Journal of the Energy Institute 93 (2020) 1819e1832

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Journal of the Energy Institute

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Microwave pyrolysis of polystyrene and polypropylene mixtures using

different activated carbon from biomass
Prathiba Rex, Immanuvel Palies Masilamani, Lima Rose Miranda*
Department of Chemical Engineering, A. C. College of Technology, Anna University, Sardar Patel Road, Chennai, 600 025, India

a r t i c l e i n f o a b s t r a c t

Article history: In this study, microwave pyrolysis was experimented with mixed types of plastic waste. Two different
Received 22 October 2019 plastic wastes polystyrene waste (PSW) and polypropylene waste (PPW) were used as feedstock. Carbon
Received in revised form and activated carbon were synthesized from different biomass; rice husk (RH), corn husk (CH) and co-
16 March 2020
conut sheath (CS) respectively which are used as microwave susceptors. The effect of impregnation on
Accepted 23 March 2020
product yields was studied. Microwave pyrolysis at 900 W and with a polymer to an absorbent ratio of
Available online 2 April 2020
10:1, produced the highest oil yield of 84.30 wt% when coconut sheath activated carbon (CSAC) was used
as an absorbent. The reaction time was 10 min for the complete decomposition of polymer mixtures. Oil
Keywords:
Microwave pyrolysis
properties were determined and a high calorific value of 46.87 MJ kg
1 was obtained. These properties
Mixed plastic waste were compared to conventional fuel properties and the product oil has a density of 0.76 g ml
1 and
Activated carbon viscosity of 2.4 cSt which is an equivalent fraction obtained to that of gasoline. Product oil has a styrene
Rice husk recovery of 67.58% from microwave pyrolysis. The results demonstrate that, microwave pyrolysis has a
Corn husk great potential for energy recovery from mixed plastic waste and the use of agricultural residues as
Coconut sheath absorbents enhanced the production efficiency of the process.
© 2020 Energy Institute. Published by Elsevier Ltd. All rights reserved.

1. Introduction waste using HZSM-5 zeolite as catalyst was studied by Sebestye n

Plastics are in high demand for various sectors like packaging,
household storage and automotive parts to building construction.
Hence, plastics usage has increased the amount of plastic waste
deposited in disposal sites. The plastic waste which is accumulated
should be methodologically addressed. Pyrolysis is one technique
where plastic waste is heated in the absence of air to recover the
valuable hydrocarbons leading to fuel production. Currently, a
number of studies have emphasized the pyrolysis of mixed types of
plastics, which feature in the real world of plastic waste. Plastics
like; household packaging and water container can be effectively
converted to gasoline range of hydrocarbons by pyrolysis method
[1]. Complex plastic mixtures like polystyrene, polypropylene, and
polyethylene were studied by Lo pez et al. [2] with ZSM-5 and red
mud as a catalyst; in which ZSM-5 has a strong effect on the
characteristics and distribution of pyrolysis products.
Feedstock types strongly affect the product yields moreover; the
solid product obtained from a complex plastic mixture has a higher
heating value (HHV) when compared to low-rank coal [3]. Hin-
dering effect of cellulose and beech milled wood lignin in plastic
* Corresponding author.
E-mail address: limamiranda2007@gmail.com (L.R. Miranda).
et al. [4], in which the biomass hinders the catalytic activity
resulting in a lower yield of aromatic products. Kalargaris et al. [5]
experimented on the usability of plastic oil in diesel engines, it was
noted that the plastic oil had similar characteristics as that of diesel
fuel. The pyrolysis method has significant advantages in the con-
version of waste plastics into valuable products. But some factors
like a higher amount of energy consumption and reaction time are
to be considered during the process. To overcome these factors,
microwave pyrolysis method can be employed as an effective
heating source in the treatment of waste and environmental
remediation [6]. Microwave pyrolysis is used because it rapidly
heats the materials hence by microwave pyrolysis method plastic
waste management will become more effective thereby reducing
pollution and landfill capacity [7]. Moreover, microwave pyrolysis
will enhance the product yields with lesser reaction time and
temperature [8]. Dielectric properties are important in the deter-
mination of heating characteristics of materials in microwave py-
rolysis reactions [9].
The waste polyolefins can be experimented in microwave-
assisted pyrolysis which can yield liquid products that may be
used as a source of chemicals or fuel without any preliminary
treatments [10]. Microwave pyrolysis of plastic waste offers a
volumetric heating procedure in industrial scale for the conversion

https://doi.org/10.1016/j.joei.2020.03.013
1743-9671/© 2020 Energy Institute. Published by Elsevier Ltd. All rights reserved.
1820 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832
of waste plastics into valuable commercial products [11]. The
product oil from microwave pyrolysis on further distillation will
yield low sulfur naphtha and diesel. This process has the potential
to reduce the menace of plastic waste and the production of valu-
able fuel [12]. Two types of catalyst NiO and HY zeolites were used
in microwave pyrolysis of polyethylene, in which the liquid yield
was 56.5 wt% and comprised of gasoline range hydrocarbons [13].
Activated carbon as a susceptor in microwave pyrolysis of tire
increased the pyrolysis temperature to 500  C, thereby enhanced
fuel production [14]. Moreover, the char from the microwave py-
rolysis has a heating value of 30 MJ kg
1 [15]. The effectiveness of
different microwave absorbents such as graphite, activated carbon,
silicon carbide and flyash was extensively studied to recover the
useful products from the synthetic polymer using microwave py-
rolysis, in which 100:1 wt/wt. of polypropylene:graphite produced
48 wt% of product oil, the composition of oil consists of alkenes and
cycloalkanes [16]. Microwave-assisted pyrolysis of polyethylene
was studied using two different types of absorbents such as con-
ventional coke and activated carbon [17]. In which, activated carbon
produced oil equivalent to diesel and petrol. Extensive cracking of
used frying oil (UFO) was examined when particulate carbon and
activated carbon were used as absorbents. The studies showed that
energy consumption and reaction time was reduced [18]. Carbon
absorbent in microwave pyrolysis of oil palm shell improved the
process of heating and selectivity of products [19]. The use of SiC
(silicon carbide) as microwave absorbent enhanced the liquid yield
and carbon yield, in microwave-assisted pyrolysis of plastic films
and dried grains. The increase in liquid yield was attributed to the
increase in temperature of 650  C [20]. Iron was also used as mi-
crowave absorbent to pyrolyze the waste plastics from electric and
electronic equipments, the studies showed that the reaction time
was 60 min to produce a liquid yield of 76.6 wt% and a solid residue
of 21.2 wt% [21]. 66% of styrene was recovered by the use of tire
powder as microwave absorber, the microwave pyrolysis of poly-
styrene also resulted in liquid product with low viscosity [22].
These studies demonstrated the use of different absorbents in mi-
crowave pyrolysis; however, it is essential to explore different
carbon absorbents that can be used in the microwave pyrolysis
method. This study intends to experiment the potential use of
different activated carbons synthesized from agricultural residues
and a detailed material characterization was comprehensively
studied. This work is also important to accelerate waste plastic
recycling and it unfolds the platform to produce gasoline range
hydrocarbons.
The aim of this study is to microwave pyrolyze polypropylene
and polystyrene waste mixtures. Also, synthesize carbon and acti-
vated carbon from biomass which is used as an absorbent for mi-
crowave pyrolysis of polymer mixtures. Biomass materials are rice
husk, corn husk and coconut sheath which are agricultural resi-
dues. This is one of the novel methods to microwave pyrolysis
polymer mixtures with different absorbents. This study also ex-
plores the distinguishable properties of carbon and activated car-
bon in microwave pyrolysis of polymer mixtures. The effects of
activated carbon to polymer ratio were also studied for the
augmentation in fuel production, as well as the time needed for
complete pyrolysis of the polymer mixtures. The product oil was
ascertained for its suitability as an alternative for conventional fuel.
2. Experimental methods
2.1. Materials
The polystyrene waste (PSW) comprises of compact disc (CD)
cases and plastic rulers. Polypropylene waste (PPW) is used plastic
syringes obtained from S.V.S plastics, Chennai, India. The size of the
PSW is approximately 0.5 cm and PPW is approximately 0.3 cm.
PSW and PPW were washed, shredded and used as sample material.
The precursor rice husk was collected from Villupuram, Tamilnadu,
cornhusk was collected from Chennai, Tamilnadu and coconut
sheath was collected from Nagercoil, Tamilnadu. Sodium carbonate
and orthophosphoric acid (85%) were purchased from Sisco
research laboratories (SRL). The chemicals are of analytical grade.
The solutions were prepared using distilled water.
2.2. Preparation of carbon
200g of each biomass (rice husk, corn husk, and coconut sheath)
was cleaned and washed separately using distilled water. They
were dried in a hot air oven. After drying, the husks were placed in a
silica crucible and carbonized at a temperature of 500  C for 5 h in a
muffle furnace. The carbons thus obtained were called as rice husk
carbon [RHC], corn husk carbon [CHC] and coconut sheath carbon
[CSC] and were used as an absorbent in the microwave pyrolysis.
2.3. Preparation of activated carbon
The activated carbon (AC) from biomass rice husk (RH), corn
husk (CH) and coconut sheath (CS) was prepared by chemical
activation method using orthophosphoric acid as the activating
agent with an impregnation ratio of 1:2. The biomass was soaked
for 24 h in orthophosphoric acid. The mixture was dried at 110  C
for 1.5 h and then transferred to a sealed ceramic container. The
mixture was then placed in a muffle furnace at 400  C for 1 h [23].
The activated carbons were repeatedly washed with distilled water
and then with sodium carbonate solution (0.1 N) to remove the
residual acid content. The activated carbons thus obtained were
named as rice husk activated carbon (RHAC), cornhusk activated
carbon (CHAC) and coconut sheath activated carbon (CSAC).
2.4. Characterisation of carbon and activated carbon
The synthesized carbon and activated carbon materials were
characterized using Fourier transform spectroscopy (FTIR) to
determine the functional groups present in it. Surface morphology
of the material was examined using Quanta 200 FEG scanning
electron microscope (HRSEM) with high resolution of 1.2 nm and
magnification range of minimum 12 X to 1,00,000 X. The elements
present in the materials were determined using energy dispersive
x-ray spectrometry (EDX). Porosimetric measurements such as
pore volume, pore size and BET surface area were determined using
micrometrics ASAP 2020 porosimeter. The samples were degassed
at 200  C.
2.5. Microwave pyrolysis experiments
Fig. 1 shows the microwave pyrolysis experiment set up with an
output power of 900W. A borosilicate quartz flask of 250 ml holds
the material inside the microwave oven. A borosilicate adaptor was
used to connect the quartz flask to the condenser (1) the quartz
flask was insulated with glass wool to avoid heat loss. The joints are
tightly sealed using Teflon tape, to avoid the escape of non-
condensable gases. The non-condensable gases were condensed
by two-stage condensation units at ambient temperature. The re-
action vessel, condenser, and the adaptor were weighed before and
after the experiments. Microwave pyrolysis is an effective method
to convert waste plastics to product oil. Initially, the microwave
pyrolysis experiments were investigated at different microwave
power such as 180 W, 360 W, 540 W and 720 W. 2g of carbon and
10 g of the plastic waste were experimented. The reaction time was
maintained for 20 min, no product yield was obtained. The next set
 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832
Fig. 1. Experimental setup used for microwave pyrolysis.
of experiments was conducted at a microwave power of 900 W,
product yield was obtained. Further experiments were carried out
with 900 W and a reaction time of 10 min.
2.6. Thermogravimetric analyzer (TGA)
Thermogravimetry is an analytical method to measure the
weight loss of the substance against temperature. NETZSCH STA
449 F3 Jupiter a thermogravimetry analyzer was used to determine
the decomposition temperature of plastic waste. The temperature
was measured from 30  C to 930  C with a heating rate of 20  C
min
1 and nitrogen as flow gas.
2.7. Characterization of product oil
2.7.1. Gas chromatography- mass spectrometry (GC-MS)
GC-MS equipped with flame ionization detector (FID) was used
to determine the different compounds present in the liquid oil.
Each compound was determined using the database available from
the NIST library search. Tedlar gas sampling bags of 500 ml was
used to collect the non-condensable gases from the reaction. GC
coupled with thermal conductivity detector (TCD) was used to
analyze the percentage of CO2, N2, O2, and CH4 gases.
2.7.2. Oil analysis
Oil properties were determined according to Indian standards.
Ostwald viscometer was used to determine the viscosity. Aniline
point was determined using IS 1448[P: 3]: 2007. To examine the
Corrosiveness, the test of copper strip IS 1448-152 (2004) was used.
The volumetric titration method was used to determine the acid
number of the oil and the standard method used was IS 1448-1-
1(2002). Cloud point was determined using the cloud point appa-
ratus and followed the standard method of [IS 1448-10-1(2012)].
Distillation characteristics were experimented using the IS 1448-18
method.
2.8. Cost analysis
Techno-economic analysis (TEA) is a method to determine the
1821
economic performance and viability of a pyrolysis process. It can be
estimated by knowing the capital cost, operating cost, and pro-
duction cost [24]. Capital cost is determined by adding all the cost
pertaining to purchase of the equipments. The quotes obtained
during purchase of equipments were used as base data for the
calculations. A direct cost factor which includes utilities and
building cost was multiplied with the equipment cost. Fixed capital
investment (FCI) was determined by the summation of direct cost
factor and indirect cost factor values. The following Eqs. (1)e(4) are
used to evaluate the costs.
FCI ¼ ðcost of equipment  direct factorÞ
þ ðcost incurred during modification and design
 indirect factorÞ (1)
TPC ¼ FCI þ 15 % FCI (2)
Capital cost ¼ plant capacity þ total equipment cost þ FCI þ TPC
(3)
Operating cost was calculated by considering feedstock cost,
maintenance cost, electricity cost and labour cost. Maintenance
cost depends on percentage of fixed capital investment. Feedstock,
labour and electricity cost are considered as variable operating
costs. And, the production cost was calculated from the basis of
research data. To study the techno-economic analysis, the
description parameters were provided in Table 1.
Cost of feed materials ¼ amount of feedstock  operating time
 working days
(4)
Annual operating cost
Production cost ¼ (5)
Annual production cost
1822 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832

Table 1
Descriptive parameter.

Laboratory microwave pyrolysis system Scalability of microwave pyrolysis system

Plant capacity (kg/h) 0.05 100

Working days (days/year) 300 300
Operating time (h/day) 8 8
Tariff rate of electricity in India (₨/kWh) 6.35
Labor cost in India (₨/h) 66
Plastic (₨/kg) 15
Activated carbon (₨/kg) 28

3. Result and discussion 3.2. TGA analysis of plastic waste

3.1. Proximate analysis
The proximate analysis of the plastic wastes and the biomasses
are shown in Table 2 and it was analyzed using standard experi-
mental methods IS 1350-1(1984). PSW and PPW have very high
volatile matter (99.56% and 92.65% by weight) making them highly
suitable for the recovery of hydrocarbons by pyrolysis. It was re-
ported that plastic waste with high volatile matter (z98 wt%) and a
low ash content of (<1 wt%) will enhance the pyrolysis volatiles
thereby producing more liquid oil [25]. Moisture content (MC) was
absent in the polymer samples. The presence of ash in PPW is
associated with the inorganic matter present in the raw material
that is used as additives [26].
Rice husk has a high ash content of 36.08 wt% which can be
tendered towards its source of cultivation. When compared to other
crops, rice husk has the potential to develop high ash content [27].
Moreover, it contains a fixed carbon of 12.56 wt% and a moisture of
7.02 wt%. Coconut sheath (CS) also a potential source for carbon. It
contains 69.60 wt% of volatile matter. It has an ash content of
5.10 wt% only. This indicates that the lignin content in CS is lesser
than that of rice husk [28]. Cornhusk (CH) possesses a lesser
moisture content of 6.06 wt%. Biomass with higher moisture con-
tent will affect the reaction temperature, 15 wt% of moisture con-
tent is the maximum allowable value recommended for biomasses
[29]. During impregnation and carbonization, the volatile matter in
the biomass that constitutes the lignocelluloses component, are
liberated as volatiles and the remaining non-volatiles present in the
biomass leads to the formation of porous materials. The fixed car-
bon content indicates the feasibility of the biomass materials to
produce carbon products such as activated carbon. Selection of
biomass materials which has a lesser ash content is desirable,
because higher ash content would produce undesired reactions and
rupture the structure of pores [30]. Moisture content in the biomass
is also an important factor that determines heating rate of the
absorbent materials. Lesser moisture content, the heating rate will
be faster [31]. From the proximate analysis, it can be determined
that the selected biomass materials are rich in carbon sources, the
absorbing ability of microwaves will be better in corn husk and
coconut husk materials. But, rice husk material has higher ash
content.
Fig. 2 shows the TGA curves obtained for PSW, PPW and poly-
styrene mixed with polypropylene (PSWþPPW). It is observed that
the degradation temperature for PSW is from 390  C to 460  C and
maximum degradation takes place at 426  C. The degradation
temperature for PPW is from 425  C to 490  C and maximum
degradation occurs at a temperature of 470  C. The decomposition
temperature was 317  C for a blend of equal ratios of PSW and PPW.
Maximum degradation was observed at 440  C for PSWþPPW and
shown in Fig. 3. It was noted that the synergistic effect of PSW and
PPW has significant features such as 1) lowering of the decompo-
sition temperature 2) potential to reduce the pyrolysis reaction
time and 3) accelerate the decomposition.
3.3. Characterisation of activated carbon
3.3.1. Different absorbents and their composition
In microwave-assisted heating, the role of absorbent is impor-
tant to determine the extent of cracking of polymer molecules. The
selection of absorbents depends on the penetration depth or skin
depth which signifies that the absorbent material will get trans-
mitted, reflected and absorbed. Materials such as Au, Ag and Zr
have a penetration depth (dp ¼ 1.3e6.7 mm), they are categorized as
microwave reflectors. Materials with high penetration depth
(dp ¼ 56e75 m) are microwave transmitters which include Teflon
and fused quartz. Activated carbon, carbon black and charcoal with
penetration depth (dp ¼ 0.5e11 cm) are termed as microwave ab-
sorbers [32].
The elemental carbon and other elements were determined
using EDX analysis and displayed in Table 3. Rice husk has 22.08 wt

Table 2
Proximate analysis.

Proximate analysis (wt. %)

Volatile matter Fixed carbon Ash content Moisture content
PSW 99.56 0.44 e e
PPW 92.65 5.39 1.96 e
RH 44.34 12.56 36.08 7.02
CH 75.96 13.23 4.75 6.06
CS 69.60 19.4 5.10 5.90
Fig. 2. TGA curves of PSW, PPW and PSWþPPW.
 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832 1823

are influenced by temperature, moisture content, microwave field

and chemical composition. The change in the dielectric properties
are related to thermal behaviour of the material [38]. Microwave
absorbing ability of the absorbent can decrease by the coke for-
mation of reacting materials in microwave pyrolysis [39].

3.3.2. Surface and porosimetry measurements

Surface characteristics, methylene blue and Iodine numbers of
the activated carbon are given in Table 4. The activated carbon
prepared from rice husk is microporous with a pore size of
0.9472 nm and an iodine number of 791 mg g
1. The methylene
blue number which indicates mesopore distribution in the acti-
vated carbon [40] is less in activated carbon materials prepared
from rice husk (RHAC), cornhusk (CHAC) and coconut sheath
(CSAC). It can be due to the chemical activation method and tem-
perature used for activation. Cornhusk (CHAC) has a surface area of
Fig. 3. Derivative weight of plastic waste. 679 m2 g
1 and pore size of 0.1171 nm. The absorption of micro-
waves is in the microporous region of CHAC and porous natures of
absorbents are important in determining the extent of pyrolysis
% carbon content and 40.19 wt% silica content. When the rice husk reaction. The absorption characteristics of CSAC show a well-
is chemically activated (RHAC), the carbon content increased to formed surface area of 764 m2 g
1 and pore size of 0.1083 nm.
56.37 wt%. This is due to the volatilization of organic byproducts. This surface characteristic provides reactive sites for pyrolysis
The carbon content of the activated carbons from corn husk (CHAC) cracking of polymer molecules and gets converted into product oil.
and coconut sheath (CSAC) is nearly the same with a wt.% of 83.78. Lam et al. [18] suggested that carbon absorbents with a low surface
It was observed that the carbon content in RHAC is lesser than that area of 7.18 m2 g
1 will have low reactive sites; thereby the con-
in CHAC and CSAC. It can be due to the presence of elements such as version of polymer molecules will be reduced. For a commercial
silica amounting to 8.13 wt.%, 1.14 wt.%. of sodium and 6.73 wt%. of activated carbon, it was observed that it possess both mesoporous
phosphorous. It was reported that the presence of silica content in and microporous region with a surface area of 692 cm2 g
1. In
microwave absorbent will lead to low dielectric tangent values general, the formation of mesopores and micropores depends on
(0.05), however, the silica contents have acidic properties that the preparation methods and activation temperature.
could work as a catalyst for pyrolysis reaction [33,34]. These ab- The surface properties of the produced activated carbon were
sorbents synthesized from agricultural residue has elemental ox- also compared with other microwave absorbers such as graphite,
ygen in the range of (14.33 wt%-36.37 wt%). Huang et al. [35] particulate carbon and MCM-41 and given in Table 4. It was
studied the catalytic effect of CaO in microwave pyrolysis (500 W) observed that, the produced activated carbon exhibits microporous
of corn stover. Their studies revealed that the catalyst CaO did not structure and a well developed surface area. Whereas, the other
enhance the reaction temperature. But the addition of catalyst microwave absorbers are mesoporous but has very low surface
slightly enhanced the formation of oil product, when compared to area. It was also noted that, low surface area will tend to have weak
the experiment without absorbent. Most importantly, the energy absorption thereby it causes difficulties for the polymer molecule to
yield, gas yield, solid residue and calorific value were not affected diffuse into surface of the absorbent. Surface area of the absorbent
by the addition of CaO catalyst in microwave pyrolysis. This is significant to provide the reaction sites for microwave pyrolysis
enunciates the fact that the presence of oxygen is incomparable of polymer materials. From the comparison of microwave absor-
with that of carbon in microwave pyrolysis. Carbon and activated bents, the produced activated carbon demonstrates higher surface
carbon were synthesized from biomasses. The synthesized micro- area; thereby the polymer molecules will have better reaction sites
wave absorbents are carbonaceous and they possess a high value of and leads to the formation of products.
dielectric constant which is capable of converting electromagnetic
energy to heat [36]. For activated carbon, the dielectric constant is 3.3.3. Scanning electron microscope (SEM) analysis
between 0.22 and 2.95 and for carbon; the value is 0.11e0.29. SEM provides information about the surface morphology.
Materials with high dielectric tangent values can be rapidly heated Fig. 4(ael) shows the SEM image of biomass. With the magnified
using microwaves [37]. The dielectric property of the material helps image at 250 X, Fig. 4(a, e, i) shows the surface morphology of rice
in faster completion of reaction at higher microwave power. They husk (RH), cornhusk (CH) and coconut sheath (CS) which indicates
a porous and fibrous morphology. Fig. 4(b, f, j) are the SEM images
of non-impregnated particles of rice husk carbon(RHC), corn husk
Table 3
carbon (CHC) and coconut sheath carbon(CSC), it shows the irreg-
Elemental composition. ular and non-porous structure. Fig. 4(c,g,k) shows the SEM images
of impregnated rice husk (RHAC), corn husk (CHAC) and coconut
Feed Wt.%
sheath (CSAC), in which the biomass materials are distinguished in
C H O Si their surface texture. Since the organic byproducts will be removed
RH 22.08 e 37.73 40.19 by the chemical activation method. From literature, rice husk on
RHC 24.88 e 31.61 43.51 impregnation (RHAC) by chemical activation method will exhibit a
RHAC 56.37 e 27.56 8.13
porous structure with crevices [41]. Activation of corn husk
CH 53.47 e 41.20 4.85
CHC 56.90 e 16.56 26.53 enhanced the formation of pores and exhibits a coral shaped
CHAC 83.79 e 15.04 e structure. The large pores are visible at a magnification of 250 X
CS 55.74 e 30.40 2.01 shown in Fig. 4 (g). The intensity of chemical activation on the
CSC 21.42 e 36.37 19.63 surface of coconut sheath has pronounced the formation of floral
CSAC 83.77 e 14.33 0.66
petal which is embossed with tiny pores [28]. Fig. 4(d,h,l) shows
1824 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832

Table 4
Surface properties and characteristics of activated carbon.

Feed BET surface area (m2 Pore size Pore volume Iodine number (mg Methylene blue number (mg Reference
g
1)a (nm)b (cm3g
1)c g
1) g
1)

RHAC 567 0.9472 0.3546 791 29 This study

CHAC 679 0.1171 0.4521 1270 44
CSAC 764 0.1083 0.4918 1214 48
Commercial AC 692 0.5372 0.2878 679 251

Activated carbon from coconut husk 850 1.5 0.318 e e [18]

Particulate carbon 7.18 2.2 0.004 e e
MCM-41 6.13 12.4 0.019 e e
Graphite 2.9 17 0.01 e e [31]
a
BET method.
b
Horvath-Kawazoe method.
c
Single point adsorption total pore volume of pores less than 2451.900 Å radius at P/Po ¼ 0.9921.

Fig. 4. SEM analysis of biomass (a) RH (b) RHC (ced) RHAC (e) CH (f) CHC (geh) CHAC (i) CS (j) CSC (kel) CSAC.

SEM images of RHAC, CHAC and CSAC at a higher magnification of compounds [43]. The peak at 1648 cm
1 and 1507 cm
1 are the
2500 X, in which the pores are more visible and uniform in struc- alkenes and aromatic C]C functional groups [23]. The peaks below
ture, whereas in case of RHAC it shows a cervical structure. 1100 cm
1 can be considered as fingerprint region. Fig. 5(d and e,f)
shows the FTIR spectrum obtained for corn husk (CH), corn husk
carbon (CHC) and corn husk activated carbon (CHAC) in which the
3.3.4. FTIR analysis of absorbents
alkene functional groups at 1100 cm
1 [23] diminished on chemical
The surface functional groups of biomass can be qualitatively
activation of corn husk, which is visible in FTIR curve of CHAC (see
analyzed by FTIR. Fig. 5(a-i)- shows the FTIR spectrum of biomass
Fig. 5).
materials. Fig. 5(aec) depicts the functional groups present in rice
Fig. 5(g and h, i) shows the functional groups present in coconut
husk (RH), carbonized rice husk (RHC) and activated carbon (RHAC)
sheath (CS), CSC, and CSAC it has adsorbed moisture and a sharp
in which broad hydroxyl eOHe group is visible at 3450 cm
1, due
peak at 1100 cm
1. On chemical activation, the functional groups
to adsorbed moisture. The peak at 2920 cm
1 is attributed to the
will disappear and released as volatiles. This indicates that acti-
CeH alkane group which is visible in RH [42]. This alkane group
vated carbon has elemental carbon in its structure. This manifests
diminishes in RHC and RHAC due to carbonizations at 400  C and
that the activated carbon prepared from biomass such as 1) RHAC 2)
500  C. In turn, a broad shoulder peak is visible at a wavenumber of
CHAC and 3) CSAC has carbon functional groups and will perform as
1790 cm
1 for RHAC. This is due to the activation of biomass (RH)
a receiver for incident microwaves.
with H3PO4. Hence, this peak is attributed to PeOeP phosphorous
 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832
Fig. 5. FTIR spectrum of biomass (a) RH (b) RHC (c) RHAC (d) CH (e) CHC (f) CHAC (g)
CS (h) CSC (i) CSAC. The functional groups are (1) strong and broad hydroxyl OeH
stretch at 3450 cm
1 (2) CeH stretch at 2920 cm
1 (3) PeOeP phosphorous com-
pounds at 1790 cm
1 (4) C]C (alkenes and aromatic) at 1648 and 1507 cm
1 and
(5)e(7) fingerprint region.
Fig. 6. Microwave pyrolysis of plastic waste using various activated carbons.
3.4. Microwave pyrolysis experiments
3.4.1. Microwave pyrolysis of polystyrene waste (PSW)
Initially, 10 g of Polystyrene waste (PSW) was added with 1g of
Rice Husk Carbon (RHC) and loaded in a quartz flask. The experi-
mental results are shown in Table 5- The product fraction consists
of 66.7 wt% oil, 18.40 wt% residue and 14.90 wt% non-condensable
gases. The amount of residue and gaseous compounds obtained
from PSWþRHC was high. This can be due to 1) Primary vapors
undergoing secondary reactions, in turn; more non-condensable
gases are produced and 2) Coking reactions and generation of
high spot temperature for PSW decomposition [10]. Polystyrene
waste with cornhusk carbon (CHC) improved the oil yield to
1825
83.30 wt% and reduced the residue yield to 0.90 wt%. It is noted that
high carbon content in CHC enhanced the volumetric heating of
PSW during microwave irradiation, thereby increasing the oil yield.
Coconut sheath carbon (CSC) was used to decompose PSW, it was
observed that 86.10 wt% of the oil was obtained and the gas yield
reduced to 10.50 wt%. This scenario is due to a well-formed porous
structure developed for CHC and CSC. From our previous studies
Prathiba et al. [44], the temperature was measured as 330  C for
PSW decomposition.
3.4.2. Microwave pyrolysis of polypropylene waste (PPW)
The pyrolysis of PPW with RHC yielded more gaseous products
as given in Table 5, which is due to the high activity of CeC bond
scission [1]. At 900 W pyrolysis of PPW with CHC, RHC and CSC the
oil yield was lesser. However, Undri et al. [10] obtained a liquid yield
of 74.70 wt% in microwave pyrolysis of polypropylene using carbon
as the susceptor with a microwave output power of 4 KW. The
experimental limitation of a maximum 900 W prevented experi-
mentation at higher wattages. At lower microwave powers,
decomposition of polypropylene will yield more non-condensable
gases. This was also evident in Suriapparao et al. [45] where a
lesser oil yield of 55.30 wt% was obtained, with 450 W microwave
output power and 10:2 polymer to absorbent ratio.
The vapor temperature was measured for the pyrolysis reaction
and noted as 380  C. It was observed that the average time
consumed for PPW pyrolysis was 252 s, which is slightly higher
when compared to PSW pyrolysis. Table 6 present the results ob-
tained by various literature in microwave pyrolysis. In this study,
there was a considerable reduction in reaction time and a lesser
amount of absorbent was required to decompose the plastic waste.
It highlights the fact that only plastic and biomass waste was used
in this study which was recovered as oil yield. Moreover, the
augment in oil yield can be explained as; carbon synthesized from
waste biomass RHC and CHC can absorb microwaves and transfer
the heat to the polymer. Coconut sheath carbon (CSC) has the
selectivity to recover product fractions from polymer waste. The
experiments were run in triplicate the standard deviation was
within 5%.
3.4.3. Effect of impregnation
The microwave pyrolysis of plastic waste was experimented
with carbon materials and discussed in section 3.4.1 and 3.4.2. The
effect of impregnation on microwave pyrolysis is discussed in this
section and shown in Table 7. The biomass was chemically activated
and named as Rice Husk activated Carbon (RHAC), cornhusk acti-
vated carbon (CHAC) and coconut sheath activated carbon (CSAC). It
was observed that when RHAC was used to decompose PSW the oil
yield was 83.30 wt% and the residue was 5.10 wt%. Owing to the
uniform microporous structure of RHAC, the retention of coke is
reduced and the blocking probability at pore entrance decreased.
The Carbon content in CHAC was 83.79 wt% which influenced a
higher oil yield of 88.40 wt%. Although the carbon content was
83.77 wt% in case CSAC, the oil yield was 77.80 wt% and an increase
in gas yield of 15.80 wt%. This phenomenon was due to visible hot
spots that appeared for an initial time of 1 min which leads to
excessive and uncontrolled cracking thereby increasing the gas
yield. During microwave pyrolysis of PPW with RHAC, more
amounts of gaseous products were produced. It was observed that
CHAC and CSAC used for PPW decomposition improved the oil yield
and total conversion of 100 wt% were obtained. This states that
biomass on impregnation influences the product fractions.
By impregnation and calcinations of the biomass, the pores have
enlarged by the subsequent removal of activating agent. Thus there
is formation of microporous structure in activated carbons. The
carbon matrix have absorbed the incident microwaves and got
1826 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832

Table 5
Yield fractions of individual feedstock.

Feed Absorbent Polymer: Mass of polymer (g) Mass of absorbent (g) Time, (sec) Residue yield (wt.%) Oil yield (wt.%) Gas yield (wt.%) Total conversion (wt.%)
absorbent
ratio

PSW RHC 10:1 10 1 178 18.40 66.70 14.90 81.60

CHC 10:1 10 1 123 0.90 83.30 15.80 99.10
CSC 10:1 10 1 190 3.40 86.10 10.50 96.60
PPW RHC 10:1 10 1 220 0.30 19 80.70 99.70
CHC 10:1 10 1 320 e 41.23 58.77 100
CSC 10:1 10 1 216 e 58.30 41.70 100

Table 6
Product yield fractions in literature.

Feedstock Polymer: Absorbent Mass of polymer Temperature Time Residue yield (wt. Oil yield (wt. Gas yield (wt. Reference
Susceptor (g) (oC) (min) %) %) %)

PS e Cylindrical mesh of e 1100e1200 12e15 5 80 15 [46]

iron
PS 100:47.3 Carbon 100 408 22 9.8 86.5 3.7 [10]
PS e Makarwal coal e e 16 18 76 6 [47]
PSW 10:1 Coconut sheath carbon 10 450e500a 3.1 3.40 86.10 10.50 This
study
PP 100:1 Activated carbon 5 400e600 30 0.40 29.80 69.80 [16]
PP 10:2 Graphite 20 600 11.5 6.0 55.30 38.70 [45]
PPW 10:1 Coconut sheath carbon 10 450e500a 3.6 e 58.30 41.70 This
study
a
Vapor temperature.

Table 7
Effect of impregnation.

Feed Absorbent Polymer: Mass of polymer (g) Mass of absorbent (g) Time, (sec) Residue yield (wt.%) Oil yield (wt.%) Gas yield (wt.%) Total conversion (wt.%)
absorbent
ratio

PSW RHAC 10:1 10 1 215 5.1 83.30 11.60 94.90

CHAC 10:1 10 1 171 2.70 88.40 8.90 97.30
CSAC 10:1 10 1 170 6.4 77.80 15.80 93.6
PPW RHAC 10:1 10 1 206 0.32 25.40 74.28 63.60
CHAC 10:1 10 1 235 e 51.90 48.10 100
CSAC 10:1 10 1 224 e 47.70 52.30 100

polarized by which the microwave energy was converted to heat
energy. Moreover, the micropores can induce deeper penetration of
microwaves which can result in multiple microwave reflection and
scatter within the surface of the absorbent. On comparison of re-
sults obtained from the use of carbon and activated carbon absor-
bents, it clearly shows that the oil yield has been significantly
improved by using RHAC. It also shows that, a considerable
reduction in silica content of RHAC have exposed more surface area
for microwave absorption. Due to deeper degree of penetration of
microwaves, there was no considerable reduction in reaction time.
Moreover, carbon absorbents have low surface area and less porous,
hence microwave absorption and reflection are possible only on the
front side of exposed carbon surface [48].
3.5. Microwave pyrolysis of mixed plastic waste
Microwave pyrolysis of mixed plastic waste experimented with
an equal ratio of polystyrene waste (PSW) and polypropylene waste
(PPW). Carbon from biomass was used, to study the effect of
polymer to absorbent ratio with three different ratios.
3.6. Effect of polymer to carbon ratio
Microwave pyrolysis can be carried out when a certainty exists
between the amount of polymer and its corresponding absorbent
ratio; hence the effect of polymer to absorbent ratio was studied.
Uniform mixing of carbonized particles with polymer is ensured for
effective microwave irradiation. Carbon prepared from rice husk
(RHC) was used with PPW and PSW in microwave pyrolysis.
Table 8- shows the effect of absorbent to polymer ratio in micro-
wave pyrolysis. The mass of polymers was constant for each ratio
(10 g of PSW, 10 g of PPW) only the mass of absorbent was changed
as 1g, 2g and 4g. For a polymer to an absorbent ratio of 10:0.5 (20 g
of plastic: 1 g of RHC), total conversion obtained was 99.20 wt%. The
vapors from the reaction were mostly non-condensable gases
amounting to 52.05 wt%. The ratio was then increased to 10:1, the
oil yield improved slightly and the non-condensable gases
decreased. The experiments were conducted with a 10:2 ratio, the
vapors thus formed were almost non-condensable gases account-
ing to 60.50 wt%, oil yield decreased to 38.55 wt%. This is due to two
reasons 1) Decrease in specific microwave power consumption of
37.5 W g
1 (microwave power absorbed per unit mass) which is
distributed in the carbon bed and 2) Increase in mass of absorbent.
It was observed that there were uncontrolled secondary cracking
reactions of primary vapors which lead to a high yield of gaseous
fractions with a low yield of oil [31]. Moreover, from the reaction
time, it is observed that lower amounts of absorbent lead to faster
completion of pyrolysis reaction and an increase of absorbent
 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832 1827

Table 8
Yield fractions of plastic waste.

Feedstock Absorbent Polymer: Mass of polymer Mass of absorbent Time, Residue yield Oil yield Gas yield Total conversion
absorbent (g) (g) (sec) (wt.%) (wt.%) (wt.%) (wt.%)
ratio

PSW þPPW RHC 10:0.5 10,10 1 158 0.80 47.15 52.05 99.20
10:1 10,10 2 135 1.40 50.65 47.95 98.60
10:2 10,10 4 190 0.95 38.55 60.50 99.05
CHC 10:0.5 10,10 1 185 1.55 46.25 52.20 98.45
10:1 10,10 2 117 0.20 58.05 41.75 99.80
10:2 10,10 4 145 e 42.80 57.20 100
CSC 10:0.5 10,10 1 237 e 76.70 23.30 100
10:1 10,10 2 180 e 81.50 18.50 100
10:2 10,10 4 222 e 70.10 29.90 100

facilitates controlled heating of feedstock. From Table 8- it is
evident that the gaseous products from PPWþPSW reflect the
dominance of PPW in the product yield.
Carbon prepared from corn husk (CHC) was used to pyrolyze
mixed plastic waste. At a ratio of 10:1 (20 g plastic waste: 1 g CHC),
resulted in an oil yield of 58.05 wt% and reduced the gas yield to
41.75 wt%. By an increase in the amount of absorbent added, the gas
yield would tend to increase [49]. PSW and PPW consist of the
aromatic rings and methyl groups attached to its backbone. The
synergistic effect of PSW and PPW produces more aromatic com-
pounds in product oil due to PSW and lighter hydrocarbons (C2eC6)
in gas yield due to PPW. Li et al. [50] studied the pyrolysis of mixed
plastics using pillared clays, in which the synthesized catalyst Fe-
PILC produced an oil yield of 79.3 wt% with a reaction time of
30 min. In this study, using microwave pyrolysis the reaction time
was drastically reduced to 117 s with an oil yield of 58.05 wt%. It
implies that a well-defined combination of porous structure and
polymer to absorbent ratio will enhance the product fractions.
Coconut sheath carbon (CSC) was used to decompose the plastic
waste, with a polymer to an absorbent ratio of 10:0.5 the oil yield
was 76.70 wt%. Total conversion of 100 wt% was obtained by using
CSC. This is due to the complex polymer molecule that surfaced in a
well developed porous structure with an average pore size of
5.506 mm and converted into product fractions. On increasing the
absorbent ratio to 10:1, 81.50 wt% of the oil was obtained with a
reaction time of 180 s. Thus the prepared carbon material from
coconut sheath has an ability to decompose the plastic waste and
convert it into valuable products with lesser reaction time. At a 10:2
ratio of CSC, gas yield increased to 29.90 wt% and oil yield of
70.10 wt%. This phenomenon was due to oil molecule which was
visualized in the gas stream was cracked into smaller hydrocarbons
thereby increasing the gas yield. In general, this can be explained as
more the amount of carbon, the polymer receives higher heating
rates hence the longer polymer chain gets converted into simpler
hydrocarbons which escape as non-condensable gases. This effect
of polymer to absorbent ratio correlates well with the available
literature studies [16,44,50].
3.7. Microwave pyrolysis of plastic waste using activated carbon
3.7.1. Effect of polymer to activated carbon ratio
Microwave pyrolysis of PSW and PPW mixtures were studied
using different activated carbons RHAC, CHAC, and CSAC. In this
quest, the effect of polymer to activated carbon ratio (10:0.5, 10:1,
and 10:2) was used to study the amount of activated carbon
required to pyrolyze the plastic mixtures. The results are shown in
Table 9, polymer mixtures to RHAC at a ratio of 10:0.5 produced an
oil yield of 62.35 wt% and a gas yield of 35.85 wt%. The ratio was
increased from 10:0.5 to 10:1, the oil yield increased to 69.55 wt%,
whereas the gas yield decreased to 29.23 wt%. It implies that some
gas components were converted to oil yield owing to an increase in
the amount of absorbent. While in turn gas yields increased from
29.23 wt% to 38.48 wt% with further increase in the ratio from 10:1
to 10:2. This scenario is within the expectation of the available
literature [49] when the amount of absorbent increases it results in
secondary cracking producing more amount of non-condensable
gases. The synergistic effect of polymer mixtures with CHAC
increased the oil yield to 77.40 wt%. The increase in oil yield can be
regarded as the formation of condensable vapors. CSAC, when py-
rolyzed with the polymer mixtures, produced an oil yield of
84.30 wt% and a gas yield of 15.70 wt% at a ratio of 10:1. Further
increase of the ratio from 10:1 to 10:2, gas yield was prominent in
the products amounting to 25.31 wt%. In microwave pyrolysis, the
product yield is influenced by the initial heating rate of the
absorbent, bound moisture content in the absorbent [31], surface
area, and generation of microplasma. However, in RHAC, CHAC, and
CSAC the oil yield and the total conversion were effective at a ratio
of 10:1. Therefore, the conditions are more favorable for product
yields when a polymer to activated carbon ratio of 10:1 was used.
Ding et al. [13] also studied the catalytic microwave pyrolysis of
polyolefins with HY-zeolite as the catalyst, in which the optimized
ratio was 10:1 for an effective degradation.
3.7.2. Comparison of synthesized activated carbon with commercial
activated carbon
The synthesized activated carbon was compared with com-
mercial activated carbon and shown in Table 10. From the results, it
is clear that the reaction time was considerably reduced by syn-
thesized activated carbon (RHAC). It was observed that with a re-
action time of 113 s, nearly 69.55 wt% of oil yield was obtained. Wan
Mahari et al. [51] studied plastic waste with used Frying oil (UFO)
and obtained an oil yield of 81 wt% with a reaction time of 15 min. It
is emphasized that in this study, the reaction time was10 min for a
complete pyrolysis reaction. Total conversion of 100 wt% was ach-
ieved by the use of CHAC and CSAC.
The rapid heating of coconut sheath activated carbon (CSAC)
achieved a higher amount of product oil 84.30 wt%, with a gas yield
of 15.70 wt%. This can be attributed to a large surface area of
764 m2 g
1 that provides more reaction sites for pyrolysis cracking
of polymer molecules [18]. Higher heating value (HHV) and energy
yield determine the energy content in the product oil. It was
observed that the oil has 46.87 MJ kg
1 and energy yield of 91.07 wt
%. indicating that, product oil with good combustion characteristics
can be obtained by using different absorbents in microwave py-
rolysis. Fig. 6- shows the microwave pyrolysis of mixed plastic
waste using different absorbents. Mixed plastic waste was pyro-
lyzed with commercial activated carbon (AC). The oil yield was
59.05 wt% and a higher gas yield of 38.97 wt% was obtained. The
higher amount of gas yield is due to 1) the decomposition of hy-
drocarbons 2) aromatization and 3) the depolymerization of
1828 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832

Table 9
Effect of polymer to activated carbon ratio.

Feedstock Absorbent Polymer: Mass of polymer Mass of absorbent Time, Residue yield Oil yield Gas yield Total conversion
absorbent (g) (g) (sec) (wt.%) (wt.%) (wt.%) (wt.%)
ratio

PSW þPPW RHAC 10:0.5 10,10 1 250 1.80 62.35 35.85 98.20
10:1 10,10 2 113 1.22 69.55 29.23 98.78
10:2 10,10 4 226 2.62 58.90 38.48 97.38
CHAC 10:0.5 10,10 1 171 0.03 70.47 29.50 99.97
10:1 10,10 2 200 e 77.40 22.60 100
10:2 10,10 4 234 2.04 63.95 34.01 97.96
CSAC 10:0.5 10,10 1 182 e 76.71 23.29 100
10:1 10,10 2 176 e 84.30 15.70 100
10:2 10,10 4 161 2.33 72.36 25.31 97.67

Table 10
Yield comparision.

Feed Absorbent Polymer: Mass of Mass of Time, Residue yield Oil yield Gas yield Total conversion HHV of oil (MJ Energy yield
absorbent polymer (g) absorbent (g) (sec) (wt.%) (wt.%) (wt.%) (wt.%) kg
1) (wt.%)
ratio

PSW þPPW RHAC 10:1 10,10 2 113 1.22 69.55 29.23 98.78 46.87 75.20
CHAC 10:1 10,10 2 200 e 77.40 22.60 100 46.81 83.57
CSAC 10:1 10,10 2 161 e 84.30 15.70 100 46.83 91.06
AC 10:1 10,10 2 124 1.98 59.05 38.97 98.02 46.32 63.09

hydrocarbons. Comparatively, product yield from commercial AC
was lesser than the yields obtained from synthesized activated
carbon from biomass. The product yield depends on 1) heating of
carbon in microwave field 2) precursor from which the carbon is
prepared 3) physical or chemical activation method and 4) pres-
ence of trace elements [52]. Based on the factors, activated carbon
prepared from biomass is a good absorber of incident microwaves
for rapid heating of the material. The reduction in time has an
added advantage for lesser energy utilization.
Table 11- shows available literature studies in microwave py-
rolysis of polypropylene. There are more studies for microwave
pyrolysis to experiment with the co-pyrolysis of biomass and
plastic waste using different absorbents. It was observed that the
co-pyrolysis of biomass and plastic produced an average oil yield of
56.13 wt%, even though the addition of catalyst did not facilitate a
complete conversion of materials. Moreover, the addition of more
absorbent increased the gas yield. Most importantly, in pyrolysis
process that experiments waste plastics the residue obtained and
complete decomposition is an important factor for a sustainable
process. The augment of the oil yield obtained in this study illus-
trates the fact that the addition of PSW to PPW will reduce the
gaseous fractions and residues. Moreover, the rapid heating of
materials was achieved by using CSAC as an absorbent with a
reduction in reaction time. This study explored the platform to use
waste biomass as an effective absorbent in microwave pyrolysis.
3.7.3. Effect of different power levels
Microwave pyrolysis of mixed plastic waste experimented with
different power levels such as 180, 360, 540, 720 and 900 W. The
effect at different power levels in the yield of mixed plastic waste
products was investigated. For these studies, 10g (each) of PPW and
PSW was mixed with 2g of RHAC in a ratio of (10:1). The reaction
time of 10 min was maintained at each power level. At lower power
input of 180, 360 and 540 W, it was observed that there was no
appreciable increase in temperature. It was observed that at lower
microwave output power (1) there is an absence of microplasma
generation and (2) quantum of energy required by the polymer
mixture to undergo pyrolysis is inadequate. To ascertain the
product yield, the reaction time was also increased to 20 min no
significant changes were observed. Hence, the microwave output
power was increased to 720 W and the oil yield was obtained at a
reaction time of 250 s which is shown in Fig. 7. It is observed that at
720 W the polymer mixture undergoes cracking reactions with an
increase in residence time resulting in a higher gas yield of 51.91 wt
%. At 900 W the oil yield obtained was 69.55 wt%, with a gas yield of
29.23 wt%. This is due to the rapid microplasma generation at
higher microwave power. Microplasma is an electrical discharge
that can be observed when there is a rapid oscillation in the elec-
tromagnetic field that generates high temperatures. The hydro-
carbons that come across this microplasmic region will undergo
secondary cracking thereby increasing the gas yields [55].

Table 11
Yields of microwave pyrolysis of plastic waste in literature.

Feed Absorbent Polymer: Time, Residue yield Oil yield Gas yield Total conversion Reference
absorbent (min) (wt.%) (wt.%) (wt.%) (wt.%)
ratio

PPþ Bambooþ Silicon carbide (SiC) 2:1 15 5.91 61.62 32.47 94.09 [53]
HZSM-5
PPþLigninþ HZSM-5 SiC 1:1 15 22.51 47.37 30.12 77.49 [54]
PPþmixed wood saw Graphite 10:2 10e11.5 13.1 59.4 29.5 86.9 [45]
dust
PSWþPPW Coconut Sheath Activated Carbon 10:1 10 e 84.30 15.70 100 This
(CSAC) study
 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832
Fig. 7. Effect at different microwave output power.
3.8. Product analysis
3.8.1. Gas chromatography-mass spectrometry analysis
The product oil was analyzed to examine the composition of
various hydrocarbons present in it. From GC-MS analysis, the oil
consists of 80.58% of aromatic content and 11.29% of olefinic con-
tent. It is due to polystyrene present in the polymer mixture. The
liquid oil analysis consists of single ring aromatics such as toluene
(3.39%), styrene (67.58%), ethylbenzene (1.82%) and a-methyl sty-
rene (1.71%). Styrene is formed by unzipping reactions or end chain
b-scission reactions [56]. Gasoline like fractions (GLF) has a carbon
distribution of C8eC12, which consists of paraffin, isoparaffins, cy-
cloparaffins, aromatics and olefins. The oil obtained from micro-
wave pyrolysis has 81.76% of GLF. Diesel like fractions (DLF) has
higher carbon distributions from C13eC20. The oil obtained has
5.37% of DLF and others are waxes which has a carbon distribution
of C23eC25.
The major non-condensable gases present in microwave pyrol-
ysis of polymer mixtures at 900W are determined using GC-TCD the
gases detected are CO2, CH4, N and O2. The production of 15.6%
methane will be from polypropylene waste due to its H/C ratio
which is 2.0 for Polypropylene waste [45]. CO2 gas was below the
detectable limit (BDL) of 0.1 since CO2 gas will be absent in the
pyrolysis of polymers. Microwave pyrolysis results in light hydro-
carbon molecules due to its deeper degree of cracking and a unique
method of volumetric heating. On the increase of microwave
output power, will result in the production of lighter hydrocarbon
molecules such as CH4 and H2 [57]. Nitrogen detected as N was
present amounting to 67.0% and oxygen (O2) was 17.2%. Hence
microwave pyrolysis of mixed plastic waste has the potential to
produce light hydrocarbons such CH4 which can be used as fuels
and chemicals for industrial purposes.
3.9. Properties of oil
To identify if the product oil has specific characteristics for fuel
production, the fuel properties must be determined. Table 12 shows
the properties of product oil. The kinematic viscosity of the oil is the
resistance offered by it to flow and shear under the influence of
gravity. Higher viscosity blocks engine parts due to low atomization
[58]. The obtained results indicate that the viscosity of the oil range
from 2.13 to 2.49 cSt, which is in the region of gasoline viscosity
1.3e2.4 cSt. API gravity of the oil was determined as 57.16 which
belongs to gasoline fractions. If the API gravity of oil is greater than
1829
31 it signifies that it is light oil which consists of light hydrocarbons.
The density of the oil varied from 0.75 to 0.79 g ml
1 which were
also near to the BS-IV specification for gasoline 0.73 g ml
1. Diesel
index (DI) is the property that denotes the ignition quality of the oil.
High diesel index denotes high paraffin content in oil while low DI
denotes high aromatic content in oil. An increase in aromatics de-
creases ignition quality [59]. The diesel index of the obtained py-
rolysis oil was 46.87. Aniline Point of oil was determined as 82  F.
From the values obtained for diesel index and aniline point it states
that the oil has aromatic content. Cetane number (CN) is the
measure of the ignition delay of fuel. Ignition delay is the measure
of the time between the injection of fuel and the beginning of its
ignition. Higher the cetane number the fuel has short ignition delay
due to the presence of n-paraffins in the fuel. Complex molecular
components like aromatics which need high pressure and tem-
perature for ignition [60]. The product oil has a cetane number of
42.81 which is lower than the standard cetane number of 71 for
gasoline. Since the CN is less the ignition delay period will be much
longer however, cetane improvers can be added to the fuel to
minimize the ignition delay.
The acid number is the quantification for the amount of acid
present in fuel oil. The acid number of the pyrolysis oil was deter-
mined as 0.59e0.95 mg KOH g
1, it suggests that the oil obtained is
slightly acidic. The acid value can be reduced by using acid lowering
agents. From copper corrosion test, a category of 1-slightly tarnish
was obtained for the oil. The heating value or calorific value of a fuel
is the amount of heat generated by the complete combustion of a
unit mass of the fuel under standard conditions of temperature and
pressure [61]. The calorific value of fuel influences the output po-
wer of an engine. The product oil has a high gross calorific value of
46.87 MJ kg
1 and has good combustion characteristics. The ob-
tained values were within the range of 44e48 MJ kg
1 which was
reported by Anuar Sharuddin et al. [62e64]. Lower temperature
behavior of fuel can be determined by the cloud point. The product
oil has a cloud point of 6  C due to wax content amounting to
12.87%. The cloud point value is lesser when compared to con-
ventional fuel gasoline. It was suggested that polymeric depressant
additives are very effective in reducing the temperature of cloud
point, mainly the additives are naphthalene polyacrylates, poly-
methacrylates and co-polymers of a-olefins. By using these addi-
tives, cold flow properties of the liquid oil from plastic waste can be
improved [65].
Distillation Characteristics of product oil have a significant effect
on its use as a fuel additive since it provides information on its
behavior during storage and use. Higher Distillation temperature
decreases the delay of ignition and decreases the probability of
knocking in diesel engines [59]. The initial boiling point (IBP) of the
pyrolysis plastic oil was determined as 170  Ce188  C and the final
Boiling Point (FBP) was determined as 290  C. The boiling point
range of oil is from 170oC to 290  C. This boiling range is due to the
presence of a higher amount of aromatic and olefinic content. On
further process of the boiling range of the oil can be aligned with
that of gasoline range hydrocarbons.
3.10. Production cost of oil in microwave scaled-up unit
Techno-economic analysis was studied to determine the feasi-
bility and application of research studies to a scaled-up unit. TEA is
important to design a profitable plant, understanding the market
scenarios and the social consequences of pyrolysis process. To es-
timate the capital cost, it is necessary to know the plant capacity
and the basic equipment cost. Fixed capital investment includes
both the direct factor and indirect factor. Direct factor are instru-
mentation, electrical, insulation and buildings. Indirect factor are
engineering, construction, licensing and auxiliary services. In order
1830 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832

Table 12
Physical properties of oil.

Properties PSWþ PPWþRHAC PSWþPPWþAC PSWþPPWþCHAC PSWþPPWþCSAC Diesel [BS IV] 2017 [Nation Gasoline [BS IV]2017 [Nation
wide] wide]

Kinematic viscosity 2.13 2.23 2.45 2.49 2.0e4.5 1.3e2.4

@ 40  C, cSt
Aniline Point, oF 82 82 82 82 >120 145
API gravitya 54.68 48.75 57.16 57.16 30e40 59.72
Density, g ml
1 0.75 0.79 0.76 0.76 0.83 0.73
Specific Gravity @ 15  C 0.76 0.79 0.75 0.75 0.84 0.74
Diesel Indexb 45.33 40.17 46.87 46.87 <55 86.59
Cetane numberc 41.73 38.12 42.81 42.81 51 71
Gross calorific value, MJ/ 46.87 46.32 46.81 46.83 43.5e55.7 45.6
kg
Cloud point,o C 6 1
1 6
15
19
HHV,MJ/Kg 46.87 46.32 46.81 46.83 43.5e55.7 45.6
Energy yieldd (wt.%) 75.20 63.09 83.57 91.06 e e
Copper strip corrosion test 1-slightly tarnish 1-slightly 1-slightly tarnish 1-slightly tarnish 1-slightly tarnish Not less than 1
tarnish
Acid numbere, mg KOH 0.59 0.73 0.87 0.95 0.50 (max) 0.148
g
1
IBP,oC 188 170 179 185 172 27
FBP,oC 285 290 285 265 350 225
a
API gravity ¼ (141.5/specific gravity) e 131.5.
b
Diesel index ¼ (aniline point * API gravity)/100.
c
Cetane number ¼ (0.7*Diesel index) þ10.
d
Energy yield (wt.%) ¼ [HHVoil/HHVfeed] x yield of oil.
e
[V1N1eV2N2]/oil used in g.

to know, the production cost of oil it is important to evaluate capital
and operating costs. Table 13 shows the TEA analysis to evaluate the
production cost of oil. Operating cost are the parameters obtained
during initial start of the process such as 1) the cost of plastic waste
(₨/kg) 2) cost of activated carbon (₨/kg) 3) electricity tariff rate
(₨/kWh) and 4) labour cost (₨/h). All these costs are obtained w.r.t
market survey in India and given in Table 1.
In a lab-scale system, the amount of feedstock was 0.05 kg (25 g
of PPW and 25 g PSW) for each operation. In one working day,four
experiments were conducted that include the time of preparation,
equipment cooling time and cleaning for the next batch of exper-
iment. The total cost of feedstock was estimated as ₨ 900/year
(cost of plastic waste ₨ 15/kg x 0.05 kg of feedstock/operation x 4
operation/day x 300 days/year). The cost of activated carbon/sus-
ceptor was calculated as ₨168/year (optimum quantity of activated
carbon 0.005 kg/operation x 4 operations/day x 300 days/year x
cost of activated carbon ₨ 28/kg). Cost of electricity for lab-scale
microwave pyrolysis was estimated as ₨13716/year (tariff rate ₨
6.35/kWh x microwave power 0.90 kW  8 h/day x 300 days/year).
Maintenance cost was calculated from fixed capital investment. No
labour cost was estimated for this lab-scale system.
For the scalability of microwave pyrolysis system, the experi-
mental result obtained from lab-scale microwave pyrolysis was
used to estimate the key parameters. The scaled-up unit was
designed to treat 100 kg/h of plastic waste with working days of
300 days/year and a plant operation of 8 h/day. Feedstock cost was
calculated as ₨ 18 lakhs/year. The cost of activated carbon was ₨
336000/year (300 days/year x 4 operations/day x 10 kg/operation x
₨ 28/kg). Electricity cost was estimated as ₨ 22860/year (₨ 6.35/
kWh x 1.5 kW  8 h/day x 300 days/year). The labour cost in India is
₨ 66/h; the labour cost for scaled-up unit was calculated as ₨
158400/year (₨ 66/h x 8 h/day x 300 days/year).
From the operating cost and capital cost, the cost of production
of oil can be estimated. In a lab-scale microwave pyrolysis process,
the experimental results demonstrated that 84 wt% of oil can be
collected for feed rate of 0.05 kg/h. Based on these results, the
production of oil was calculated as 0.1686 kg/day (0.05 kg/h x
84.3 wt% x 4 experiments/day). In order to determine the annual

Table 13
Techno-economic analysis for microwave pyrolysis w.r.t cost of production.

Cost elements Laboratory microwave pyrolysis system Scalability of Microwave pyrolysis system

Capital cost
(1) Plant capacity (kg/h) 0.05 100
(2) Total equipment cost (₨) 38,462 3,85,000
(3) Fixed capital investment (FCI, ₨) 71,844 4,53,036
(4) Total plant cost (TPC, ₨) 82,621 5,88,947
Operating cost
(I) Cost of feed materials (₨/year) 900 18,00,000
(II) Cost of susceptor/absorbent (₨/year) 168 3,36,000
(III) Cost of electrical consumption (₨/year) 13,716 22,860
(IV) Cost of maintenance (₨/year) 2155 13,591
(V) Cost of labor (₨/year) e 1,58,400
Estimated production cost of oil
(a) Production of oil (kg/day) 0.1686 337
(b) Annual production of oil (L/year) 67 1,33,105
(c) Cost of production (₨/L) 251 18
Price of gasoline fuel (₨/L) 76 e
Price of diesel fuel (₨/L) 70 e
 P. Rex et al. / Journal of the Energy Institute 93 (2020) 1819e1832
production of oil, density of oil (0.76 kg/L) was used and estimated
to be 67 L/year (0.1686 kg/day x 300 days/0.76 kg/L). The overall
cost of production of oil is the ratio of summation of operating cost
to annual production of oil. The production cost of oil in microwave
is higher when compared with diesel and gasoline price in India,
2019. From gaining a thorough research data from lab-scale system,
it was understood that the production cost of oil in a scaled-up
microwave pyrolysis unit is ₨ 18/L. This low-cost fuel from
scaled-up unit has the potential to serve the humanity from esca-
lating diesel and gasoline prices. Nevertheless, the gaseous prod-
ucts from pyrolysis have significant values, they comprise of H2,
CH4, CO, and light fractions C2H4. These light gases can be reformed
or extracted to manufacture chemical additives [24]. The char from
microwave pyrolysis is a good source of carbon; neither can be
reused as susceptor nor can be sold as activated carbon for effluent
treatment in industries.
4. Conclusions
In this present work, three types of agricultural residues rice
husk, corn husk and coconut sheath were used to develop micro-
wave absorbents and the performance of these absorbents was
investigated in microwave pyrolysis of PSW and PPW. The conclu-
sions are derived as: Proximate analysis revealed that, selection of
biomass materials with less moisture and ash content is desirable.
The elemental composition of the absorbents showed presence of
higher carbon content in coconut sheath and corn husk. The
morphological characteristics of the absorbents exhibited coral-
shaped, floral-petal and crevices like structure with high surface
area. The study of individual plastic waste PSW and PPW using
carbonized and activated carbon particles signifies that the oil yield
increased and gas yield reduced when activated carbon was used:
whereas, non-condensable gases are more in carbonized particles.
This demonstrates the effect of impregnation which has enhanced
the oil yield of individual plastic waste. While the synthesized
activated carbon was used for mixed plastic waste a sharp increase
in oil yield was achieved. The carbon content present in the
absorbent helps in the decomposition of plastic waste during mi-
crowave irradiation. In comparison with commercial AC, the syn-
thesized CSAC produced 84.30 wt% of oil while commercial AC
produced 59.05 wt%. only. This explains the robustness of synthe-
sized activated carbon from RH, CH, and CS. Moreover, the product
oil has a density of 0.76 g ml
1 which can be a substitute for gas-
oline range hydrocarbons provided with an advanced process to
reduce aromatic content. Microwave scalability studies also
revealed that production cost of pyrolysis oil was estimated as Rs
18/L, which is much lower than the gasoline fuel that is sold at a
rate of Rs 76/L. It suggests that production of fuel from plastic waste
has a huge potential to produce low cost fuels. These studies have
demonstrated that, cost-effective absorbents can be developed
from biomass and also it will inspire more studies for the devel-
opment of microwave absorbing materials.
Acknowledgements
Authors like to thank the University Grants Commission, India-
Maulana Azad National Fellowship for the fellowship grant (F1-
17.1/2015-16/MANF-2015-17-TAM-58352/SA-III), and Sophisticated
Analytical Instrumentation Facility (SAIF), IIT Madras.
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