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Impact of KOH Activation on Rice Husk Derived Porous Activated

Carbon for Carbon Capture at Flue Gas alike Temperatures with
High CO2/N2 Selectivity
Rajib Nandi,* Mithilesh Kumar Jha,* Sujit Kumar Guchhait,* Debanjan Sutradhar,
and Shashikant Yadav*

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ABSTRACT: Metal-free porous activated carbon is an effective alternative

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to capture CO2 due to its high surface area and textural advantages. In this
regard, the present research work explores a suitable method for producing
activated porous carbon with a high specific surface area through a two-step
reaction involving rice husk and KOH at 600 °C for 1 h to capture CO2. By
varying the ratio of rice husk biomass to KOH, the texture and specific
surface area of the activated porous carbon has been altered. A high surface
area of ∼755 m2/g and a micropore volume of 0.243 cm3/g have been
observed in the porous carbon produced with a KOH/biomass weight ratio
of 3 (PAC2). Nitrogen contents in PAC1 and PAC2 were approximately
2.27 and 2.71 atom %, respectively. When compared with other materials,
PAC2 has the highest CO2 adsorption capability, reaching up to 3.13
mmol/g at 0 °C and 1.55 mmol/g at 50 °C. The isosteric heat of adsorption
confirms the presence of both physisorption and chemisorption. The materials turn out to be highly CO2/N2 selective, with the
highest selectivity of 131, proving that the samples are potential materials for capturing CO2 from flue gases. These findings
unequivocally show that porous activated carbon can be used to make CO2 adsorption efficient, inexpensive, and, more importantly,
extremely effective.

■ INTRODUCTION
The anthropogenic CO2 concentration has increased rapidly
class of hybrid porous solid sorbents with promising
technological advancement. These were naturally explored
since the industrial era started, and it is now exceeding 410 for gas adsorption because they had especially high porosities
ppm, which is more than 50% higher than preindustrial levels.1 and high surface areas.15 With regard to post-combustion CO2
According to IPCC, the global mean temperature has already capture, MOFs with metal-binding sites displayed higher CO2
increased 0.8−1 °C, and it needs to be controlled before the affinities, ensuring adequate adsorption capacity. However,
temperature increases to 2 °C by 2100. The carbon dioxide- these sites also had the drawback of the stability of the MOFs.
capturing process is an important technology for the world to The majority of the studied COFs are fairly typical physical
become net-zero, where most of its energy comes from fossil adsorbents. As COFs have a low adsorption capacity compared
fuels.2−4 Amine scrubbing is the most cutting-edge technology with other materials, especially under post-combustion CO2
for CO2 capture from flue gas. However, this technology capture conditions, they are typically used in high-pressure
suffers from significant drawbacks, including a high energy environments.
requirement, equipment corrosion difficulties, solvent degra- In this regard, porous activated carbon materials exhibit
dation, and possibly hazardous waste generation.5 However, significant potential because they are easily synthesized, are
CO2 capture by adsorption is effective, having low-cost inexpensive, have adaptable pore architectures, possess high
materials, low heat capacity, fast kinetics, high CO2 adsorption
capacity, high CO2 selectivity, and very high thermal,
mechanical, and chemical stabilities.6 Various novel solid Received: October 28, 2022
sorbents such as zeolites,7 silica,8 porous polymers,9 carbon,10 Accepted: December 27, 2022
metal−organic frameworks (MOFs),11 and ionic liquids12 are Published: January 13, 2023
reported for carbon capture. In contrast to the traditional
materials used for CO2 capture and utilization, MOFs11 and
covalent organic frameworks (COFs)13,14 represent a novel
© 2023 The Authors. Published by
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chemical and thermal stability, etc.16 Agricultural residues and properties, CO2 adsorption capacity, and CO2/N2 selectivity
food waste such as almond shells,17 coconut shells,18 performance of the sorbent in detail with various model fits.
mushroom,19 rice husk (RH),20 etc., have been widely studied Here, rice husk has been used as feedstock, and a two-step
in the preparation of porous activated carbon after feedstocks method was followed to prepare porous activated carbon while
go through one-step or two-step carbonization and activation varying the KOH/biochar mass ratios. The maximum BET
processes. The properties of these porous activated carbons surface area of 755 m2/g and micropore volume of 0.243 cm3/
can be altered by altering the activator/carbon source ratio,21 g were obtained at a KOH/carbon ratio of 3 (porous activated
activation temperature,22 and activating agents such as K2CO3, carbon 2; PAC2). Various physicochemical properties of the
KOH H3PO4, ZnCl2, etc.23−27 synthesized material have been characterized by X-ray
Recently, extensive research interest has been focused on diffraction (XRD), field-emission scanning electron micros-
studies on the production of activated porous carbon from copy (FESEM), thermogravimetric analysis (TGA), BET,
waste or biomass and their application for CO2 adsorption. CHNS, X-ray photoelectron spectroscopy (XPS), and CO2
Rattanaphan et al.28 synthesized activated carbon from used adsorption studies. By modifying the preparation conditions
tea leaves using NaOH as an activator and modified it with and performing surface modifications, CO2 adsorption
ethylenediamine to serve as a CO2 sorbent. At 30 °C and 1 bar capacities of 2.89 and 3.13 mmol/g, at 1 bar, 0 °C for PAC1
pressure, they claimed that the CO2 adsorption was equivalent (porous activated carbon 1) and PAC2, respectively, were
to 2.5 mmol/g. Nitrogen-doped activated carbons were found. PAC1 shows a very high CO2/N2 selectivity of 131 at
prepared by Yue et al.29 using urea-modified coconut shell 0.1 bar and ∼ 37 at 1 bar (calculated viz. IAST method).
and K2CO3 as the activating agent. The activated carbon
material shows CO2 uptakes of up to 3.71 mmol/g at 25 °C
and 5.12 mmol/g at 0 °C at 1 bar. Activated carbon was also
■ EXPERIMENTAL SECTION
Materials. Rice husk was collected from West Bengal,
prepared by Choi et al.30 utilizing pollens and KOH as the potassium hydroxide (KOH) was from Merck, and concen-
activating agent for CO2 adsorption. A KOH/carbonized trated hydrochloric acid (98% HCl) was obtained from
pollen ratio of 3:1 at 800 °C produced the highest activated (Merck). All of the compounds were used as received without
carbon material with a surface area of 1460 m2/g. This material additional purification.
has a high CO2/N2 selectivity (15−12 in the 0−1 bar range) Synthesis of Rice Husk Biochar (RHBC) and Porous
and the highest CO2 sorption values of 5.63 and 3.42 mmol/g Activated Carbon. The rice husk sample was washed with
at 0 and 25 °C, respectively. Hong et al.31 synthesized activated distilled water and placed in an oven at 70 °C overnight to
carbon utilizing packing peanuts by physical and chemical remove moisture. Then, the dried rice husk was pyrolyzed at
activation. It is found that chemical activation can provide a 600 °C in a vertical vacuum pyrolyzer for 2 h to obtain rice
greater microporous carbon structure compared with physical husk biochar. The heating rate was fixed at 5 °C/min. The rice
activation.31 At a KOH/carbon ratio of 5, the highest husk biochar was further used to synthesize activated carbon.
Brunauer−Emmett−Teller (BET) surface area of 2420 m2/g The biochar was activated by KOH in two different weight
has been reported. They claimed that as the KOH/carbon ratios, i.e., 1:1 and 1:3 (biochar/KOH), respectively. Then, the
mass ratio increases, both the specific surface area and the total mixture was heated at 400 °C for 30 min, after which the
pore volume increase. However, the maximum CO2 adsorption temperature was increased to 600 °C and maintained for 1 h.
abilities of 6.51 and 4.07 mmol/g at 0 and 25 °C, respectively, After cooling, the sample was collected and neutralized with
were obtained using peanut-derived activated carbon with a 0.5M HCl and finally washed with distilled water. The
KOH/carbon ratio of 3 rather than 5. Recently, KOH- obtained product was dried in an oven. The final products
impregnated rice-husk-derived activated carbon was used by activated by the mixed activators were named porous activated
Wang et al. to create a high-performance adsorbent for indoor carbon 1 (PAC1; biochar/KOH weight ratio 1:1) and porous
CO2 adsorption.20 DKOH-AC revealed a high adsorption activated carbon 2 (PAC2; biochar/KOH weight ratio 1:3).
capacity of 2.1 mmol/g at a low amount of indoor CO2 Characterization of Adsorbents. Proximate and ultimate
(2000−500 ppm). The outcomes demonstrated that despite analyses of raw rice husk and the biochar were performed to
sacrificing the BET surface area, KOH impregnation greatly determine the basic contents and elemental compositions of
increased the CO2 adsorption capability (via chemisorption). the materials. The elemental composition of the materials was
Among the aforementioned carbon materials, those with determined by a CHNS analyzer using an Elementar
microporous structures are useful for CO2 capture due to instrument. The proximate characterization was conducted as
their remarkable properties, which have led to high CO2 per the standard ASTM standards (D-3173, D-3174, and D-
capture efficiency and selectivity. To the best of our 3175) to determine the moisture, volatile matter, and ash
knowledge, there are very few reports on the effect of the content of both biomass and biochar samples.32 For moisture
concentration of activation agents on the porous texture, determination, samples were oven-dried at 105 °C for 2 h. The
surface properties, and CO2 adsorption performance of samples were heated at 950 °C for 7 min in a muffle furnace
sorbents. However, the inability to regulate the growth and for volatile matter determination. For ash content determi-
formation of the pore structure is still a significant challenge in nation, the samples were heated at 750 °C for 30 min. Fixed
the preparation of activated carbon adsorbents derived from carbon was determined by subtracting the sum of moisture,
waste biomass. The novelty of this study is the utilization of volatile matter, and ash from 100. The powder X-ray
waste biomass to prepare an effective carbon-based adsorbent diffraction (PXRD) study was conducted using a Bruker D8
with efficient CO2 capture properties with great selectivity, and Advance instrument in the scanning range of 20−80°. The X-
the role of the activating agent concentration to prepare ray diffractometer had a Cu cathode for the generation of X-ray
effective porous activated carbon has been discussed in detail. of wavelength 1.54 Å. Thermal parameters of the materials
In the present work, we examined the effect of activation were evaluated by thermogravimetric analysis using a Perkin-
agent/biomass precursor ratios on the porous texture, surface Elmer STA6000 thermogravimeter. It was performed in the
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Figure 1. SEM images of (a) RHBC and (b, c) activated carbons PAC1 and PAC2, respectively, prepared with different KOH-to-biomass ratios at
a temperature of 600 °C.

temperature range of 30−900 °C with a heating rate of 20 °C/ where qe (mmol/g) is the adsorption capacity at equilibrium,
min under non-isothermal conditions (N2 atmosphere with a q0 (mmol/g) is the saturated amount of the gas adsorbed, and
flow of 50 mL/min). The morphological analysis of the b is given by b = b0 eQ/RT, where b0 is the adsorption affinity, Q
samples was carried out by field-emission scanning electron is the isosteric heat of adsorption, R = 8.314 J mol−1 K−1, and P
microscopy (FESEM) (model JEOL JSM-7610F). The (kPa) is pressure.
elemental and chemical compositions of the sample were
determined using a Thermo Scientific K-Alpha X-ray photo- qe = kFP1/ nF (2)
electron spectrometer (XPS) equipped with an Al Kα X-ray
source. Surface area and other parameters were determined by Here, kF is the Freundlich constant and nF is the adsorption
N2 adsorption−desorption isotherms at 77 K using a 3FLEX intensity.
3500 from Micromeritics Instrument Corporation. Before the q0bP
measurements, all samples were degassed at a temperature of qe =
200 °C for 24 h. Using the Brunauer−Emmett−Teller (BET) (1 + (bP)k T )1/ k T (3)
equation, the specific surface area (SBET) values of the samples
Here, kT′ is the surface heterogeneity parameter. This equation
were calculated, the total pore volume was computed at a
reduces to the Langmuir model when kT′ becomes 1.
relative pressure of P/P0 = 0.99, the micropore volume was
The isosteric heat of adsorption was calculated by the
determined by the t-plot method, and the average pore width
Clausius−Clapeyron equation.35 It is used to measure the
was determined as 4Vt/SBET. The pore size distribution (PSD)
enthalpy change when adsorbate molecules are adsorbed from
was estimated by the nonlocal density functional theory
the bulk phase to the adsorbed phase. The calculation was
(NLDFT) assuming a slit-pore model.
performed for all samples based on their adsorption isotherms
CO2 Adsorption Experiments and Model Fit. The CO2
at three different temperatures: 0, 25, and 50 °C.
adsorption study was also conducted using a 3FLEX 3500 from
The equation is given as follows:
Micromeritics Instrument Corporation. All of the samples were
tested at three different temperatures 0, 25, and 50 °C. The ij P yz HS ijj 1 1 yzz
lnjjj 2 zzz = j z
R jjk T2 T1 zz{
adsorption plots were fitted to different adsorption isotherms, jP z
i.e., the Langmuir, Freundlich, and Toth isotherms. The k 1{ (4)
Langmuir model predicts that adsorption occurs only in a where ΔHS (kJ/mol) is the isosteric heat of adsorption, R =
monolayer formation on the adsorbate; it is a theoretical 8.314 J mol−1 K−1, and pressure and temperature are denoted,
expression. The empirical Freundlich model predicts multilayer respectively, as P (kPa) and T (K).
adsorption on a heterogeneous adsorbent, whereas the Toth Adsorbent selectivity is a very important parameter as it
model is a three-parameter model extended from the Langmuir shows the capability to adsorb at different temperatures and
equation taking the heterogeneity of adsorbent surfaces into pressures. Moreover, in the case of mixed component
account.33 The Langmuir, Freundlich, and Toth models are adsorption, it is necessary to determine the selectivity of one
given below in eqs 1−3, respectively:33,34 adsorbent over another toward a component. To determine
q0bP the selectivity of the adsorbent in a mixed component
qe = adsorbate, the ideal adsorption solution theory (IAST) was
1 + bP (1) proposed.36,37 In this method, the adsorption of a binary
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mixture can be predicted from pure component adsorption KOH + CO2 K 2CO3 + H 2O (12)
isotherms. First, the pure component data are fitted to the
In addition, the biomass carbon reacted with potassium
Toth isotherm model (it showed the highest R2 value), and
carbonate or potassium oxides, which contributed to the
then calculations are based on the selectivity equation:
development of pores. During washing with HCl and water,
Adsorption selectivity: potassium compounds (i.e., K2O, K2CO3, and K) that are
x1/y1 intercalated into the carbon structure are eliminated, as a result
Sads = of which a high surface area and highly porous activated carbon
x2/y2 (5) were generated.
where x is the molar fraction of components in the adsorbed K 2CO3 + 2C 2K + 3CO (13)
phase and y is the same in the bulk phase (in different sites).
K 2CO3 + 2C K 2O + 2CO (14)

■ RESULTS AND DISCUSSION

The FESEM morphologies of rice husk biochar (RHBC) and
K 2O + C 2K + 2CO (15)
Proximate analysis of the material before pyrolysis and after
KOH-impregnated porous activated carbon (PAC1 and
forming the biochar shows 63.45 and 21.36% volatile matter in
PAC2) are shown in Figure 1a−c. From the morphological
them, respectively, and the amount of fixed carbon content
analysis, it is found that no pores are present in the biochar;
increased from 7.91 to 34.35% after pyrolysis (Table 1). The
however, KOH activation produces a highly developed porous
structure with micron-sized pores observed on the surface of
porous activated carbons (i.e., PAC1 and PAC2, respectively). Table 1. Properties of the Rice Husk and Its Biochar
It has also been noticed that pores increase drastically with an properties rice husk biochar (BC)
increase in the KOH impregnation ratio. Moreover, after Proximate Analysis
chemical activation, the smooth and regular surface of the moisture (%) 10.53 4
RHBC was replaced by pores, and PAC2 showed a very volatile matter (%) 63.45 21.36
uniform highly porous structure compared with PAC1. The ash content (%) 18.11 40.39
surface after activation has larger pores of around 2−5 μm size, fixed carbon content (%) 7.91 34.25
with micropores and mesopores concealed inside the surface. Ultimate Analysis
The surface area analysis of PAC2 shows ∼76.34% as the carbon (%) 25.6 70.87
micropore area out of the total surface area. The main function hydrogen (%) 4.5 1.514
of KOH is to assist in the oxidation of rice husk. In the nitrogen (%) 0.5 1.48
activation process, it is thought that the reaction between sulfur (%) 0.4 0.1
KOH and carbon creates gases that encourage the creation of oxygen (%) 69 26.036
pores, particularly small mesopores and micropores. KOH also
removes tar and aids in the removal of pollutants such as SiO2.
Carbon is oxidized to produce carbon dioxide, hydrogen, ultimate analyses suggest that the overall carbon percentage of
metallic potassium, water, and potassium carbonate. In this the biochar increased from 25.6 to 70.87%. This proves that
regard, Singh et al.38 and Serafin et al.16 proposed a redox pyrolysis was able to remove all of the volatile matter inside the
reaction mechanism between biomass carbon and KOH and material and make the material more carbonaceous with
described the effect of the activating agent on pore formation. potential for CO2 capture.39
The synthesis of activated carbon and the emergence of high X-ray diffraction patterns of rice husk, rice husk biochar, and
porosity are the results of subsequent reactions and the porous activated carbon are shown in Figure 2. Three
evolution of volatiles from the biomass surface that took place characteristic peaks are seen in the XRD patterns of rice
during the carbonization process in conjunction with chemical husk at 2θ values of 16, 23, and 35°, which are reported to be
activation. Typically, when KOH combines with biomass peaks of cellulose, and the peaks observed between 10 and 35°
carbon, K2CO3, metallic potassium, evolved hydrogen, and are attributed to the diffraction of amorphous carbon.40 In the
carbon monoxide are produced. The reactions are as follows pyrolytic rice husk biochar, the broad peak found between 18
and 29° is attributed to the C (002) plane. There is another
2KOH + C + H 2O K 2CO3 + 2H 2 (6) broad region with less intensity at 2θ between 42 and 47°
attributable to the C(100) plane. Previous results suggest that
6KOH + 2C 2K 2CO3 + 2K + 3H 2 (7) these peaks reflect the condensed aromatic carbonized planes;
or the sharper the peak, the higher the degree of condensation of
the aromatic ring.40−43 All of these characteristics were
2KOH + 2C 2CO +2K + H 2 (8) retained in the KOH-impregnated activated carbon; however,
the C(002) and C(100) peaks are slightly more intense than
2KOH K 2O + H 2O (9) those of biochar, which confirms that KOH activation has
The functional groups abundant in biomass are also degraded enhanced its degree of carbon ordering.
in the presence of KOH into volatiles such as water and carbon Thermogravimetric analysis (TGA) of the rice husk (RH)
dioxide, which contribute to porosity as they are released and rice husk biochar (RHBC) are shown in Figure 3a,b. The
through the structure of carbon. initial degradation at around 40−150 °C accounts for weight
loss due to the moisture present in both samples. The RH
2C + 3H 2O 2CO + 6H 2 + 2CO2 (10) sample showed two weight-loss stages at 200−450 °C,
attributed to the decomposition of hemicellulose and cellulose,
C + CO2 2CO (11) and at 450−750 °C, assigned to the gradual decomposition of
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Figure 2. XRD patterns of (a) rice husk and RHBC and (b) RHBC and activated carbons (i.e., PAC1 and PAC2) prepared with different KOH/
biomass ratios at a temperature of 600 °C.

Figure 3. TGA−derivative thermogravimetry (DTG) analysis of (a) rice husk (RH) and (b) rice husk biochar (RHBC).

Figure 4. N2 adsorption−desorption isotherms of (a) rice husk biochar (RHBC) and (b) activated carbons (i.e., PAC1 and PAC2) prepared with
different KOH/biomass ratios at the temperature of 600 °C. (c) Pore size distribution of RHBC, PAC1, and PAC2.

Table 2. Textural Properties of BCRH and Its Activated Derivatives PAC1 and PAC2
samples SBET(m2/g) SBETmicro(m2/g) SBETmicro/SBET (%) Vt(cm3/g) Vmi(cm3/g) V<0.7 nm V<0.7 nm/Vmi (%) Vmi/Vt (%)
RHBC 9.77 0.02
PAC1 413.59 330.63 79.94 0.312 0.130 0.076 58.46 35.04
PAC2 755.73 630.20 83.39 0.393 0.243 0.176 72.46 52.78

lignin.6,44,45 Biomass having a high amount of hemicellulose DTG curve. The gradual weight loss after that is due to the
and cellulose results in microporous carbons, needed for carbonization of biomass.46 The sample RHBC is clearly stable
carbon dioxide adsorption, and rice husk is proved to have a up to 600 °C, and the gradual decrease in weight afterward is
high amount of hemicellulose and cellulose, as seen in the believed to be due to carbonization.
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Figure 5. N 1s XPS spectra of (a) RHBC, (b) PAC1, and (c) PAC2 samples.

Figure 6. (a) Survey spectra of RHBC, PAC1, and PAC2 samples. O 1s XPS spectra of (b) PAC1 and (c) PAC2. (d−f) C 1s XPS of RHBC, PAC1,
and PAC2, respectively.

The N2 adsorption−desorption isotherms are used to of the KOH amount is also observed (see in Table 2). PAC2
determine the physical characteristics of all samples, including exhibited the highest surface area of 756 m2/g, of which 630.20
their specific surface area, micropore volume, total pore m2/g constitutes the micropore area. This slightly less surface
volume, and pore diameter. Figure 4a,b shows the N2 area may be due to the formation of solid K2CO3 (see equation
adsorption−desorption isotherms and textural properties of
nos 6−15).47 The adsorption isotherm curves for the activated
all carbonaceous materials that are summarized in Table 2.
Rice husk biochar shows a very minute surface area and no biochars are type I according to the IUPAC classification. The
micropore area, which is very clear through the isotherm hysteresis plots in Figure 4b are almost horizontal and parallel
(Figure 4a). However, the KOH-activated samples showed a over a wide range; this depicts a H4-type hysteresis, suggesting
significant increase in the surface area, and a significant effect that the sample contains slit-like pores.48 In both the activated
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samples, high adsorption is seen at a very low relative pressure, highest nitrogen content (2.71 atom %), an N/C ratio of
which indicates the presence of mainly the micropores.49,50 0.056, and also the highest oxygen content of 49.08 atom %.
The BET surface area of the rice husk biochar is significantly PAC1 and PAC2 show relatively high nitrogen contents
low (9.77 m2/g) with no micropores and a pore volume of compared with that of RHBC. The high-resolution O 1s
0.02 cm3/g. The micropore area and volume were calculated spectra of PAC1 and PAC2 are shown in Figure 6b,c. In the O
through a t-plot analysis. PAC1 showed an SBET of 413 m2/g 1s spectrum, two prominent peaks are observed in all samples,
with a micropore area of 330 m2/g. With an increase in the which are assigned to C�O groups (531.2 eV) and C−OH or
char/KOH ratio to 1:3, the SBET increased to 755 m2/g, the C−O−C groups (532.8 eV).52,53 On the other hand, the high-
total pore volume to 0.393 cm3/g, and the micropore volume resolution N 1s spectra, shown in Figure 5a−c, can be
to 0.243 cm3/g. The data confirm that SBET and Vmi increased deconvoluted to contributions of pyridinic-N (398.6 eV),
due to KOH impregnation. Figure 4c shows the pore size pyrrolic-N (400.4 eV), and oxidized pyridinic-N (402.3 eV) in
distribution (PSD) curves of the porous activated carbon the carbon structure.53 Because these are chemically more
computed using the N2 adsorption data at 77 K. It was found active than their counterparts inside the carbon network, the
that the number of pores increased considerably with an carbon atoms on the edges of the graphitic layers can be
increase in the KOH impregnation ratio, which may due to the replaced with externally doped nitrogen atoms more easily,
effect of KOH. KOH activation caused the development of which leads to the generation of pyridinic-N and pyrrolic-N on
micropores, resulting in an enhanced surface area and total the surface.52,53 The pyrrolic peak is more prominent than the
pore volume as well as pore enlargement, particularly in the pyridinic peak in the chemically activated samples (Figure
presence of a large amount of KOH.30 The distribution clearly 5b,c), and these groups are predicted to be more effective at
suggests that the samples are mainly nano-microporous (0.3− attracting acidic CO2 molecules.53 The much higher amount of
0.6 nm) in nature, which helps in improving the CO2 carbon burnoff in activated samples results in the collapse of
adsorption capacity.51 the hexagonal ring into the pentagonal ring, which decreases
The chemical compositions of the RHBC, PAC1, and PAC2
the intensity of the pyridinic peak. The formation of pyrrole
samples were studied by XPS. Figures 5 and 6 show the XPS
peaks is caused by the chemical reactions of KOH, which
spectra of C 1s, O 1s, and N 1s observed for the RHBC, PAC1,
displaces more carbons from the surface of the condensed
and PAC2 samples. The quantitative surface chemical
aromatic structure of the carbon network.
composition is summarized in Table 3. PAC2 shows the
The CO2 adsorption at three distinct temperatures of 0, 25,
and 50 °C was measured under pressure. A comparison of the
Table 3. Quantitative Characterization of the Surface
CO2 adsorption capacities of different samples under various
Compositions of RHBC, PAC1, and PAC2
conditions is shown in Figure 7a−c and Table 4. PAC2
surface atomic concentration (%) exhibited the highest adsorption of 3.13 mmol/g at 0 °C at 1
C 1s O 1s N 1s bar pressure. At low pressure (0.1 bar), the samples also
RHBC 72.57 25.88 1.14
showed promising results, probably due to the presence of
PAC1 82.47 15.26 2.27
narrower micropores (V<0.7 nm).54 PAC2 has the highest
PAC2 48.21 49.08 2.71 amount of narrower micropores compared with the other
activated carbons (V<0.7 nm/Vmi is 72.46 > 58.46%), and this
resulted in the CO2 uptake of PAC2 being slightly higher (1.50
mmol/g) than that of PAC1 (1.48 mmol/g) at 0 °C

Figure 7. CO2 adsorption isotherms of the rice husk-derived carbons of (a) RHBC, (b) PAC1, and (c) PAC2.

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Table 4. CO2 Adsorption Capacities of RHBC, PAC1, and

PAC2
CO2 uptake (mmol/g)
0 °C 25 °C 50 °C
sample 0.1 bar 1 bar 0.1 bar 1 bar 0.1 bar 1 bar
RHBC 0.63 1.39 0.35 1.06 0.22 0.74
PAC1 1.48 2.89 0.86 2.11 0.53 1.54
PAC2 1.50 3.13 0.88 2.24 0.57 1.55

temperature and 0.1 bar pressure. At lower temperatures and

higher pressure, all three samples show the highest CO2 Figure 9. Comparison of CO2 uptake of the rice husk-derived carbons
adsorption capacity. Porous activated carbon was found to of RHBC, PAC1, and PAC2 under different conditions.
be a good CO2 uptake material at ambient temperature as well
as at 50 °C. At ambient temperatures and pressure, the samples
RHBC, PAC1, and PAC2 adsorb 1.06, 2.11, and 2.24 mmol/g,
respectively. PAC1 and PAC2 showed very similar results at 50
°C and 1 bar (1.54 and 1.55 mmol/g, respectively). The data
were further fitted to the Langmuir, Freundlich, and Toth
isotherms (Figure 8a,b), and the Toth isotherm displayed the
highest R2 of 0.999, suggesting heterogeneity of the adsorbent.
A comparison of the CO2 uptake under different conditions
has been plotted and shown in Figure 9.
The isosteric heat of adsorption of the samples was
computed using eq 4, and the relationship between that heat
and the amount of CO2 loaded is depicted in Figure 10. With a
continuously increasing CO2 load, the heat of adsorption tends Figure 10. Isosteric heat of adsorption of the rice husk-derived
to decrease for all samples. This might be due to high-energy carbons of RHBC, PAC1, and PAC2.
active adsorption sites getting bound to CO2 molecules, which
gradually decreases the heat of adsorption with the
consumption of high-energy active sites.55 The average in a CO2/N2 mixture (15:85 as per flue gas compositions). To
isosteric heat of adsorption for the materials are 24.94, calculate the selectivity, the data were first fitted to the Toth
26.66, and 25.26 kJ/mol for RHBC, PAC1, and PAC2, isotherm as it showed the highest R2 value of 0.999, and the
respectively. The higher the heat of adsorption, the stronger data were substituted in the selectivity eq 5. Here, we selected
the CO2 adsorption properties. Generally, an isosteric heat of the best set of data according to the CO2 adsorption
adsorption of 0−20 kJ/mol confirms physisorption, and a value performance, which is PAC1 and PAC2 at 0 °C, and compared
greater than 20 kJ/mol throughout the process implies that the the data with the N2 adsorption data for the same samples at
adsorption mechanism may include both physisorption and the same temperature. N2 adsorption was very lower compared
chemisorption.54,56 In the present study, the average isosteric with CO2 adsorption. Both samples showed very high
heat of adsorption for the samples are 24.94 kJ/mol for RHBC, selectivity at lower as well as ambient pressures at 0 °C.
26.66 kJ/mol for PAC1, and 25.26 kJ/mol for PAC2. These Manoranjan et al.45 and Wilmer et al.57 reported that the heat
results support the fact that KOH-activated porous carbon of adsorption plays a crucial role in determining the selectivity
shows both physical and chemical adsorption of CO2. of an adsorbent, and a heat of adsorption in the range of 18−
Under real-life conditions, the adsorbate might not be 27 kJ/mol is ideal for CO2 sorbents. In our study, the average
present as a single component, rather it will be present in a isosteric heat of adsorption for the materials are 24.94, 26.66,
mixed gas; as obtaining the adsorption quantity of a single and 25.26 kJ/mol for RHBC, PAC1, and PAC2, respectively.
component from the mixed adsorbate can be difficult, the Figure 11 shows the selectivity factors for the activated
IAST theory is used to calculate the selectivity of the adsorbent carbons. PAC1 showed the highest selectivity at 0.1 bar (131

Figure 8. Langmuir, Freundlich, and Toth isotherm model fits of the rice husk-derived carbon of (a) PAC1 and (b) PAC2.

4809 https://doi.org/10.1021/acsomega.2c06955
ACS Omega 2023, 8, 4802−4812
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Figure 11. (a) Toth fit and (b) IAST selectivity of rice husk-derived carbons of PAC1 and PAC2.

compared with 98 for PAC2) as well as at 1 bar (36.67 Mithilesh Kumar Jha − Dr. B. R. Ambedkar National
compared with 30 for PAC2). Such a high selectivity indicates Institute of Technology, Jalandhar 144011, India;
the good CO2-capturing ability of the KOH-activated carbons Email: [email protected]
from a flue gas stream. Sujit Kumar Guchhait − Sardar Swaran Singh National
Institute of Bio-Energy, Kapurthala 144601, India;
■ CONCLUSIONS
In summary, two distinct impregnation ratios were used in a
orcid.org/0000-0002-4534-4179;
Email: [email protected]
two-step procedure to create activated carbons from the Shashikant Yadav − Dr. B. R. Ambedkar National Institute of
chemical activation of rice husk. The optimum conditions for Technology, Jalandhar 144011, India; Email: shashikanty@
preparing the activated carbons were carbonization at 600 °C nitj.ac.in
and then KOH activation at a KOH/char ratio of 3:1. The Author
BET surface area obtained under this condition is 755 m2/g
with a micropore volume of 0.243 cm3/g. XRD of the sample Debanjan Sutradhar − Dr. B. R. Ambedkar National Institute
confirmed the amorphous nature of the sample, and FESEM of Technology, Jalandhar 144011, India; Sardar Swaran
confirmed that the KOH impregnation had a very positive Singh National Institute of Bio-Energy, Kapurthala 144601,
impact on the samples; with an increase in the impregnation India
ratio, the pore volume, especially micropore volume, increased. Complete contact information is available at:
The pore size distribution of the samples showed the presence https://pubs.acs.org/10.1021/acsomega.2c06955
of narrower micropores in the activated samples, which proved
to be the best for CO2 adsorption. The results are confirmed in Author Contributions
the CO2 adsorption study as PAC2 showed the highest CO2 R.N.: conceptualization, methodology, experiments, writing�
adsorption capacity of 3.13 mmol/g at 0 °C compared with original draft preparation; M.K.J.: supervision; Sujit Kumar
2.89 mmol/g for PAC1 and 1.39 mmol/g for RHBC. The data Guchhait: methodology, writing�original draft preparation,
showed comparable results at ambient temperature and at an conceptualization, preparation of the graphical abstract; D.S.:
elevated temperature of 50 °C. The high CO2 adsorption original draft preparation, preparation of activated carbon from
capacities of PAC1 and PAC2 are attributed to the presence of biomass; S.Y.: supervision, conceptualization, original draft
the highly microporous surface area and high nitrogen content preparation.
in the form of pyridinic-N and pyrrolic-N species in the
framework of the porous structure. The Toth model fitted the Notes
data very well because of the heterogeneity of the material. The The authors declare no competing financial interest.
isosteric heat of adsorption is more for PAC1, and the values
prove the occurrence of both physisorption and chemisorption
in the adsorption process. The activated carbon material shows
■ ACKNOWLEDGMENTS
R.N. and D.S. thank NITJ and SSS-NIBE for providing
a CO2/N2 selectivity of 131.39 at 0.1 bar and 36.67 at 1 bar research facilities. S.K.G. thanks the SSS-NIBE and Ministry of
(for PAC1), which indicates the material’s potential to be used New and Renewable Energy (MNRE), Govt. of India, for
for CO2 capture from a flue gas mixture. This research work is
providing fellowship. M.K.J., S.Y. thanks NITJ for providing
very significant from the perspective of our future efforts to
research facilities
produce effective and affordable activated carbons from
biomass. The methodology described here combines carbon-
ization with chemical activation and is a simple process using
inexpensive and easily available carbon sources that could be
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■ AUTHOR INFORMATION
Corresponding Authors
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9856.
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