Beruflich Dokumente
Kultur Dokumente
Rock Keey Liew, Elfina Azwar, Peter Nai Yuh Yek, Xin Yi Lim, Chin Kui
Cheng, Jo-Han Ng, Ahmad Jusoh, Wei Haur Lam, Mohd Danial Ibrahim, Nyuk
Ling Ma, Su Shiung Lam
PII: S0960-8524(18)30830-7
DOI: https://doi.org/10.1016/j.biortech.2018.06.051
Reference: BITE 20068
Please cite this article as: Liew, R.K., Azwar, E., Yek, P.N.Y., Lim, X.Y., Cheng, C.K., Ng, J-H., Jusoh, A., Lam,
W.H., Ibrahim, M.D., Ma, N.L., Lam, S.S., Microwave pyrolysis with KOH/NaOH mixture activation: A new
approach to produce micro-mesoporous activated carbon for textile dye adsorption, Bioresource Technology (2018),
doi: https://doi.org/10.1016/j.biortech.2018.06.051
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Microwave pyrolysis with KOH/NaOH mixture activation: A new approach to produce
Rock Keey Liew a, Elfina Azwar a, Peter Nai Yuh Yek a,b, Xin Yi Lim a, Chin Kui Cheng c,
Jo-Han Ng d, Ahmad Jusoh e, Wei Haur Lam f, Mohd Danial Ibrahim g, Nyuk Ling Ma h, Su
a.
Pyrolysis Technology Research Group, Eastern Corridor Renewable Energy Group, School
Malaysia.
b
School of Engineering and Technology, University College of Technology Sarawak, Lot 88,
Terengganu, Malaysia.
f
State Key Laboratory of Hydraulic Engineering Simulation and Safety, Tianjin University,
Peiyang Park Campus, 135 Yaguan Road, Haihe Education Park, Tianjin, 300350, People’s
Republic of China.
g
h
School of Fundamental Science, Universiti Malaysia Terengganu, 21030 Kuala Nerus,
Terengganu, Malaysia.
1
lrklrk1991@gmail.com, elfina.azwar@gmail.com, peteryeknaiyuh@gmail.com,
lam@umt.edu.my
*
Corresponding author. Tel: +609 6683844; fax: +609 6683991; Email address:
Graphical abstract
Abstract
combining microwave pyrolysis and chemical activation using NaOH/KOH mixture. The
pyrolysis was examined over different chemical impregnation ratio, microwave power,
microwave irradiation time and types of activating agents for the yield, chemical
composition, and porous characteristic of the AC obtained. The AC was then tested for its
feasibility as textile dye adsorbent. About 29 wt% yield of AC was obtained from the banana
peel with low ash and moisture (< 5 wt%), and showed a micro-mesoporous structure with
high BET surface area (< 1038 m2/g) and pore volume (< 0.80 cm3/g), indicating that it can
be utilized as adsorbent to remove dye. Up to 90% adsorption of malachite green dye was
achieved by the AC. Our results indicate that the microwave-activation approach represents a
2
Keywords: Pyrolysis; Microwave; Activated carbon; Activation; Hydroxide mixture
1. Introduction
The global exportation of banana had shown an increment from USD 9 billion to USD
11 billion in 2015 (Workman, 2016), which indicated an increasing world demand for
banana. Consequently, a significant amount of banana peel was generated by household and
food processing industries after consumption. Banana peel is commonly disposed via
landfilling that subsequently releases undesirable landfill gases (e.g. methane and carbon
dioxide) to the atmosphere through microbial decomposition. These gases can absorb heat
energy arising from the earth surface and in turn increase the earth temperature to promote
global warming. Therefore, efforts should be made to mitigate global warming by reducing
the source of these gases, which are derived from the large amount of waste disposed to the
landfill.
inert environment that can produce mainly three types of pyrolysis products: solid char, liquid
oil, and incondensable gas (Lam et al., 2016a; Wan Mahari et al., 2017). In this study,
microwave pyrolysis was used to convert banana peel into useful products. The use of
microwave heating has the advantage of providing a faster and more efficient pyrolysis
process compared to that heated by electrical furnace or oven (Lam et al., 2017b; Wan
Mahari et al., 2016). When the biomass containing microwave absorber (e.g. carbon) was
exposed to microwave energy, heat was rapidly generated and uniformly distributed for
extensive pyrolysis decomposition to occur (Lam et al., 2017a; Lam et al., 2017c; Mushtaq et
al., 2015), hence a relatively short processing time was needed to obtain the desired product.
3
The solid char produced from pyrolysis is of interest due to its multi-functionalities.
The char can be used as a soil amendment to enhance microbial interaction in soil (Visioli et
al., 2016), biofertilizer to culture mushroom (Nam et al., 2018), solid fuel (Liew et al.,
2018b), catalysis (Lam et al., 2015), adsorption of palm oil mill effluent (Lam et al., 2018), or
used as a precursor to produce activated carbon (Chen et al., 2016). Activated carbon is a
highly porous carbon material that is commonly applied as adsorbent in many adsorption
processes, such as removal of organic pollutants (Wang et al., 2017) and adsorption of carbon
dioxide from flue gas and air (Singh et al., 2017). The global market size for activated carbon
was recorded at USD 2 billion in 2012 and forecasted to reach USD 4 billion in 2019.
To produce activated carbon, the raw material (e.g. biomass) is thermally decomposed
through carbonisation – a charring process to convert biomass into char by pyrolysis. Then,
the char is ‘activated’ via physical or chemical activation to increase the char porosity (Liew
et al., 2018a; Yek et al., 2017). Physical activation uses carbon dioxide or steam as activating
agents while chemical activation is performed using chemicals (e.g. alkali metal hydroxides
and carbonates) to produce activated carbon. Chemical activation shows advantages over
physical activation in requiring lower activation temperature (450 – 700 oC) and producing
There were studies reported on the production of activated carbon using chemical
activation coupled with microwave pyrolysis (Nair & Vinu, 2016). Chemicals such as
potassium hydroxide (Sevilla et al., 2017) and zinc chloride were used as the activating agent,
however, there have yet to be studies reported in the literature on the application of a
chemical mixture to produce activated carbon except for the one previously reported by our
team on pyrolysis conversion from orange peel. Our previous study showed that the use of
chemical mixture seemed to have a beneficial effect in increasing the surface area and
4
The above findings provide the motivation for this study, which was performed to
convert banana peel into activated carbon using microwave pyrolysis with emphasis on the
parameters (i.e. microwave power, microwave irradiation time, chemical impregnation ratios
and types of chemical used for activation) on the yield and characteristic of activated carbon
obtained were investigated with the intention to explore the potential of using this pyrolysis
The activated carbon was then evaluated for its feasibility as adsorbent to remove
malachite green dye for potential use in wastewater treatment. MG represents a synthetic dye
that is widely applied as coloring agent in textile industry for production of cotton and wool
products (e.g. clothes and scarf) (Yu et al., 2017). However, the wastewater released from the
textile industry contains residual MG dye that has been reported to be harmful to aquatic
organisms (Zhang et al., 2018). Thus, removal of MG dye from the wastewater should be
Banana peel was collected from a local food stall in Kampung Tok Jembal, Kuala
Terengganu, Malaysia. The peels were rinsed with tap water to remove dirt particles and cut
into smaller pieces with diameter size of 2 cm to facilitate the analysis of thermal behaviour
by thermogravimetric analysis (TGA), otherwise a large sample could decrease the efficiency
of heat transfer from the surface of sample to its core during TGA, resulting in incomplete
pyrolysis of the sample and hence producing inaccurate results from TGA. The peels were
then oven dried at 110 °C for 24 hours. The purpose of drying was to remove the moisture
5
content in order to prevent hydrolysis that would lead to rotting of the banana peel, thus the
2.2 Microwave pyrolysis using hydroxides mixture to convert banana peel into activated
carbon
performed using microwave pyrolysis to produce activated carbon (AC) from banana peel. A
two-step approach comprising carbonization and chemical activation could produce AC with
a higher surface area compared to one-step approach (i.e. carbonization and activation are
simultaneously performed in one process). This is because the majority of volatile matter can
be removed from the banana peel during the first step (i.e. carbonization), and subsequently
led to the formation of pores on the remaining non-volatile components that in turn
transformed into biochar. Then, the use of chemical activation as the second step led to
formation of more pores and also widened the existing pores present on the surface of
biochar, thus producing AC with higher porosity, surface area, and pore volume.
A microwave oven with a frequency of 2.45 GHz (Samsung) was used to perform the
pyrolysis experiment. A custom-made 1 L quartz reactor was used as the pyrolysis reactor. N2
purge-gas was flowed through the reactor to maintain an inert atmosphere A type-K
thermocouple was used to monitor the pyrolysis temperature throughout the experiment. It
was found that the temperature ranged from 800 – 900 oC for carbonization and 400 – 500 oC
for activation. Figure 1 illustrates the set-up of the microwave pyrolysis system used to
produce AC.
Banana peel possesses dielectric loss tangent (tan δ) of 0.375 (Seaman & Seals,
1991), thus indicating it can absorb microwave energy efficiently and convert into heat
energy to undergo carbonisation. Carbonisation was first performed via microwave pyrolysis
to convert banana peel into a char product. 15 g of banana peel was measured and added to
6
the pyrolysis reactor, which was then inserted into the microwave oven. The carbonisation of
banana peel was conducted for 20 minutes at 700 W of microwave power under a continuous
N2 flow of 0.25 L/min. A char yield of approximately 35 wt% was obtained and the char was
then subjected to chemical activation using hydroxides mixture for conversion into AC.
Chemical activation was conducted with chemical impregnation as the first step.
Chemical impregnation ratio is defined as the weight ratio of the hydroxides to the char in
gram basis. For example, 0.5 g of hydroxides was used to soak 1 g of char to produce a
chemical impregnation ratio of 0.5. In this study, 5 g of char was soaked in a solution of
hydroxides mixture over a range of chemical impregnation ratio (0.5, 1.0 and 1.5) for 24
hours. The hydroxides mixture was prepared by dissolving potassium and sodium hydroxides
in distilled water. The char was then filtered from the hydroxides solution and again
subjected to microwave pyrolysis for conversion into AC. The microwave pyrolysis at this
stage was performed over different microwave powers (300 W, 500 W, and 700 W) and
microwave irradiation times (5 min, 10 min, and 15 min) to investigate the effects of these
process parameters on the yield, chemical composition and porous characteristic of the AC
obtained. The resulting AC was immersed in 0.1 M of HCl and then washed with hot distiled
water to remove the chemical residues remained within the AC. The AC was oven-dried at
110 °C for 24 hours and stored in a sample vial for further analysis. The production of AC
was repeated by soaking the char separately with hydroxide solutions of potassium and
sodium, respectively. This was followed by activation via microwave heating at 700 W of
microwave power for 10 minutes to investigate the effects of using different activating
7
(1)
Wf is the weight of AC produced (g) and Wi is the weight of banana peel (g).
The char and activated carbon were characterised for their elemental and proximate
contents, porous characteristics and surface morphology. The proximate contents (moisture
and volatile matter) of samples were obtained using a Mettler Toledo thermogravimetric
analyzer (TGA). The TGA analysis was performed from ambient to 900 °C at a heating rate
of 10 oC/min using N2 at a flow rate of 25 ml/min (Lam et al., 2016b). The sample was
burned in a furnace at 950 °C for 10 minutes to obtain the ash content. The fixed carbon was
calculated by difference (i.e. Fixed carbon = 100 wt% – moisture – volatile matter – ash).
Elemental contents of carbon (C), hydrogen (H), nitrogen (N), and sulfur (S) of sample
were quantified using a FlashEA 1112 CHNS Elemental Analyse, while the oxygen content
The surface morphology of sample was examined using JEOL JSM-6360LA Scanning
Electron Microscope (SEM) at 10 kV of accelerating voltage. The samples were coated with
The porous characteristics of the sample were obtained using ASAP micromeritics
2020 porosimeter. The sample was degassed at 100 °C for 10 hours with 10 oC/min of ramp
experiment was then performed using liquid nitrogen at -196 °C to obtain the N2 adsorption-
desorption isotherm. The isotherm obtained was used to calculate BET surface area (SBET)
and estimate the total pore volume (Vt) at a relative pressure of 0.98. The average pore size of
the sample was estimated using Barrett-Joyner-Halenda (BJH) desorption method. The
8
micropore volume (Vmic) was determined by the t-plot method, whereas the mesopore volume
(Vmeso) was calculated by difference (Mesopore volume (cm3/g) = Total pore volume –
micropore volume).
The AC was also tested for its performance to adsorb malachite green (MG). The
AC and 100 ml of MG aqueous solution with an initial concentration of 10 mg/L. The use of
a low concentration of MG solution (10 mg/L) to perform the adsorption experiment was
deemed sufficient to evaluate the adsorption performance of the AC produced as has been
performed and reported by Jalil et al. (2012). The beaker added with AC and MG solution
was agitated at room temperature at a mixer speed of 150 rpm for 10 mins to ensure the AC
was mixed thoroughly with the MG solution (Santhi et al., 2016). 10 mins of contact time
was selected according to the actual practice in wastewater treatment by the relevant industry
(e.g. < 10 mins of contact time). However, it should be mentioned that the contact time
between AC and adsorbates could vary in different wastewater treatment plants depending on
the plant design, amount of AC used, and flow rate of wastewater towards AC.
The MG solution was then filtered by filter paper (Whatman No. 1, diamater 25 mm) in
order to separate AC from the MG solution and the residual concentration of MG was
2018). The adsorption efficiency of MG by the activated carbon was calculated using
equation (2) whereas the removal percentage of MG dye was calculated using equation (3).
(2)
9
where qe (mg/g) = adsorption efficiency of activated carbon; C0 (mg/L) = initial concentration
(3)
The influence of microwave to the banana peel could be explained by the interaction
between microwave radiation and the microwave absorbent material (e.g. carbon-containing
material such as biomass) (Lam et al., 2017a). Microwave radiation offers selective heating
the conventional heating that usually heated by an electrical furnace, the heating mechanism
shown by conventional heating is non-selective where the heat energy targets everything
within the chamber of the furnace. Banana peel (biomass material) represents a microwave
absorbent material that can absorb microwave energy and convert into heat energy within the
When the banana peel was exposed to microwave radiation, the microwave would
induce the polarization effect on the chemical bonds (e.g. covalent bond) of the
lignocellulosic components (cellulose, hemicellulose and lignin) present within the banana
peel and as a result the lignocellulosic components would undergo molecular oscillation (e.g.
bending and stretching). This oscillation would occur at the rate of super high frequency (up
10
to million times per second). Then, substantial heat energy would be generated from the rapid
oscillation motions resulted from the strong frictional force between the oscillating
molecules. As a result, the heat energy generated would have led to the cracking of
lignocellulosic components into volatiles and the carbonization of the remaining non-volatile
component of the banana peel. The non-volatile component of the banana peel would then
turn into biochar after carbonization and the liberation of the volatiles would create pores on
During the subsequent step of chemical activation performed on the biochar, the
interaction between microwave radiation and the chemical impregnated on the biochar (e.g.
sodium and potassium hydroxides) would further lead to the formation of new pores and
widen the existing pores, thus producing AC with high porosity, surface area and pore
volume. This could be due to the intercalation effect of the energized alkali metal atom in
creating more pores on the biochar after the alkali metal (e.g. K and Na) has been exposed to
microwave radiation; the activation mechanism is presented and discussed in Section 3.3.2.
The effects of microwave radiation on the production of AC were further discussed in the
following sections with respect to the yield, chemical compositions, and porous
characteristics of AC obtained.
wt% yield of AC was obtained from the banana peel char via this microwave pyrolysis
approach. It was found that the yield of AC produced was inversely proportional to the
microwave power and irradiation time where lower yield was obtained at higher microwave
power and longer irradiation time. This could be explained by the release of more volatile
11
matter during the activation stage of char at a higher microwave power and longer irradiation
time (Liu et al., 2010). When higher microwave power was used or the pyrolysis process was
performed at a longer irradiation time, the carbon elements present in the char, being a good
microwave absorbent, would absorb more microwave energy. The higher amount of
microwave energy then induced dipole rotation of carbon molecules (present in the char) at
the rate of million times per second. This rapid rotation of carbon molecules within the char
in turn produced frictional force and released more heat energy within the char itself which in
turn improved the pyrolysis cracking of char and released more volatile matter (Lam et al.,
2017a). As a result, lower yield of AC was obtained due to the release of higher amount of
volatile matter from the char (which then transformed into AC). Figure 3 illustrates the
mechanism of pyrolysis cracking derived from the heat generated from the dipole rotation of
Lower yield of AC (19 wt%) was obtained from a higher chemical impregnation ratio
(1.5). This indicates that the use of a higher amount of alkali metal hydroxides solution to
impregnate the char facilitated the removal of more volatile components from the char during
the subsequent microwave pyrolysis treatment. When higher amount of the chemical was
used, more alkali hydroxides molecules were available to break the chemical bonds such as
the alkyl-aryl bonds present within the char matrix (Demirbas, 2004). This in turn enhanced
the removal of some carbon components in the form of volatiles (e.g. CH 4, CO2 or CO)
during the subsequent thermal activation using microwave pyrolysis. Hence, the higher
chemical impregnation ratio resulted in the lower conversion of char into AC.
The yield of AC was also found to be influenced by the types of activating chemical
used. It was reported that KOH-activation produced AC in powder form while NaOH-
activation generated AC in granular form (Xu et al., 2008). The AC produced via KOH-
activation in this study was also in powder form and it showed the lowest yield (22 wt%) as
12
compared to that obtained by other types of activating chemicals. This was probably caused
by the unintended loss of AC during the washing step after activation since some of the AC
obtained in powder form were washed out in this step. In contrast, the AC obtained via
NaOH-activation was in granular form and it showed the highest yield (25 wt%) whereas the
According to the basicity strength of alkali metal hydroxides, KOH is more alkaline
than NaOH when dissolved in water due to the lower ionisation energy of potassium (K)
atom compared to sodium (Na) atom. Lower ionization energy indicates a weaker strength of
the ionic bond between a metal atom (i.e. K) and hydroxyl ion (OH-), thus the bond can be
easily broken when dissolved in water to form an aqueous solution, thus resulting in the
release of more hydroxyl (OH-) ions in the aqueous solution of KOH. These hydroxyl ions
were likely to have attacked and weakened the chemical bonds present within the char matrix
(e.g. the covalent bond between the monomer units such as ether bond (–C–O–C–) of
impregnated char matrix was more likely to be converted into AC with simpler
lignocellulosic dimer/polymer units by releasing more volatile matter from the breaking of
the weak chemical bonds in the char matrix during the subsequent microwave pyrolysis
treatment.
3.3 Analysis and characterization of feedstock (banana peel) and pyrolysis product
(char, AC)
Table 2 shows the elemental and proximate contents of banana peel, char, and AC. The
elemental contents of all samples contained mainly carbon (48.0–89.0 wt%) and oxygen
(10.2–45.0 wt%) followed by small amounts of hydrogen (0.7–6.0 wt%) and nitrogen (0.1–
13
2.0 wt%). Sulfur was not detected probably because the sulfur content was too low to be
detected by the elemental analyser. Proximate analysis of all samples showed that volatile
matter (8.8–55.0 wt%) and fixed carbon (34.0–83.5 wt%) represented the major contents
followed by small amounts of moisture (1.2–10.0 wt%) and ash (2.9–5.5 wt%). The ash
content of the AC produced (2.9–5.0 wt%) was within the commercially acceptable value (<
5 wt%) and consistent with the range of ash content from banana peel and char (4.0-5.5 wt
%), suggesting that the ash derived from chemical activating agent residues was removed
during washing step. These properties are important since higher ash content (> 5 wt%) could
have catalytic effect that can lead to undesired reaction (e.g. catalytic cracking reactions
between metal oxides in the ash with the other compounds in the AC) occurred during the
high temperature regeneration process (700–900 oC) of the used activated carbon (Dizbay-
Onat et al., 2017). The porous structure of the AC could be destroyed by the undesired
reactions and this could lead to reduction of the adsorption sites available. The presence of
ash could also induce corrosion on the reactor heating surface which eventually reduce the
Banana peel showed high contents of carbon (48 wt%) and fixed carbon (34 wt%),
indicating its feasibility to be recovered as a carbon-dense product such as char and activated
carbon. The carbon content of char was increased while the oxygen and hydrogen contents
were decreased after carbonisation of banana peel. It was reported that the banana peel
contained 67.5 wt% of cellulose, 23.7 wt% of hemicellulose and 8.8 wt% of lignin (Agama-
decompose via a few chemical reactions (e.g. dehydration, carbon rearrangement, and
breaking of alkyl-aryl linkages) to release water (H2O), methane (CH4), hydrogen (H2),
carbon monoxide (CO) and carbon dioxide (CO2) molecules (Asmadi et al., 2011; Cao et al.,
14
2013; Wang et al., 2009), thus producing char with higher content of fixed carbon (non-
volatile) and lower content of oxygen and hydrogen (Foo & Hameed, 2012).
It was observed that the carbon and fixed carbon of the AC produced were increased
at a higher chemical impregnation ratio, microwave power and microwave irradiation time
(Table 2). In contrast, the oxygenated contents (oxygen and volatile matter) were decreased.
When a higher chemical impregnation ratio was used, the oxygen-containing chemical bonds
(e.g. C-O and -COOH) present within the char matrix were likely to be weakened by the
concentrated hydroxyl ions (-OH-) during the chemical impregnation stage. This in turn
facilitated the release of oxygenated compounds such as CO2, CO and carboxylic acid (-
COOH) during the subsequent microwave pyrolysis treatment. Although the release of CO2,
CO and carboxylic acid (COOH) may reduce some amounts of carbon element, the carbon
content within AC is still higher than oxygen content, considering that the amount of carbon
element released is lower than oxygen element. Interestingly, the hydrogen content was
increased from 1.6 wt% to 2.3 wt% when higher chemical impregnation ratio was used,
suggesting that hydrogenation (addition of hydrogen atoms) occurred during the microwave
pyrolysis treatment where the hydrogen was probably derived from the activating chemical
solution or the char itself. The hydrogen atoms present on the surface of AC could potentially
act as adsorption sites for polar substances, suggesting its potential to be used in the
separation process of polar and nonpolar molecules in both solution or gases mixtures
AC. At higher microwave power (i.e. 700 W), the banana peel char, containing carbon
(which is a good microwave absorber material), was exposed to more microwave radiation
and thus absorbing more microwave energy. The absorbance of more microwave energy was
likely to have induced and increased the dipole rotation of the carbon atoms present within
15
the char matrix at a super high frequency (i.e. up to million times per second) (Figure 3). As a
result, more heat energy were generated that led to extensive decomposition of the char
matrix, particularly the oxygenated fractions, leading to the increased release of these
The banana peel char was likely to comprise complex polymeric compounds with
unsaturated carbon–carbon double bonds (Neutelings, 2011), alkyl-aryl linkage (e.g. carbon–
carbon single bond), and carbon–oxygen bond (Collard & Blin, 2014). The use of higher
microwave power (700 W) had provided enough energy (approximately 420 kJ, i.e. 700 W x
600 s/1000) to break the chemical bond between carbon and oxygen that has the bond energy
of 360 kJ (Benson, 1965). This converted some of the oxygenated compounds originally
present in the char into smaller compounds in the form of volatiles, leading to the decrease of
the oxygen element in the resulted AC. The bond energy (BE) measures the amount of energy
needed to break the chemical bond. Moreover, 700 W of microwave power could also
produce enough energy to break the carbon–carbon single bond (BE = 350 kJ) and this
probably had promoted the rearrangement reaction of the carbon atoms to form a more
complex polycyclic structure (Collard & Blin, 2014). Combined with the presence of
compounds with carbon–carbon double bond (BE = 600 kJ) in the char that cannot be broken,
the carbon elements were concentrated and preserved in the final form of AC. This explains
the production of AC (BP 700) with higher contents of carbon (82 wt%) and fixed carbon (78
wt%) at higher microwave power as compared to that obtained at lower microwave power
time. The longer exposure to microwave energy was likely to have promoted several
reactions to the cellulose and hemicellulose of banana peel char, such as dehydration into
16
(Van de Velden et al., 2010). As a result, AC with lower volatile matters was produced after
the release of these compounds (i.e. water, anhydrosugars, carbonyl compounds) from the
banana peel char. Moreover, the hydrogen content was decreased from 1.8 wt% to 0.7 wt%
when the microwave irradiation time was increased from 5 to 15 mins. Longer microwave
irradiation time seemed to have promoted reactions to convert banana peel char into AC with
more unsaturated polycyclic carbon structure. The longer exposure to microwave radiation
(i.e. 15 mins) on the char matrix would have created enough heat energy to induce the
conversion of large compounds of banana peel char at high temperature (i.e. > 500 oC)
(Collard & Blin, 2014). The C-H bond present in the saturated carbon structure would be
broken and form a new C-C bond by releasing H2 gas which subsequently produce
The use of different chemical activating agents showed effects to the chemical
compositions of the AC obtained. It was generally found that AC with high contents of
carbon (≥ 70 wt%) and fixed carbon (≥ 73 wt%) can be obtained from the use of NaOH,
KOH, and the hydroxides mixture as the activating agents. The AC obtained also showed a
high BET surface area (≥ 985 m2/g). In particular, the AC produced from the hydroxides
mixture (BPNaK) showed the lowest moisture content (4.0 wt%). AC with low moisture
content can provide more adsorption sites available for use as an adsorbent. Otherwise, the
moisture would have blocked the adsorption sites of the AC, thus decreasing its adsorption
efficiency. Our results indicate that the use of microwave pyrolysis with hydroxides mixture
showed potential to produce AC with desired properties comprising high carbon content, high
17
The porous characteristics of the banana peel char and the AC produced from the char
to its precursor material (i.e. banana peel char) after chemical activation. The AC was
detected with a BET surface area ranging from 320 m2/g–1130 m2/g, total pore volume of
0.20 cm3/g–0.80 cm3/g and an average pore size (8 nm–34 nm) that is within the range of a
mesoporous material (i.e. 2–50 nm). In addition, most of the AC produced (except BPK)
contained mainly mesopores as indicated from their higher mesopore volumes (0.13 cm3/g–
0.52 cm3/g) compared to micropore volume. The results showed that the use of hydroxides
It was observed that the porous characteristics of the AC obtained were significantly
affected by different process parameters. When the chemical impregnation ratio was
increased from 0.5 to 1.0, the BET surface area was increased. This indicates that the increase
of the concentration of activating chemical had facilitated the development of new pores or
widened the existing pores present on the surface of the AC, thus resulting in the increased
surface area. However, further increasing the chemical impregnation ratio to 1.5 had caused
the decrease in surface area. The concentration of the activating chemical at this ratio was
found to be too high and could over-react with the carbon structure and resulted in the
destruction of the pores; similar observation was reported by Foo and Hameed (2012). Thus,
a chemical impregnation ratio of 1.0 in this study represents the optimum ratio for chemical
The effects of microwave power and microwave irradiation time on the BET surface
area and total pore volume of AC obtained were different. For microwave power, both
surface area and pore volume were increased when a higher microwave power was applied
during the thermal activation. At higher microwave power (e.g. 700 W), increased intensity
of microwave energy was radiated to the impregnated char that in turn induced the generation
18
of heat energy within the char matrix. This heat energy was likely to have caused the
expansion of the small pores within the char via gasification reaction that was reported to
commonly occur during the pyrolysis process (Foo & Hameed, 2012), hence increasing the
total pore volume of the AC. In addition, the heat energy could be absorbed by the alkali
metal atoms (i.e. Na and K) from char matrix and became energised atoms (i.e. Na* and K*)
to form new pores on the surface of the AC via intercalation (Lam et al., 2017b). During the
intercalation process, the energised metal atoms could insert or migrate into the carbon
structure of the AC to form pores on the surface and thus increase the surface area and total
The use of different microwave irradiation time was found to have effects on the
surface area and pore volume of the AC produced. Higher surface area (1035 m2/g) and pore
volume (0.68 cm3/g) were detected from the AC produced at microwave irradiation time of
10 mins. However, the surface area and pore volume were decreased when the microwave
irradiation time was increased further to 15 mins. The prolonging of microwave heating on
the char would have promoted further decomposition and cracking of char into volatiles,
leading to the destruction of the existing pores (Xin-Hui et al., 2011). This explains the
decrease in surface area and pore volume obtained at a longer microwave irradiation time
(beyond 10 mins). It was also found that a shorter process time (< 15mins) was required to
produce activated carbon using microwave pyrolysis as compared to that required by the
The effects from using a hydroxide mixture on the porous characteristics obtained
were compared with that obtained from using a single hydroxide on its own (i.e. NaOH and
KOH respectively). It has been reported that KOH-activation could produce microporous AC
2013). It was hypothesised that AC with hybrid properties (i.e. containing both micropores
19
and mesopores) could be produced from the use of hydroxide mixture. The results obtained
concurred to this hypothesis where the BPNaK was detected with a considerable volume of
both micropores (0.28 cm3/g) and mesopores (0.45 cm3/g). In contrast, the BPK contained
mainly micropores (0.70 cm3/g) while BPNa was detected with mesopores in majority (0.52
cm3/g). Our results indicate that AC with desired porous characteristics could be produced by
with the physical characteristics (e.g. electronegativity and specific heat capacity) of alkali
metal atoms (e.g. K and Na). A reaction mechanism associated with the physical
characteristics of the alkali metal could account for the production of microporous or
mesoporous AC. It has been reported that microporous AC was usually produced from KOH-
(Sirimuangjinda et al., 2013). When hydroxide mixture was used as an activating agent, the
+
alkali metal hydroxide molecule (KOH and NaOH) would be dissociated into cations (K and
Na+) and hydroxyl anions (OH-) when dissolved in water. The K+ and Na+ cations would then
be solvated by the water molecules and formed solvated complexes. During the chemical
-
impregnation of banana peel char, the hydroxyl anion (OH ) was likely have loosely bound to
the carbon surface of the char by van de Waals forces to form a negatively charged carbon-
hydroxyl surface. Then, the potassium and sodium-solvated complexes with positive charges
Subsequently, intercalation was likely to happen during microwave pyrolysis where the
solvated complex with positive charges then inserted or migrated into the carbon structure of
the AC to form micropores or mesopores on the surface of the resulted AC (i.e. BPNaK). The
results obtained in this study on porous characteristics (Table 3) concur with this activation
mechanism where the BPNaK was detected with a considerable volume of both micropores
20
(0.28 cm3/g) and mesopores (0.45 cm3/g) rather than consisting mainly (e.g. > 85%) of either
micropores or mesopores; this helps to explain the formation of both types of pores by the use
of hydroxide mixture.
The pore size of the resulted AC could be related to the molecular size of the solvated
complex which depends on the electronegativity of the cation. For example, sodium (0.93)
has a higher electronegativity than potassium (0.82). Thus, the molecular size of solvated
sodium complex is larger than the solvated potassium complex, allowing it to form larger
pores on the resulted AC. The formation of pores could be initiated when the solvated sodium
complex received heat energy derived from microwave radiation. The resulting energised
solvated sodium complex, containing higher heat energy than that contained in potassium
complex (due to the higher specific heat capacity of sodium (1228 J/kgK for sodium and 757
J/kgK for potassium)), could cause more vigorous motions (e.g. translational motion and
rotational motion) on the char surface. As a result, the energised sodium complex could
migrate more into the carbon structure of the char and create a larger pore than the potassium
Irregular shapes and sizes of pores were observed on the surface of the AC produced under
different process parameters. The surface porosity of the AC was increased when the
chemical impregnation ratio was increased from 0.5 to 1.5. However, cracks were observed
on the surface of BP1.5 which corroborates with its lower BET surface area and total pore
volume (See Table 3) as compared to BP1.0, indicating that the concentration of the chemical
activating agent used was too high. Hence, a chemical impregnation ratio of 1.0 was found
suitable to produce AC with high surface area and pore volume in this study.
21
With respect to the effects of microwave power, well-developed pores were observed
from the AC produced at 500 W and 700 W of microwave power (i.e. BP500 and BP700
respectively). Fewer pores were shown on the surface of BP300, thus indicated that 300 W of
microwave power was insufficient to induce enough heat energy for the solvated
sodium/potassium complex to be migrated into the carbon structure to form pores. This also
concurs with the low BET surface area (320 m2/g) and total pore volume (0.20 cm3/g)
detected. Thus, a minimum microwave power of 500 W was required to induce enough heat
Microwave irradiation time also significantly affected the development of pores on the
surface of AC. At 5 mins of microwave irradiation time, pores with irregular shapes and sizes
were formed on the surface. When the microwave irradiation time was increased to 10 mins,
the existing pores were enlarged and new pores were formed on the surface. This was
probably because the longer exposure to microwave radiation has caused more heating to the
banana peel char, thus promoting the decomposition of the remaining volatile fraction present
within the char matrix. As a result, more volatile matter were released and this resulted in
more void space (pores) formed on the surface of AC. Nevertheless, the pores observed from
BP15 were deformed and ruptured, which suggested that 15 mins of microwave irradiation
time was too long and was likely to have provided an excessive heat energy for pores
destruction.
chemical activating agents. It was observed that the pores of BPNa showed larger pore size as
compared to BPK, whereas the AC produced from the use of hydroxide mixture (BPNaK)
contained both small pores (micropores) and larger pores (mesopores), and the micropores
were also observed to have formed within the mesopores. The production of BPNaK with
considerable volumes of both micropores (0.28 cm3/g) and mesopores (0.45 cm3/g)
22
demonstrated that the use of hydroxide mixture has the ability to produce an AC with
improved porous characteristics where both micropores and mesopores would be available to
act as adsorption sites for use as adsorbent. Combined with the low content of moisture (4
wt%) and ash (3.8 wt%), BPNaK shows potential to be used in wider applications,
considering that an AC with high moisture and ash content could have moisture and ash
blocking the adsorption sites and reduce the functionality of the AC. Thus, BPNaK was
selected and further tested for its performance as a dye adsorbent; the results are presented
Table 4 shows the results obtained when different amounts of BPNaK (0.05–0.20 g)
were tested for adsorption of malachite green (MG) - a synthetic dye commonly present in
wastewater released from textile industry. The adsorption efficiency of BPNaK on MG dye
was found to range from 10.6 to 22.5 mg/g with the removal percentage ranging from 45 to
90%.
It was observed that the adsorption efficiency and removal percentage of of MG dye
were increased with the increasing amount of BPNaK (0.05 g to 0.25 g). This could be due to
the availability of more adsorption sites for the MG dye to be adsorbed onto when higher
amount of BPNaK was used, thus resulting in higher adsorption efficiency and removal
percentage obtained. Similar trend was reported in other literature where higher adsorption
efficiency was achieved with the use of higher amount of adsorbent (Nekouei et al., 2016). In
addition, it was also suggested from the results that a minimum amount of adsorbent (i.e. 0.25
The activated carbon adsorbed with MG can be collected and stored in a container for
regeneration. It can be regenerated via thermal or chemical method. For thermal method, the
23
spent AC can be heated at 300 oC for 1 hour using microwave heating in order to desorb the
MG molecules from the AC surface. For chemical method, a mixture of 5% acetic acid and
methanol could be used in the desorption process of MG from AC (Altıntıg et al., 2018).
Table 5 shows the comparison of some process features and energy consumption of
microwave pyrolysis performed in this study to other pyrolysis methods that produced
activated carbon using conventional heating source. It was found that microwave pyrolysis
requires a relatively shorter process time to perform both carbonization and activation (i.e. 35
min) over the one reported using conventional pyrolysis (90 – 300 min). In addition, the
estimated energy consumption for microwave pyrolysis (1470 kJ) was found to be about
three times lower than that required for conventional pyrolysis (4320 – 77400 kJ). This
indicates that microwave pyrolysis represents a potentially time-saving approach that requires
lower energy consumption due to the need of a shorter process time, thus lower production
Table 6 shows the estimated production cost of AC by the microwave pyrolysis coupled
with hydroxide mixture approach to allow a simple evaluation of its economic feasibility. The
estimation was based on the cost incurred by the feedstock, transportation, chemicals
(hydroxides mixture and hydrochloric acid), N2 gas, and the electricity used by the pyrolysis
method in producing the AC. The production cost was estimated to be about USD 0.90 / kg
of AC, which is significantly lower than the market price of AC (up to USD 5.63 / kg of AC)
and also the production cost (USD 1.67 / kg of AC) reported by Selvaraju and Bakar (2017).
This can be a good indication that the microwave pyrolysis coupled with hydroxide mixture
approach contributes to the economic feasibility of this approach and shows potential to be
24
4. Conclusion
Activated carbon with high BET surface area, total pore volume, carbon and fixed
carbon contents, i.e BPNaK, was produced using hydroxide mixture as a chemical activating
agent over a chemical impregnation ratio of 1.0, 700 W of microwave power, and 10 mins of
microwave irradiation time. The BPNaK showed a micro-mesoporous surface (i.e. small
pores presence on large pores) with a high removal percentage (up to 90%) on malachite
green dye. Our results demonstrated that the use of microwave pyrolysis combining with
Acknowledgements
The authors acknowledge the financial support by the Universiti Malaysia Terengganu to
E-Supplementary data
E-supplementary data of this work can be found in online version of the paper.
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28
Table 1 Process parameters in AC production .
29
Table 2 Elemental and proximate contents of banana peel, char and activated carbon (wt%)
30
Table 3 Porous characteristic of banana peel char and activated carbon
31
Table 4 Adsorption performance of malachite green by BPNaK
32
Table 5 Comparison of process features and energy consumption
Properties This study Other study
Total process time (min) – carbonization 35 min 90 min (Ahmed et al., 2017)
& activation 180 min (Pandiarajan et al., 2018)
300 min (Peng et al., 2018)
Heating source Microwave Conventional heating (i.e. muffle
heating furnace, tubular furnace)
33
Table 6 Estimated production cost of AC
34
Figure 1 Schematic layout of microwave pyrolysis system.
35
Figure 2 Effects of process parameters on the yield of activated carbon. (BP300, 500, 700 =
AC produced under different microwave power (300–700 W); BP5, 10, 15 = AC produced
under different microwave irradiation time (5–15 mins); BP0.5, 1.0, 1.5 = AC obtained from
different chemical impregnation ratio (0.5–1.0); BPNa, BPK, BPNaK = AC produced from
36
Figure 3 Pyrolysis cracking derived from the heat generated from the dipole rotation of
37
Highlights:
Activated carbon (AC) was produced by microwave pyrolysis with hydroxide mixture.
Four process parameters were examined for the yield and properties of AC produced.
AC showed micro-mesoporous structure with high surface area and pore volume.
38