH 4:1 700 5 1 n/a 1643 8.0 4.8 – – [79]
Yeast 1 – – KOH 1:1 600 n/a 1 50 1348 – 4.8 – – [80]
Peanut 2 500 1.5 KOH 1:1 700 5 1.5 120 956 5.2 4.0 – – [39]
shell
Sunflower 2 500 1.5 KOH 1.25:1 700 5 1.5 120 1790 7.1 4.6 – – [39]
seed
Coffee 2 400 n/a KOH 1:1 600 5 1 300 831 4.9 2.8 – – [57]
ground
Bamboo 2 500 1.5 KOH 3:1 600 10 1.5 n/a 1846 7.0 4.5 – – [66]
EFB 2 250 0.33 KOH 5:1 800 2 n/a n/a 2510 5.2 3.7 2.3 – [81]
Fungi 2 500 2 KOH 0.5:1 n/a 3 1 n/a 1479 5.5 3.4 – – [82]
Algae 2 200 24 KOH 2:1 700 n/a n/a n/a 1940 7.4 4.5 2.8 – [83]
Starch 2 230–250 2 KOH 4:1 700 3 1 n/a 2190 5.6 3.5 2.2 – [84]
Cellulose 2 230–250 2 KOH 4:1 700 3 1 n/a 2370 5.8 3.5 1.8 – [84]
Sawdust 2 230–250 2 KOH 2:1 600 3 1 n/a 1260 6.1 4.8 3.6 – [84]
Palm shell 2 600 1 KOH 3:1 850 10 1 n/a 1250 6.3 4.4 – – [85]
Pitch 2 420 3 KOH 1:1 800 5 2 100 1770 – 3.8 – – [86]
Bean dreg 2 400 1 KOH 1:2 700 5 1 40 1060 – 4.2 – 1.8 [87]
Celtuce 2 600 n/a KOH 4:1 800 n/a 1 n/a 3404 6.0 4.4 – – [88]
leaf
Pine 2 500 1.5 KOH 2:1 700 n/a 1.5 n/a 1486 7.7 5.0 – – [89]
nutshell
Algae 2 180 24 KOH n/a 600 2 4 n/a 418 2.4 1.4 0.4 0.2 [90]
Poly- 2 400 2 KOH 3:1 550 n/a n/a n/a 1965 6.0 – – – [91]
aniline
Poly- 2 400 2 K2CO3 3:1 650 n/a n/a n/a 1695 7.6 – – – [91]
aniline
Sludge 2 800 n/a NaOH n/a 700 5 1 100 179 – 1.3 – – [92]
(solid)
a
IR = Impregnation ratio (activator to precursors/char.
b
CO2 adsorption at 30  C.
c
Unit of IR is vol. activator/wt precursors.
8 N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16

The final region which is at temperature >700  C is related to the adsorption at 1 bar. Despite having the highest surface area of
reduction of K2O by carbon or H2 to form the metallic potassium, as sample C600K5, its CO2 uptake (4.2 mmol/g) was lower than the
denoted by Eqs. (10)–(12) [78,81,109]. Wang et al. [82] proposed corresponding uptake by sample C600K3 (4.4 mmol/g), in which
that the development of greater microporosity and surface area in the surface area was 1250 m2/g and the volume of ultra-micro-
this KOH activation is attributed to the collaborative effects of pores was 0.29 cm3/g. In comparison, the sample C600K5 has
chemical activation that entails redox reaction of KOH to surface area and ultra-micropores volume of 1890 m2/g and
carbonate, in-situ physical activation that involves carbon gasifi- 0.28 cm3/g, respectively. Likewise, Zhu et al. [79] reported similar
cation with CO2, and expansion of carbon lattices due to findings whereby an activated sawdust that has the greatest
intercalation of the potassium compound. surface area of 2435 m2/g was incompetent in adsorbing large
amount of CO2 molecules, due to lower micropores volumes that
2KOH ! K2 O þ H2 O ð6Þ
only constitute 29% of the total pore volumes. On the other hand,
activated sawdust that has CO2 adsorption capacity of 8 mmol/g
has 73% of micropores volumes, despite its low surface area of
C þ H2 O ! CO þ H2 ð7Þ
1643 m2/g. Hence, it concludes that the fraction of micropores
volume in the activated carbon structures is a primary contributor
towards CO2 adsorption.
CO þ H2 O ! CO2 þ H2 ð8Þ
Referring to Tables 2 and 3, the CO2 adsorption capacity of
activated carbons is shown to reduce at elevated temperatures.
Thereby, it proves that CO2 adsorption of activated carbons is an
K2 O þ CO2 ! K2 CO3 ð9Þ
exothermic and a physisorption reaction which favours low
temperature. The reduction in the amount of CO2 adsorbed at
elevated temperatures is elucidated in terms of high mobility of
K2 CO3 ! K2 O þ CO2 ð10Þ
CO2 molecule at high temperature. At elevated temperature, high
surface adsorption energy and molecular diffusion rate results in
instability of the adsorbed CO2 molecules [114]. Accordingly,
K2 O þ H2 ! 2K þ H2 O ð11Þ
desorption of CO2 adsorbates will take place. Nevertheless, the
actual temperature of flue gas streams in post-combustion
technology is often up to 150  C. Hence, an extensive work which
K2 O þ C ! 2K þCO ð12Þ
focuses on CO2 adsorption at 0  C does not reflect the real condition
of flue gas stream in power plant. In addition, applicability of the
2.3. General discussions activated carbons in capturing CO2 at higher temperatures can
reduce the operational cost in cooling the flue gas to lower
In adsorbing CO2 from the flue gas, there will be a presence of temperature, and makes the process more economical and feasible
water vapour as well [110]. This water vapour will surround the [115]. Therefore, it demands the development of activated carbons
outer surface of activated carbons and forming an external fluid that can well operate at high temperatures. In view of this, surface
film, in which the mass transfer will take place via molecular modification of the activated carbons must be explored for the
diffusion (external resistance) [110]. Following the external fluid practical applications of CO2 separation from flue gases.
film resistance, an internal mass transfer proceeds through the In post-combustion technology, the flue gas is considered as
macro- and micropores inter-connected network (intra-particle CO2/N2 binary mixture due to the lower composition of the other
diffusion) in the activated carbon, where the CO2 molecules are impurities. Consequently, the challenge in this post-combustion
mostly adsorbed [111]. The microporous activated carbon contains CO2 capture is related to its lower CO2/N2 selectivity, which is
micro-particles of various shapes such as slab, cylinder, and sphere within the range of 2–15 [4,6]. Moreover, Cheung and Hedin [116]
[112]. Besides, in the gas phase adsorption, macropore adsorption reported that the kinetic dimension of CO2 and N2 in gas phase is
can be neglected whilst microporosity diffusion is dominant. It has 0.51 nm and 0.43 nm, respectively. The closer dimension of these
been reported that when the diameter of pore and adsorbates are gases contributes to lower selectivity since they will compete for
comparable, the adsorbates will never escape the adsorbent the adsorption site on the material surfaces. High selectivity of the
surface and to jump between the adsorption sites (surface activated carbon is a good indicator of the materials' effectiveness
diffusion) [13].Realizing the significance of pore engineering for in separating CO2 from the gas mixtures, as it indicates that these
CO2 uptake, pore size and pore volume of the activated carbons active materials are only preferable for CO2 adsorption. One of the
must be taken into consideration. In CO2 capture at an atmospheric techniques in improving CO2/N2 selectivity can be achieved by
condition, narrower micropores with pore sizes of <1 nm are increasing basicity of the carbon material, in which it will promote
favourable since they assist in the retention of CO2 into the pore the CO2 uptake via acid-base interaction. Besides, it is reported that
wall [6,57,83,84]. Besides, pore size of <1 nm is expected to block an incorporation of Lewis base (electron donor) onto the surface of
the N2 passage onto the pore walls [113]. However, a pore with activated carbon is promising, as it accelerates the interaction
small width shows inefficiency of CO2 uptake as it is closer to between adsorbent and CO2 which is referred as a weak Lewis acid
kinetic dimension of CO2 that is around 0.33 nm. Therefore, the (electron acceptor) [117,118]. Therefore, recent works on the
lower limit of micropore size is fixed at 0.33 nm [39]. Meanwhile, surface modification of activated carbons will be thoroughly
pore size >1 nm is not preferable for CO2 adsorption at 1 bar, since a discussed in the following section.
dense pack of the CO2 molecules may not be attained [66]. Thereby,
appropriate operating carbonization-activation conditions in 3. Surface modifications of activated carbons for CO2 capture
synthesizing active carbon should be explored in order to obtain
microporous carbon material. Moreover, high micropores volume By far, many investigations related to the utilization of
is desired as it specifies more availability of adsorption sites for the carbonaceous-based material in capturing CO2 have been carried
CO2 uptake to occur. Accordingly, Ello et al. [85] demonstrated the out. Nevertheless, in ensuring a specific interaction between the
implications of having high ultra-micropores volume for CO2 activated carbon and CO2 in flue gas mixture, the surface chemistry
of the adsorbent particle must be taken into consideration. The
N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16 9

surface chemistry of the activated carbon is governed by the absorption, with added advantages of minimal energy requirement
heteroatoms such as oxygen and nitrogen, controlled by the nature for regeneration, avoidance of corrosion problem, and ease in
of raw precursors as well as the activation conditions [119]. handling [133,134]. Due to these advantages, wet impregnation
However, the surface chemistry of the pristine activated carbons method of the amine compounds onto activated carbon is
which can be in form of neutral, acid, and alkaline is not vigorous to extensively practised. This technique involves mixing the aqueous
enhance the specific adsorbent-adsorbates interactions predomi- amine solution and activated carbons at specified temperature,
nantly at elevated temperature, and to selectively adsorb the CO2 time, and stirring condition, and the solvent will be removed via
molecules than the other gas pollutants. Chingombe et al. [120] filtration or evaporation [135]. Houshmand et al. [125] stated that
reported that these functional-groups on the carbon structure can in impregnation process, the amine compounds are well-dispersed
be manipulated either by thermal or chemical treatment in order into the pores, internal and external surface of the activated
to produce the adsorbents that serve specific applications. carbon, and physically adsorbed via dipole–dipole interaction, van
Therefore, surface modification of these carbon-based adsorbents der Waals force, hydrogen bonding, acid-base interaction, or ion-
must be thoroughly studied to promote their affinity and exchange mechanism. Meanwhile, the CO2 adsorption onto amine-
selectivity towards the CO2 molecule. Generally, the surface modified activated carbon is through multiple mechanisms which
modification step is performed after the activation process, and involve pore diffusion, chemical bonding, simultaneous physi-
the modification technique can be classified into three categories sorption, and chemisorption process [136].
which are physical (heat treatment), chemical (acidic, basic, Nevertheless, the performance of the impregnated activated
impregnation), and biological modification [121]. Since the CO2 carbons in CO2 capture is noticeable at elevated temperature, since
molecule are categorized as a Lewis acid, affinity of activated these amine groups tend to block the porosity in the microporous
carbon towards CO2 gas can be carried out according to the activated carbon. Consequently, it contributes to lower surface area
chemical treatment, by increasing their basicity properties and micropore volume that is responsible for CO2 capture at
through neutralization of acidic functional group, or to replace ambient temperature [133]. The pore blockage by the amine-based
acidic group to basic functionalities [122]. Besides, Sun et al. [123] compounds has been examined by the field emission scanning
reported that the chemistry of the activated carbons can be altered surface morphology (FESEM) analysis, as is presented in Fig. 4
by introducing basic groups such as sulphur, nitrogen, and metallic [131]. In the pristine activated carbon, pores and cavities on the
atoms. carbon surface can be clearly seen whereas for the amine-modified
activated carbon, no pores can be observed. In the modified
3.1. Nitrogen-modified activated carbons adsorbent, the distribution of the 2-amino-2-methyl-1-propanol

The nitrogen modified activated carbon which is usually


synthesized via post-treatment method, is conducted through
heat treatment with ammonia (NH3) or an impregnation process
with amine functional groups [124,125]. The thermal treatment
with NH3 gases or known as an amination process involves heating
the pristine activated carbons to elevated temperatures (200–
1000  C) in NH3 atmosphere for a certain period of time, prior to
cooling to ambient temperature under inert N2 flow [115,124,126].
During the heating process, NH3 decomposes into free radicals
such as NH2, NH, atomic hydrogen, and nitrogen, which will react
with carbon surfaces to form nitrogen functionalities such as
NH2,  CN, pyridinic, pyrrolic, and quaternary N2 [122,124].
The development of the nitrogen-functionalities on the carbon
surface can be proved by an increment in the nitrogen content,
according to the CHNS analysis. Plaza et al. [127] reported that
upon the amination process, the composition of nitrogen on the
synthesized activated carbon will increase from 0.7–1.0 wt% up to
4.5 wt%. Besides, these free radicals are liable for narrow
microporosity development and an enhancement in the surface
area, due to the chemical reaction between them and carbon active
sites which leads to the release of gas products; i.e. H2, CH4, HCN,
and (CN)2 [75,127]. Nevertheless, the surface of activated carbon is
said to be non-reactive towards NH3 gas. Therefore, pre-oxidation
prior to the amination process is proposed [115]. In this technique,
the carbon samples will be pre-heated with air until preferred
temperature is reached, then only purified NH3 is introduced into
the reactor [115,128]. Shafeeyan et al. [128] stated that presence of
oxygen functional groups prior to introduction of nitrogen
functionalities is significant, since it may act as anchoring sites
to react with the free radicals from NH3 decomposition process.
The impact of amination process towards the textural properties
and CO2 capture is as tabulated in Table 4. Aside from amination
process, these nitrogen functionalities can be incorporated into the
carbon matrix through wet impregnation process. Besides, amine-
based solvents are often utilized as the sources of the nitrogen Fig. 4. Surface morphology of (a) pristine activated carbon and (b) AMP-
groups. The doping of the amine compounds into the carbon impregnated activated carbon magnified at 40,000 times; reprinted with
structures is anticipated to bring similar benefits as chemical permission from [131], Copyright 2012 Elsevier.
10 N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16

(AMP) onto the surface results in formation of small and thin The recent work on the performance of CO2 capture by amine-
threads as shown in Fig. 4(b). functionalized activated carbons is tabulated in Table 4. According
Plaza et al. [133] claimed that the activated carbon should be to Table 4, it shows the competence of the amine-functionalized
impregnated without cancelling the physisorption, so that the activated carbon in CO2 capture at elevated temperature. The
modified activated carbons can be used in both ambient and enhancements in CO2 uptake by the amine-modified adsorbents at
elevated temperature. In addition, Bezerra et al. [135] affirmed that high temperature indicate an occurrence of chemisorption process,
the wet-impregnation process must be attentively prepared so that owing to acid-base reaction between amine molecules in activated
amino group can uniformly disperse onto the carbon surfaces carbon and acidic CO2 gases. This chemical reaction that is
without collapsing or clogging in pore structures in order to allow favoured at high temperature clarifies the improvement of the CO2
both diffusion and adsorption process. Accordingly, Arenillas et al. uptake of the modified carbon material. In addition, it has been
[137] suggested that mesoporous carbon is a good starting material reported that the increment in the CO2 uptake is due to expansion
for the impregnation process, as it controls good dispersion of of amine compound (i.e. PEI) in the pores. At low temperatures, the
amine polymers onto the pores and leads to high CO2 adsorption at PEI molecules reside inside the pores and only the external surface
high temperature, whilst the surface area and pore structure sites of PEI are accessible to the CO2 molecules. Meanwhile, at
governs the CO2 adsorption at lower temperature (physisorption). elevated temperatures, these PEI molecules will expand and fill in
Similarly, Dutcher et al. [19] and Wang et al. [129,138] supported the meso-structured materials, and accordingly, becomes more
that the mesoporous carbon with high surface area is a good accessible towards the CO2 molecules [139]. Furthermore, it is
platform for the impregnation step, as large pore volumes will help reported that the impregnation process will alter the surface
to circumvent the pore blockage by the additive amine-based chemistry of activated carbon, and thus, develop specific sites for
compounds, and consequently, minimize surface and inner pore the CO2 adsorption rather than dispersion force, i.e. van der Waals
diffusion resistance for the adsorption and desorption to occur. only [135]. The reactions which occur between the amine group
Besides, large pore volume of the materials will assist in high and CO2 during the CO2 adsorption process is shown in Eqs. (13)–
loading of the amine compounds into the carbon matrix. Thus, it (14), which correspond to the development of carbamate and
increases the CO2 adsorption capacity through a chemisorption bicarbonate (in presence of water) ions, respectively [25].
process [130]. Besides, Plaza et al. [133] obtained equivalent
CO2 þ 2R2 NH$R2 NH2 þ þ R2 NCOO ð13Þ
findings in which impregnated mesoporous sludge resulted in an
excellent CO2 adsorption capacity at 25  C, which is twice than
non-impregnated carbon. The findings could be due to the pore
sizes of the mesoporous materials are unaccountable for CO2 CO2 þ 2H2 O þ R2 NCOO $2HCO3  þ R2 NH2 þ ð14Þ
uptake at room temperature, and accordingly, the amine impreg- Nonetheless, multi-step scheme (activation and post-synthesis
nation process will facilitate the CO2 adsorption onto the modification) of the mesoporous activated carbon is impractical as
mesoporous activated sludge at lower temperature. it may be pricey and time-consuming. Therefore, to circumvent
this shortcoming, carbon activation using nitrogen-enriched

Table 4
Nitrogen-modified activated carbons.

Sample Modification process BET surface area (m2/g) Micropore volumes (cm3/g) CO2 adsorption (mmol/g) Ref.

Room temp. High temp.


(20–30  C) (50–120  C)
Cotton stalk Untreated 610 0.24 2.3 0.5 (120) [59]
NH3 treatment at 900  C 435 0.19 1.8 0.9 (120)

Eucalyptus wood Untreated 1889 1.063 3.0 – [75]


NH3 treatment at 400  C 2079 1.165 3.2 –

Palm shell activated carbon NH3 treatment at 800  C n/a n/a – 0.6 (105) [115]
Pre-oxidation NH3 treatment at 800  C n/a n/a – 0.7 (105)

Commercial activated carbon Untreated 768 0.358 1.2 – [128]


NH3 treatment at 800  C 889 0.442 1.7 –
Pre-oxidation NH3 treatment at 800  C 826 0.396 1.6 –

Mesoporous carbon Untreated 757 0.08 n/a 0.05 (75) [129]


Poly-ethylene (PEI) 78 0.00 3.66 4.82 (75)

Palm shell activated carbon Untreated 882 n/a – 0.8 (40–50) [130]
2-amino-2-methyl-1-proponol (AMP) 30 n/a – 1.5 (40–50)
2-amino-2-methyl-1, 3-propandiol (AMPD) 13 n/a – 1.2 (40–50)
2-(methylamino) ethanol (MMEA) 34 n/a – 1.0 (40–50)

Palm shell activated carbon Untreated 838 n/a 0.41 – [131]


Mono-ethanolamine (MEA) 65 n/a 1.11 –
AMP 102 n/a 0.77 –

Bagasse activated carbon Untreated 923 0.528 0.45 0.15 (75) [132]
PEI 484 0.258 0.30 0.20 (75)
MEA 300 0.170 0.35 0.15 (75)
Aniline (ANL) 574 0.337 0.29 0.14 (75)
N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16 11

carbonaceous precursors should be explored as it can cater for both surface, whereas large mesopores will assist in better dispersion of
physisorption and chemisorption processes, and thus, suits the the metallic species and enhance their efficiency [150,151]. In
post-combustion flue gas application in which the operating contrast, doping CoO, Co3O4, and CrO3 compounds into the carbon
temperature ranges from 50 to 150  C. materials after the activation process will cause a reduction in the
surface area as well as pore volume [151]. The surface area
3.2. Metal oxides-modified activated carbons reduction is due to deposition of the metal compounds into the
interior carbon structures, and blocks some parts of the micro- and
Aside from nitrogen doping, another technology to enhance the mesopores. Likewise, Moradi [152] observed that Fe-doping onto
CO2 uptakes from flue gases is through metal impregnation. the microporous activated carbon results in lower surface area
Impregnation by metal elements onto carbon matrix can be (1511 m2/g) and pore volume (0.81 cm3/g), as compared to host
justified in terms of the chemical reaction between metal oxide material that has surface area and pore volume of 1640 m2/g and
and CO2 molecules, especially at elevated temperature. In addition, 0.93 cm3/g, respectively.
Hosseini et al. [140] reported that the presence of copper oxide In addition, Qiao et al. [153] agreed that catalytic activation is a
onto the carbon material can enhance the adsorption capacity of good technology in converting the microporous to mesoporous
acidic molecules, since metallic oxides are classified as electron activated carbon. During this process, metal salt is anticipated to
donors. Opposite to nitrogen doping technique, the metal penetrate into the microstructures of activated carbon and to react
impregnation towards carbon adsorbent is scarce. The recent with the carbon atoms in the pore walls. Accordingly, mass of
work on metal impregnation is tabulated in Table 5. metal salt that should be loaded into the activated carbon need to
The significance of metal doping technique that includes the be optimized, since lower amount does not significantly affect the
utilization of alkaline earth metals (i.e. Mg, Ca) [144,145] and structural of the adsorbents, whilst excessive catalyst will lead to
transition metals (i.e. Cu, Co, Ni, Fe, Cr) [145–147] is elucidated in severe activation process that worsen the textural properties. In
terms of possible enhancement of CO2 adsorption due to high addition, this catalytic activation process which will drive and
affinity of metal elements towards CO2 molecules, mainly at promote the activation process is advantageous, as the activation
elevated temperatures. In addition, Yong et al. [144] mentioned can be performed at lower temperature. The lower temperature
that an introduction of alkaline metal or earth metal (i.e. Ca and Mg will prevent the sintering of metal (i.e. copper) catalyst, and thus
element) onto the activated carbons will produce a basic surface facilitate better distribution of catalyst particles onto the carbon
that has strong affinity towards CO2 molecules, and thus surfaces [148].
contributes to high adsorption capacity and selectivity. Hosseini Besides, it is reported that wet impregnation of metal
et al. [140] who studied the performance of the CO2 adsorption compounds can be further improved by an acidic treatment (i.e.
onto Cu/Zn modified activated carbon suggested that the catalytic HNO3) prior to the wet impregnation process [140]. During the first
surfaces provide active sites to adsorb a single CO2 molecule. The stage, acids act as oxidizers and thereby, increase the amount of
oxygen atoms in the CO2 molecules will contact and chemisorbed oxygen functional groups that contain proton donors. Accordingly,
onto the cationic Cu2+ and Zn2+ on the carbon support, and shorter the acid-modified carbons will have a strong connection with
distance between the cations and CO2 adsorbates will favour the metal ions (i.e. Cu2+, Zn2+) to produce metal complex, due to
adsorption process due to lesser adsorption energy [140]. formation of high polarity in the modified carbons. Moreover, Liu
The usual practice for metal impregnation process is called a et al. [20] also agreed that introduction of polar functional groups
wet impregnation technique, in which it involves a mixing process is significant for CO2 uptake, due to the fact that the CO2 molecules
of activated carbon with inorganic salts that contain specified have high quadrapole moment.
metals, and followed by a calcination process at high temperature Aside from wet impregnation technique, solid–solid mixing of
[148]. Since introduction of metal additives to the carbon carbon materials with metal-based precursors for direct pyrolysis
structures alters their surface chemistry, Alvim-Ferraz et al. process has been proposed lately [154]. The purpose of blending
[149–151] investigated the effect of impregnation technology of the precursors is to develop porous adsorbent which also contains
the metal-based element onto the char before (carbonization- active chemical for an efficient gas separation. In addition, this
impregnation-activation) and after activation (carbonization- one-step process is promising as it prevents multi-stage process
activation-impregnation) process. The findings showed that when that involves carbonization, activation, and subsequent modifica-
the transition metal-oxides (CoO, Co3O4, and CrO3) are added prior tion. Accordingly, Przepiórski et al. [141,154,155] studied the one-
to the activation step, the metal species will act as catalysts to stage pyrolysis of the mixture of PET waste with either dolomite or
facilitate faster gasification reaction, and to allow development of limestone at high temperature of 850–1000  C under an inert
large micro- and mesopores. The catalytic activation is proved by atmosphere. During the thermal treatment, dolomite and lime-
the time consumption to achieve 30 wt% weight lost in the stone decomposes to form CaO and MgO while releasing CO2 gas,
activation step, in which 1.5 wt% and 3.0 wt% CoO loading able to and PET waste will be converted to char. Besides, it is anticipated to
reduce the needed time by 50 and 67%, respectively [151]. Besides, obtain adsorbents with high porosity, owing to the reaction
the development of wider micropores allows an easier access of between the CO2 from calcination of metal carbonate sample with
the metal oxides, and contributes to significant deposition onto the the produced char from PET. From the adsorption standpoint,

Table 5
Recent work on metals-modified activated carbons for CO2 adsorption.

Sample Modification process BET surface area (m2/g) Micropore volumes (cm3/g) CO2 adsorption (mmol/g) Ref.

Room temp. High temp.


(20–30  C) (50–100  C)
Norit SA2 Untreated 1316 0.700 1.52 (30) 0.60 (50) [140]
Acid treatment ! Cu/Zn impregnation 599 0.399 2.26 (30) n/a
PET/dolomite Blending technique 106 0.05 0.22 (20) 0.28 (70) [141]
Coconut shell activated carbon Cu impregnation 1339 0.544 – 0.37 (50) [142]
MgCl2 loaded sawdust Pyrolysis 306 n/a – 5.45 (80) [143]
12 N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16

composite carbon/metal adsorbent is valuable for CO2 uptakes as it Referring to their findings, it was observed that the maximum CO2
combines physical interaction due to the presence of micropores adsorption capacity at 30  C and 105  C was approximately 2.7 and
and chemical interaction between the basic sites (i.e. CaO, MgO) 0.8 mmol/g, respectively. The comparison in terms of their
and CO2 adsorbates. Overall, mixture of metal carbonates and adsorption capacity with the conventional heated activated carbon
carbonaceous precursors is desirable, since the metal carbonates (some cases) in Tables 2 and 3 verifies the effectiveness of the
will emit CO2 gases which will act as activating agent for microwave processing in developing porous carbon materials
subsequent activated carbon formation, whereas presence of which suit for gas adsorption applications.
metal oxides can strongly fix the CO2 adsorbates onto the Another issue on the activated carbon production for CO2
adsorbent surface and improve the chemisorption process. uptake from flue gas is related to the lack of research study on the
dynamic gas adsorption. In fact, the recent works (2011-present)
4. Way forwards that predominantly focus on batch experimental run (static
adsorption) do not represent the real scenario, since adsorption
Despite the extensive research works on the invention of of the flue gas is carried out in a continuous adsorption column. In
activated carbon to cater various environmental problems, the static adsorption, the adsorbent (i.e. activated carbon) will be in
current activated carbon technology still impose several limita- contact with known amounts of gas adsorbates, whilst the
tions which include high cost expenditure and high energy dynamic adsorption occurs in an open system in which gas
consumption due to the utilization of conventional tubular furnace adsorbates continuously pass through the adsorption column until
for heating process. The difference between conventional heating an equilibrium state is achieved [165]. Besides, dynamic adsorp-
via furnace and microwave is based on the heating mechanism tion is significant because it presents good information for
[156,157]. In conventional approach via furnace, the heat source is researchers to design an appropriate operation unit for the up-
from the exterior and sample heating will occur through scaling and to suit the industrial applications [160,165,166]. In
conduction, radiation, and convection, in which the heating addition, Cukierman [166] proposed that multi-component gas
process begins from external and subsequently penetrates into adsorption is vital to be analysed, as it implies the real condition of
the interior sites [156–159]. With regards to this, the conventional flue gas stream in the post-combustion process. Moreover,
heating process is said to be time-consuming due to the longer exploration of the real flue gas condition is important as the
time needed to completely heat up the solid particles, and thus, selectivity of the synthesized activated carbons towards CO2 rather
impose a huge risk of ash formation due to longer operational time than the other gas pollutants can be identified. Therefore, integral
[159]. Oghbaei and Mirzaee [156] reported that this conventional research works that dedicate to comprehensive CO2 adsorption
furnace will induce high cost expenditures due to the exploitation with respect to adsorption capacity, selectivity, regeneration,
of large amount of heating elements, fuel, and refractory materials cyclic, kinetic, and thermodynamics analysis must be considered.
to achieve elevated temperatures and to maintain the specified Overall, the most important aspects to be considered while
temperatures for a long operational time. Likewise, Li et al. [160] researching on the activated carbon production are the selection of
mentioned that another limitation of the conventional approach is raw precursors. At present, the lignocellulosic waste materials are
related to the long-time duration which is up to several hours or extensively employed due to their widely abundance throughout
weeks to attain the specified activation process, and non- the country and are obtained at a lower cost. Moreover, utilization
uniformity temperature profile for different sample size and of carbonaceous waste prevents digging and mining process as is
shape. In addition, the temperature deviation between hot external encountered for coal and peat resources [167]. Further, exploration
surface and cool interior has obstructed the release of volatile of novel precursors which contains active sites such as nitrogen
gases and subsequently affect the quality of end products. Due to and metallic compounds is preferable as it avoids complex post-
these drawbacks, researchers have shifted to microwave technique modification process which is expensive and lengthy. The new
for the activation process. In contrast to the present technology, techniques in developing excellent activated carbon with high CO2
microwave technique offers cost saving, shorter operational time adsorption capacity and selectivity must be persistently
due to rapid temperature ramp, as well as reduction in the energy researched in order to achieve a simpler and finest method in
consumption [161]. The microwave technology is a process the activated carbon production, and without imposing environ-
wherein the heating process takes place at the molecular level mental damages. Referring to Perera [167], the activated carbons
and the sample will absorb the electrical energy and transform it are generally produced in a non-environmental manner despite
into heat [157,159]. In addition, the surface area and pore volume of their utilization in purification industry. Aside from developmental
the synthesized activated carbon through microwave heating are and utilization matters, the focus should also be emphasized on
observed to be higher than the conventional heating, since heat in effective activated carbons disposal technique in future.
the microwave technique is initiated from interior structure and
heating is carried out at a similar heating ramp, and as a result, 5. Conclusion
better volatiles diffusion from core particle to the surface occurs.
Hence, it produces better pore formation [162]. Besides, Xin-Hui Nowadays, global warming due to anthropogenic greenhouse
et al. [163] have examined the performance of the synthesized gas emission notably CO2 gas has become a major threat towards
activated carbon using microwave and conventional furnace and the ecological system. If the current trend continues without
with CO2 and steam as activators. Their findings proved that the precaution, negative outcomes such as severe flood and drought,
microwave processing produces economical carbon materials with increasing the prevalence of insects, and rise in sea level will likely
regards to low processing time and activator flow rate to achieve to occur. Hence, the potential of absorption, adsorption, cryogenic
optimal porosity and carbon yield. Therefore, it justifies that the distillation, and membrane separation to capture CO2 molecules
microwave processing can be carried out in a fast and uniform needs to be given a great attention and to ensure that only clean air
order. However, based on literature, research works on the is released to the surroundings. Though chemical absorption
microwave processing for activated carbons intend for the CO2 technique has already gains a wide acceptance for CO2 capture, the
adsorption are scarce. The only work that can be found for associated techno-economic issues prompted researchers to find
activated carbon production using microwave method is from alternative method to overcome the limitations of this state-of-art
Nasri et al. [164] who explored the potential of K2CO3-activated technology and to promote a viable and economical technique.
carbon using the microwave instrument for the CO2 adsorption. Therefore, the solid adsorption process specifically the
N.A. Rashidi, S. Yusup / Journal of CO2 Utilization 13 (2016) 1–16 13

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[158] R.H. Hesas, W.M.A.W. Daud, J.N. Sahu, A. Arami-Niya, The effects of a
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carbon from coconut shell chars in pilot-scale microwave heating equipment Department of Chemical Engineering, Universiti Tekno-
at 60kW, Waste Manage. 29 (2009) 756–760. logi PETRONAS, Malaysia. Her specialization includes bio-
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approach for production of activated carbon from phosphoric acid AP Dr. Suzana Yusup is registered with the Board of
impregnated palm kernel shell by microwave heating, J. Clean. Prod. 105 Engineers, Graduate member of Institution of Engineers
(2014) 420–427. Malaysia, Associate member of the Institutional of
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phosphoric acid activation: application in methylene blue adsorption,
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Nor Adilla Rashidi received her Bachelor in Chemical


Engineering (Hons.) in 2010 and MSc in Chemical
Engineering by research mode (2014) from Universiti
Teknologi PETRONAS, Malaysia. She is now working as a
Research Officer at Biomass Processing Group, Universiti
Teknologi PETRONAS. Her research interests include
material development, wastewater treatment, and car-
bon capture and storage.

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