Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

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Journal of Analytical and Applied Pyrolysis

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

Microwave-assisted pyrolysis and distillation of cooking oils for liquid

bio-fuel production
Samsudin Anis a, *, Rais Alhakim a, Wahyudi a, Ahmad Mustamil Khoiron a, Adhi Kusumastuti b
a
Department of Mechanical Engineering, Universitas Negeri Semarang, Kampus Sekaran, Gunungpati, 50229 Semarang, Indonesia
b
Faculty of Engineering, Universitas Negeri Semarang, Kampus Sekaran, Gunungpati, 50229 Semarang, Indonesia

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

Keywords: The goals of this study are to produce and to characterize bio-oil from pyrolysis and distillation of liquid samples
Microwave heating in a microwave reactor. Waste cooking oil (WCO) and fresh cooking oil (FCO) were employed as the feedstocks.
Pyrolysis A 900 W microwave reactor was modified and filled with 300 g of charcoal. It was used for both pyrolysis and
Distillation
distillation experiments. The pyrolysis experiments were performed at various feed flow rates and temperatures
Continuous process
Waste cooking oil
ranging from 0.051 kg/h to 0.306 kg/h and 400 ◦ C–550 ◦ C, respectively. The sample was introduced continu­
Bio-oil composition ously into the microwave reactor for 60 min. Nitrogen gas was also supplied to ensure pyrolysis condition. The
bio-oil product was then distilled to obtain fuel fractions. The results showed that the products yield and bio-oils
composition were strongly influenced by pyrolysis temperature and type of cooking oils, while there was almost
no influence of feed flow rate under the investigated condition. The bio-oil contained 90− 100 wt.% aliphatic
hydrocarbons and the rest were aromatic hydrocarbons. The bio-oil produced from WCO contained more than
50 wt.% green-diesel (C10-C15) which was comparable to that from FCO. The green-diesel fraction showed good
fuel properties agreement to that of fossil diesels. Overall, microwave-assisted pyrolysis and distillation processes
are potential ways to convert problematic WCO into useful liquid bio-fuel and green-diesel fuel.

1. Introduction pyrolysis oil and gas products can be utilized as fuel or chemical feed­
stock, while the char product can be utilized as a substitute for activated
Until now, the dependency on energy supplies from fossil fuels is still carbon although this is not yet so popular. Pyrolysis process can be
very high. This raises a variety of crucial issues including economic, carried out by applying conventional heating or microwave heating. The
security of energy supply, and as well as environmental problems [1]. As literature showed that bio-oil production process with conventional
such, concerns about the high demand for fossil fuels and global climate heating methods requires a relatively longer time due to transferring
change have attracted increasing interest in the development of heat energy to raw materials from the reactor wall to the surface of the
renewable energy [2,3]. Sustaining bioenergy production from natural material to be processed [9]. Therefore, conventional heating consumes
resources such as palm oil, fat, and other vegetable oils is considered as more energy as it suffers from heat losses to the environment [10].
the main alternative energy sources for bio-fuel production [4,5]. In Meanwhile, the heating process by using microwave irradiation is faster
addition, waste cooking oil (WCO) can also be a potential source for than conventional heating. There are several advantages in micro­
bio-fuel production [6]. This is due to the availability of easy-to-obtain waving heating including fast and environmentally friendly processes,
materials with low price. For instance, the technical potential of WCO more product yields, uniform heating, direct use of large-sized raw
production from restaurants, hotels, schools, hospitals, rural and urban materials, and can be used to treat various types of waste [11–13].
households in Indonesia can reach more than 3 million tons/year [7]. It was revealed that microwave heating has been successfully applied
The pyrolysis process is believed as one of the best ways to convert for processing of various wastes including liquid waste of WCO [14–16].
WCO into alternative fuels. This process involves the breakdown of more In general, the use of microwaves is widely applied to the trans­
complex chemical compound to be simpler one at medium to high esterification process for bio-oil production from liquid waste. Instead of
temperatures with little or without oxygen. The product of this process transesterification, the use of microwaves for pyrolysis of liquid waste
can be in the form of gas, solid (char), and liquid (bio-oil) [8]. The has also been gained attention in recent years. This is because pyrolysis

* Corresponding author.
E-mail address: [email protected] (S. Anis).

https://doi.org/10.1016/j.jaap.2020.105014
Received 5 June 2020; Received in revised form 18 October 2020; Accepted 26 December 2020
Available online 30 December 2020
0165-2370/© 2020 Elsevier B.V. All rights reserved.
S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Fig. 1. Schematic diagram of the experimental equipment for pyrolysis process.

has several advantages including the flexibility to use various types and was processed under batch microwave pyrolysis for diesel-like fuel re­
compositions of raw materials, and several valuable fuels and chemicals covery at some process parameters such as temperature and type of
can be produced. The literature showed that waste oils derived from absorber. A recent study also reported about bio-oil production from
engine oil have been successfully converted into useful products under WCO at a low temperature of 400 ◦ C under continuous microwave py­
microwave pyrolysis [15,17,18]. However, information regarding WCO rolysis [20].
processing through microwave-assisted pyrolysis process is rarely Considering the preceding description, instead of batch process,
available in the published literature. Diesel-like fuel recovery from mi­ research on continuous pyrolysis process of WCO in a wide range feed
crowave pyrolysis of waste palm cooking oil has been done [19]. In the flow rate and pyrolysis temperature under microwave irradiation is of
study, waste palm cooking oil collected from a fried chicken restaurant important to be performed. Therefore, this work is conducted to

Fig. 2. Schematic diagram of the experimental equipment for distillation process.

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S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

investigate the effect of three main parameters including feed flow rate, Table 1
pyrolysis temperature and type of cooking oils (waste and fresh cooking Experimental pyrolysis condition.
oils) on the yield of bio-oil and its composition produced from contin­ Manipulative Operating Constant variable Respond variable
uous microwave-assisted pyrolysis. The bio-oil was then distillated in a variable condition
microwave reactor to obtain fuel fractions. Special attention was also Temperature:
Temperature profile
performed to get fuel properties of bio-diesel fraction and to estimate the 450 ◦ C
energy consumption and recovery. The waste cooking oil employed in Feedstock: WCO
this study was collected from different sources, resulted in having Amount of
charcoal: 300 g
relatively complex compounds. This is important because in fact, the Feed flow rate
0.051–0.306 kg/
N2 flow rate: Mass yield of
abundant availability of waste cooking oil comes from various sources h
100 mL/min products (bio-oil, gas,
such as restaurants, traditional food stalls, and households. Process duration: solid)
60 min
Microwave
2. Materials and methods
power: 900 W
Mass yield of
2.1. Materials Feed flow rate:
products (bio-oil, gas,
0.102 kg/h
solid)
Waste cooking oil (WCO) collected from some local restaurants and Feedstock: WCO,
FCO
traditional food stalls was used for bio-oil production. Commercial fresh Amount of
cooking oil (FCO) obtained from local market in Semarang, Indonesia Temperature 400–550 ◦ C charcoal: 300 g
Chemical
was also used for comparison purposes. Prior to use, the water content in N2 flow rate:
composition of WCO,
WCO and FCO were removed by heating them at ±103 ◦ C for 30 min, as 100 mL/min
FCO, bio-oil
Process duration:
given in a previous study [12]. After cooling, filter papers were
60 min
employed to separate solid particles within the samples. For absorbing Microwave
and converting microwave energy into heat, commercial particulate power: 900 W
charcoal was employed. The charcoal was used in this work as it
available commercially and generally has good microwave absorption
ability compared to others absorber material. High purity nitrogen of 2.3. Pyrolysis and distillation experiment
99.9 % was also used to remove oxygen within reactor and piping sys­
tems and to push pyrolysis products towards the condensation system. This study relates to the use of microwave reactors for waste cooking
oil pyrolysis process and for pyrolytic-bio oil distillation process. In the
2.2. Experimental setup pyrolysis process, the feed was supplied continuously. This research was
carried out sequentially to get a fundamental point of view of the
Fig. 1 presents a schematic diagram of the research equipment for continuous processing of waste cooking oil using a microwave reactor.
pyrolysis process. In this study, continuous system of microwave- First, research was begun by examining the thermal capability of the
assisted pyrolysis of waste and fresh cooking oils was performed. To reactor at various feed flow rates. This information is important to assess
allow continuous process of the sample, a 2.5 L feed oil tank equipped the ability of microwave system to generate sufficient heat for main­
with a peristaltic pump and valves as flowrate regulator was applied and taining the targeted reaction temperature. The reaction temperature
settled over the microwave oven. A 2450 MHz microwave oven with profile was observed at feed flow rates ranging from 0.051 kg/h to
12.23 cm wavelength and 900 W maximum output power was used as 0.306 kg/h. The feed of waste cooking oil was injected after the targeted
the heating source. The microwave oven was modified to allow each reaction temperature of 450 ◦ C was achieved. This temperature was
pyrolysis experiments to be carried out properly. A reactor made of chosen because it is widely proven to be a good condition for materials
quartz glass with 1000 mL capacity was used and vertically installed decomposition through pyrolysis process. The reaction temperatures
inside microwave cavity. To measure the temperatures inside reactor were then recorded using a camera during 60 min of irradiation. At the
and microwave cavity, K-type thermocouples were used. The pyrolysis same time, pyrolysis process of waste cooking oil as the effects of feed
reaction temperature was controlled by using a temperature controller. flow rate as well as weight hourly space velocity (WHSV) and power
To prevent damage to the microwave oven, the temperature of the mi­ load (WHSV/microwave power, MP) were also examined and evaluated
crowave cavity must be maintained below 200 ◦ C. To condense the to get the best conditions of the applied system. Secondly, pyrolysis
pyrolysis vapor product, a double glass-tube condenser was used. It was process was then carried out to investigate the effect of reaction tem­
supported by a pump to circulate cooling fluid from a water bath con­ peratures at a fixed feed flow rate of 0.102 kg/h using WCO and FCO.
taining a mixture of water and ice. Glass bottles with a capacity of The reaction temperatures were varied from 400 ◦ C to 550 ◦ C. Table 1
500 mL were used as containers to collect bio-oil products. shows the experimental condition of pyrolysis studies.
Fig. 2 presents a schematic diagram of the research equipment for Prior to conducting the thermal and pyrolysis experiments, 300 g of
distillation process. In this study, microwave-assisted distillation of bio- charcoal was poured into the quartz glass reactor aimed at absorbing
oil was performed. Similar to pyrolysis process, a 2450 MHz microwave microwave energy. Addition of microwave absorber is needed as WCO
oven with 900 W maximum output power was used as the heating and FCO samples are non-polar substances or insulator materials that
source for distillation experiments. A Pyrex reactor of 1000 mL was difficult to be heated under microwave irradiation [12]. After that, the
vertically positioned inside the microwave cavity, and filled with char­ microwave reactor was then turned on until the specified pyrolysis
coal as microwave absorber. The temperature inside the reactor was temperature was reached. This condition was maintained for a while,
measured by using a K-type thermocouple. The distillation reaction then WCO or FCO sample was introduced continuously into the reactor
temperatures were adjusted with the aid of a temperature controller. A at a predetermined flow rate for 60 min. The product of pyrolysis vol­
double glass-tube condenser equipped with a pump for cool water cir­ atiles in the reactor was led into a condensation system to condense the
culation was employed to condense fuel fraction products. The fuel bio-oil. Before and during the process, nitrogen gas was injected at a
fraction products were then collected using 500 mL glass bottles. flow rate of 100 mL/min to ensure the pyrolysis process takes place
without the presence of oxygen. Once the reaction time was reached, the
microwave reactor was switched off and allowed to cool to ambient
temperature by the aid of a fan.

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S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Fig. 3. Pyrolysis temperature profile at 450 ◦ C under various feed flow rates.

The amount of bio-oil product was determined via weight difference MS 2.0 software was employed for identification of the characteristic
of the oil collector and condenser before and after the experiments. The peaks to compounds spectrum and quantitative analysis was carried out
weight change in the charcoal-contained reactor was also measured to based on the peak area integral of each identified compounds. Three oil
obtain the yield of solid product. The equipment could be easily samples were taken for obtaining the average.
dismantled for weighing purposes and reconnected back for further The obtained bio-diesel fraction from microwave-assisted distillation
experiments. The yield of gas product was determined by mass balance. was also analyzed to get its fuel properties including density (ASTM
Evaluation of the yield of products is given in the following equations: D4052-18), kinematic viscosity (ASTM D445-18), total acid number
mfB − miB (ASTM D664), flash point (ASTM D93-18), pour point (ASTM D97-17b),
YBO = × 100% (1) calorific value (ASTM D240-17), and cetane index (ASTM D4737-10,
mO
2018). The fuel properties of bio-diesel were then compared with
mfS − miS commercial fossil diesel to obtain better point of view regarding the
YS = × 100% (2)
mO quality of the produced bio-diesel.

YG = 100% − (YBO + YS ) (3) 3. Results and discussion

where YBO , YS , and YG are the yields of bio-oil, solid, and gas products,
3.1. Temperature profile
respectively in wt.%; mfB and miB are the final and initial weight of the
oil collector and condenser, respectively; mfS and miS are the final and Fig. 3 shows the temperature profile at the targeted reaction tem­
initial weight of the reactor contained charcoal, respectively; while mO is perature of 450 ◦ C at various feed flow rates. The figure shows that
the total weight of WCO or FCO during the pyrolysis process. addition of feed flow rate affects reaction temperature. In general, the
The last stage was distillation of bio-oil. In this work, the obtained microwave system was able to maintain the reaction temperature of
bio-oil from continuous microwave-assisted pyrolysis of WCO at 450 ◦ C around 450 ◦ C from the beginning to the end of the feed injection pro­
was then processed under single stage distillation in a microwave cess into the reactor for feed flow rate of 0.051 kg/h, 0.102 kg/h, and
reactor to obtain liquid bio-fuel fractions. The hydrocarbon components 0.204 kg/h. It was found that the average reaction temperatures were
of bio-oil are separated according to their boiling temperature range to 450.1 ◦ C, 448.7 ◦ C, and 447.5 ◦ C in the same order of feed flow rates,
obtain fuel fraction which are 230 ◦ C–340 ◦ C for diesel fraction, respectively. The maximum temperatures at the condition were found to
180 ◦ C–230 ◦ C for kerosene fraction, 30 ◦ C–180 ◦ C for gasoline fraction, be 453 ◦ C, 451 ◦ C, and 450 ◦ C, whereas the minimum temperatures
and the rest are grouped as heavy fuels fraction. Three samples of each were 448 ◦ C, 447 ◦ C, and 445 ◦ C, respectively. This indicates that under
fraction were taken for obtaining the average. these feed flow rate conditions, the interaction of microwave with
absorber is capable to convert microwave energy into heat to supply and
2.4. Analytical method maintain the specified reaction temperature.
In the meantime, for feed flow rate of 0.306 kg/h, the reaction
A Perkin Elmer GC Clarus 680 MS Clarus SQ 8 T was applied for temperature initially dropped from about 450 ◦ C to 434 ◦ C after eight
chemical composition analyses of the feedstocks and bio-oil products. minutes of injection of the feed into the reactor, and then gradually
The GC–MS has 30 m length of column with 250 μm of diameter. The increased until the targeted reaction temperature can be maintained.
maximum oven temperature was conditioned at around 300 ◦ C, while The result indicated that the average reaction temperature was 443.8 ◦ C
the injector split ratio was prepared at 42.2:1. To avoid sample oxida­ under this feed flow rate condition. The high feed flow rate with lower
tion, helium gas was used to purge the sample along the column at temperature could cause convective cooling effect at the absorber sur­
0.8 mL/min. Moreover, oven temperature was set at 60 ◦ C for 5 min, face that consequently requires more energy to be heated. This illus­
ramp at 5 ◦ C/min to 280 ◦ C and then hold at 280 ◦ C for 5 min. Sample trates the maximum thermal capability condition of the experimental
analysis process was run for 54 min. The sample was filtered by using a equipment used in this work in which the microwave oven takes longer
filter paper before injected into the GC at one μl. All samples were to produce enough heat to maintain the desired reaction temperature
treated and analyzed at similar program to obtain good result with ac­ from the beginning to the end of the feed injection process.
curacy of more than 98 % (or less than 2 % error) as recommended. NIST

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S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Fig. 5. Yields of products from pyrolysis of WCO at different temperatures.

Fig. 4. Yields of products from pyrolysis of WCO as the effect of feed flow rate
and its relationship with WHSV and WHSV/MP.

Based on the above results, it is expected that for higher process

capacities, more amount of absorber material in the reactor and higher
output microwave power are required to get better thermal stability.
This phenomenon is also observed in the previous studies regarding the
potential of microwave heating to handle high feed rates at a fix mi­
crowave power by regulating the amount and type of absorber in
increasing the reaction temperature [10,12,18].

3.2. Yield of product

Fig. 6. Yields of products from pyrolysis of FCO at different temperatures.
3.2.1. Effect of feed flow rate
Fig. 4 depicts the yield of products generated from pyrolysis of waste important parameters commonly used in the chemical reactor design
cooking oil in a microwave reactor as the effect of feed flow rate at a fix process. As shown in the figure, under the investigated condition, the
reaction temperature of 450 ◦ C. It could be observed that almost no used microwave-assisted pyrolysis system is capable to process each
influence of WCO feed flow rate on the yield of bio-oil. This is indicated hour feed of WCO up to about one time the mass of absorber material
by only about 3.4 % maximum difference in the yield of bio-oil from with a relatively high yield of bio-oil product. In the meantime, the
WCO pyrolysis at various feed flow rates ranging from 0.051 kg/h to WHSV/MP represents the power load of the system that is calculated as
0.306 kg/h. The slightly decrease of bio-oil yield at the highest feed flow the WHSV divided by the maximum output microwave power. This
rate applied in this study might be occurred due to significant temper­ provides more useful information about the highest possible load ca­
ature fluctuations that tended to produce a lower average pyrolysis pacity of the microwave reactor by considering the available output
temperature than others as shown previously in Fig. 3. This elucidates microwave power. As can be observed in Fig. 4, the microwave reactor
that there is a high relationship between the yield of products with had a maximum power load of around one per hour per kilowatt which
temperature stability during pyrolysis process. Another reason is the illustrates the magnitude of WHSV is approximately equivalent to the
increase of pressure inside the reactor that causes the pyrolysis volatiles magnitude of the maximum output microwave power. This means that
product being forced out of the reactor toward condensation and when the microwave reactor has an output power of 3 kW, the
product collection systems, as was also observed in other cases in a maximum WHSV is also around 3 per hour for obtaining the power load
previous study [18]. The increase in pressure is due to an increase in of one per hour per kilowatt. Furthermore, when the amount of absorber
volatile volume from the process of phase change of liquid into vapor that can be accommodated in the reactor is about 0.9 kg, the feed flow
resulting from the cracking of WCO into shorter molecules. rate that can be processed is 2.7 kg/h. It should be noted that this is a
Fig. 4 also shows that the increase of feed flow rate not only tended to rough estimate and may only apply for waste oil processing in micro­
produce more amounts of bio-oil but also slightly higher number of solid wave reactor with charcoal as absorber material under the investigated
products. This might be related to an increase in the volatile volume and condition. Nevertheless, this approach seems to be applicable for eval­
pressure in the reactor as described earlier and also associated to a uating the results of a previous study [18] in which the optimum py­
decrease in cracking reaction intensity of WCO that flows at a high rolysis process is obtained at a WHSV of 5 per hour with an output
quantity into the reactor especially for feed flow rates over 0.204 kg/h. microwave power of 5 kW, showing the system has also a power load of
This condition provides an opportunity for the formation of solid one per hour per kilowatt.
products both in the form of char and un-pyrolyzed WCO.
The relationship between yield of bio-oil with WHSV and WHSV/MP 3.2.2. Effect of temperature
is also provided in Fig. 4. The WHSV is calculated as the feed flow rate of Figs. 5 and 6 show the yield of products generated from pyrolysis of
WCO divided by the mass of absorber material. This is one of the

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S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Table 2
Comparison of yield of bio-oil from pyrolysis of WCO.
Heating method Pyrolysis process Max. carbon chain of feedstock Temperature (oC) Bio-oil yield (wt.%) Reference

Microwave Continuous C30 450 64

500 77 Present study
550 72
Microwave Batch C18 450 70
500 69 [19]
550 66
Electric resistance Batch C22 550 8
[25]
800 80
Electric resistance Batch C18 500 56
550 78 [26]
600 72
Electric resistance Continuous C18 450 73
500 62 [23]
550 35
Electric resistance Continuous – 500 63 [24]

waste and fresh cooking oils, respectively, at different process temper­ At a pyrolysis temperature of 550 ◦ C, the yield of bio-oil dropped to
atures. Pyrolysis experiments were performed at temperatures above 72 wt.% and 58 wt.% for WCO and FCO, respectively. The reduction of
350 ◦ C. This is caused by the fact that only small amounts of pyrolysis- bio-oil yield at 550 ◦ C is might be due to the secondary cracking and
volatile were generated below 350 ◦ C. A previous study reported that at carbonization reaction of WCO and FCO to generate higher quantities of
a temperature of 350 ◦ C, a lot of un-pyrolyzed oils product (77 wt.%) incondensable gas and carbonaceous char products. This result can be
and small amounts of bio-oils and gases have been obtained [19]. This inspected from the increased yield of both the pyrolysis gas and char
phenomenon was also reported in other study that evaporation started at products. At high pyrolysis temperatures of 550 ◦ C and above, the yields
325 ◦ C for waste cooking oil [21]. of gas product increase due to secondary cracking reactions. It was also
The pyrolysis product of bio-oil is directly proportional to the tem­ possible that carbonization has also taken place during the pyrolysis
perature rises. The increase of temperature accelerates the rate of process at temperatures of more than 500 ◦ C and this has led to an in­
decomposition of raw materials. It was found that temperature of lower crease in the yield of carbon char products of 1 wt.% and 2 wt.% for
than 400 ◦ C; less bio-oil was obtained compared to other temperature WCO and FCO, respectively.
variations for both WCO and FCO. It might be due to the incomplete Table 2 shows that the bio-oil obtained from microwave-enhanced
decomposition of the samples lead to less oil converted into bio-oil and pyrolysis exhibited higher yields at relatively lower temperatures
gas. This incomplete decomposition impacts on the high yield of solid compared to those produced from WCO pyrolyzed under conventional
products. In this condition, the solid product obtained refers to a mixture electric heating. Pyrolysis of WCO under conventional electric heating
of un-pyrolyzed oil with charcoal. needed higher temperatures in order to obtain the maximum bio-oil
The highest yields of bio-oil product in this work were obtained at yield. These results indicate that faster thermochemical decomposition
temperature of 500 ◦ C for both WCO and FCO. It was influenced by rate of raw materials can be achieved with the assist of microwave
decomposition rate in the pyrolysis process where the heat generated at heating. Table 2 also indicates that continuous pyrolysis processes
this temperature was enough to break chemical bonds of raw material provided better performance compared to batch processes. This
that the volatile content was evaporated. The faster the rate of chemical happened because the continuous pyrolysis process is able to perform
decomposition, the faster the breakdown process of chemical molecules fast or flash pyrolysis process which is generally applied for bio-oils
of raw material. At that condition, volatile compounds of raw materials production as also reported in other studies by Chang et al. [23] and
rapidly evaporated and tended to form bio-oil as the main product. The Chiaramonti et al. [24].
yield of bio-oil increased as the increase of reaction temperature, and In this study, the largest yield of bio-oil product was achieved at
then decrease after being reached the maximum point [22]. relatively high temperature of 500 ◦ C. This is mainly due to the carbon

Fig. 7. Chromatogram of WCO from GC–MS analysis.

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S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Fig. 8. Chromatogram of FCO from GC–MS analysis.

The GC–MS chromatograms of the feedstock (WCO and FCO) are pre­
Table 3
sented in Figs. 7 and 8, respectively. Identification of the characteristic
Chemical composition (wt.%) and HHV (MJ/kg) of the feedstocks.
peaks was carried out by employing NIST MS 2.0 software to their
Compound Formula WCO FCO spectrum. The results showed that response values and peak identifi­
n-Hexadecanoic acid C16H32O2 37.43 36.81 cation provided a high accuracy of over 99 % (or less than 1 % error)
Trans 13-Octadecanoic acid C18H34O2 42.02 44.26 that is within the allowable level of accuracy. The identified molecular
Oleic acid C18H34O2 18.32 –
compounds for both feedstocks are also provided in Table 3.
Squalene C30H50 2.23 –
1-Hepatriacotanol C37H76O – 12.25 In general, both samples mainly composed of palmitic and oleic
Z-(13,14-Epoxy/tetradec-11-en-1-ol acetate C16H28O3 – 6.67 acids. The data showed that waste cooking oil contained about 37.43 wt.
HHV 39.3 39.1 % palmitic acid and 60.34 wt.% oleic acid, while for fresh cooking oil
there were 36.81 wt.% and 44.26 wt.%, respectively. This is consistent
to a previous study that majority of fatty acid of fresh and waste cooking
chain of waste cooking oil employed is longer than that of raw materials
oils is composed of oleic and palmitic acids [19]. Fresh and waste
used in other studies. This proved that the longer the carbon chain in the
cooking oils also consisted of high carbon and hydrogen elements. Waste
oil sample, the higher the pyrolysis temperature is needed.
cooking oil had relatively short-chain of hydrocarbons than fresh
cooking oil. This is due to the repeated frying process of waste cooking
3.3. Chemical composition of the feedstock and bio-oil product oil causing carbon chain cracking. The high number of hydrocarbons in
fresh and waste cooking oils indicated that both of the feedstock could
3.3.1. Feedstock composition be pyrolyzed and converted into alternative fuel.
Gas chromatography-mass spectrometry (GC–MS) is an analytical
method that commonly applied for identification of different substances 3.3.2. Bio-oil product composition
within a sample in which the sample is heated in order to separate its There were different chemical compounds and compositions of bio-
chemical elements and to identify their molecular level contributions.

Fig. 9. GC–MS chromatogram of bio-oil from WCO produced at 500 ◦ C.

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S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Fig. 10. GC–MS chromatogram of bio-oil from FCO produced at 500 ◦ C.

Table 4
Chemical composition (wt.%), carbon component (wt.%), and HHV (MJ/kg) of the bio-oils.
WCO FCO

400 C*
◦
450 C
◦
500 C
◦
550 C
◦
400 ◦ C* 450 ◦ C 500 ◦ C

Compound
Aliphatics
Alkanes 55.50 49.85 31.38 40.14 50.42 71.91 36.91
Cycloalkanes 4.78 5.32 – 5.56 4.13 3.00 4.31
Alkenes 39.72 44.83 58.25 45.05 45.45 24.07 53.34
Alkuna – – – – – – 5.44
Aromatic – – 10.37 9.26 – 1.02 –
Sum 100 100 100 100 100 100 100
Carbon component
C5-C9 8.26 8.93 12.91 22.09 7.32 11.26 7.83
C10-C15 43.78 54.39 46.19 34.42 52.41 44.97 44.74
C16-C20 47.96 36.68 39.48 43.50 35.71 40.95 39.54
C21-C25 – – 1.42 – 2.35 – 5.83
C26-C30 – – – – 2.21 2.82 2.06
Sum 100 100 100 100 100 100 100
HHV 44 46 46 46 – – –
*
Data source: [20].

oil from waste and fresh cooking oils for each pyrolysis temperature. compounds produced at 500 ◦ C also showed that the molecular break­
This is due to they have different feedstock composition and rate of down process takes place with high intensity.
decomposition. Based on the yield of bio-oil discussed previously, the The bio-oils product of waste and fresh cooking oils pyrolysis con­
largest yield of bio-oil product was achieved at pyrolysis temperature of tained many hydrocarbon compounds. There were several compounds
500 ◦ C. So that, this condition was used for bio-oils chromatogram in bio-oil such as alkanes, alkenes, cycloalkanes, aromatic, and other
evaluation. The bio-oils GC–MS chromatograms produced at 500 ◦ C for unknown components. The main compounds of bio-oils generated at
both waste and fresh cooking oils are depicted in Figs. 9 and 10, different process temperatures for WCO and FCO are tabulated in
respectively. As can be observed in Fig. 9, bio-oil product of WCO mainly Table 4.
has domain compounds of C6-C22 bonds. This is achieved from the This study showed that the dominant compounds obtained were
cracking of WCO compounds that have longer carbon bonds from C16 to aliphatic hydrocarbons (90− 100 wt.%) and slightly aromatic hydro­
C30. carbons (1− 11 wt.%). Alkanes and alkenes were found to be the biggest
The longer the carbon bond in the oil sample, the more compounds aliphatic hydrocarbons in each bio-oil product. The aliphatic hydro­
are produced. It was shown by the number of bio-oil compounds pro­ carbons in this study also consisted of small amounts of alkuna and
duced from fresh cooking oil sample (hydrocarbon chain ≤ 37) more cycloalkanes. Alkuna or alkyne of 5.44 wt.% was only found in bio-oil
than that of used cooking oil sample (hydrocarbon chain ≤ 30). For from FCO cracking at a temperature of 500 ◦ C. The formation of
instance, the highest number of compounds produced from waste Alkuna is very possible to occur at high temperatures. In the presence of
cooking oil was obtained at a temperature of 500 ◦ C, where there were heat, saturated hydrocarbons can eliminate hydrogen gas to form un­
25 peaks with 18 identified compounds. Among them, 1-Tetradecene saturated hydrocarbons. This means that when saturated hydrocarbons
was the most common compound found in bio-oil which occupies of alkanes or alkenes are heated to high temperatures in absence of air, a
14.20 wt.%. In the meantime, at the same temperature of 500 ◦ C, there mixture of saturated and unsaturated hydrocarbons (e.g. alkenes and
were 28 peaks bio-oil compounds from fresh cooking oil sample as alkuna) is formed [27–29]. This condition then caused a reduction in the
shown in Fig. 10. Twenty-five compounds were identified at this tem­ alkane’s content at 500 ◦ C as shown in Table 4. Other studies suggest
perature, in which the bio-oil compounds were more dominated by 1- that the formation of alkynes can occur at relatively lower temperatures
Pentadecene which occupies 11.10 wt.%. The high number of with the aid of catalysts such as silica, alumina or carbonaceous

8
S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Table 6
Comparison of fuel properties of green-diesel fraction with fossil diesels (Per­
tamina Dex and Solar).
Results

Green- Pertamina Dex Solar**

Parameters Units
Diesel *
fraction Min max min max

Density @ 15 ◦ C kg/l 0.8325 0.820 0.860 0.815 0.860

Kinematic mm2/s 2.620 2.0 4.5 2.0 4.5
viscosity @
40 ◦ C
Kinematic mm2/s 1.122 – – – –
viscosity @
100 ◦ C
Total acid mgKOH/ 0.2 – 0.3 – 0.6
number g
o
Flash point C 54.5 55 – 52 –
PMCC
o
Pour point C − 9 – 18 – 18
o
Final boiling C 340 – 370 – >370
point
Higher heating MJ/kg 41.14 – 56.67 – 43.04
value
Cetane index – 50.3 48 – 45 –
Fig. 11. Average yields of fuel fractions produced from microwave distillation *
of bio-oil from WCO. Data source: [35].
**
Data source: [36].

materials [30]. In addition, there was the occurrence of components

3.4. Bio-oil distillation and green-diesel properties
cracking to generate several aromatic structures, probably originated
from the cyclization and aromatization reactions during the pyrolysis
The bio-oil produced from previous microwave-assisted pyrolysis
process [19].
process of cooking oil particularly WCO was further processed under
Alkanes obtained ranged from 30− 72 wt.%, while alkene ranged
microwave-assisted distillation reactor for obtaining the biofuel frac­
between 24− 58 wt.%. Liquid hydrocarbons of alkanes from nonane
tions. The oil sample for distillation processes was bio-oil produced at
(C9H20) to nonadecane (C19H40) derived from thermal decomposition of
450 ◦ C as it had the highest green-diesel content. The result of fuel
WCO were found to be the compounds with higher concentration in bio-
fractions obtained from microwave distillation process is presented in
oil. In the meantime, compared to alkanes, alkenes consisted of shorter
Fig. 11.
liquid hydrocarbon chain compounds, especially C9-C16. Hexadecene
The distillation results as given in Fig. 11 indicated that from a total
(C16H32) and tetradecene (C14H28) were the most dominant compounds
of 500 g of bio-oil produced around 52 g of gasoline fraction, 220 g of
in alkene with a range of 8− 15 wt.%. The results also showed that bio-
kerosene or jet fuel fraction, 215 g of green-diesel fraction, and only 13 g
fuels from FCO raw material were mainly composed of longer carbon
of heavy fuel fraction. The results showed that heavy fuel fraction and jet
chains compounds in comparison to those from WCO. The bio-oils
fuel fraction were found to be the lowest and the highest fuel fractions in
composed of nonane (C9H20) to octadecane (C26H54) compounds for
bio-oil, respectively. Moreover, in terms of percentage of the yield, the
alkanes group and 1-Nonene (C9H18) to 1-Docosene (C22H44) com­
average gasoline fraction was around 10 wt.%, jet fuel was 44 wt.%,
pounds for alkenes group.
green-diesel was 43 wt.%, and heavy fuel was about 3 wt.%. The ob­
The obtained aliphatic hydrocarbon compounds have a high per­
tained fuel fractions are in accordance with the bio-oil composition re­
centage of 90− 100 wt.%. At low temperatures of 400 ◦ C, the aliphatic
sults in which the bio-oil content was more dominated by tetradecane, 7-
hydrocarbon compounds of each raw material have a percentage of
hexadecene, (Z)-, and nonadecane with an amount of 12.35 wt.%,
100 wt.%. Aromatization reaction using WCO raw material occurred at
13.05 wt.%, and 17.68 wt.%, respectively as previously shown in Fig. 9.
temperatures of 500 ◦ C (10.37 wt.%) and 550 ◦ C (9.26 wt.%), while
These compounds are classified as kerosene/jet fuel and diesel fractions.
FCO occurred at a temperature of 450 ◦ C (1.02 wt.%). Bio-oil products
Table 5 shows that the bio-oil produced under microwave-enhanced
with high aliphatic hydrocarbons content have the potential as fuel and
pyrolysis exhibited higher quantities of C10-C19 light fractions compared
chemical raw materials [18]. In addition, the highest content of
to those attained from the oils pyrolyzed under conventional electric
green-diesel (C10-C15) of bio-oil was achieved at a temperature of 450 ◦ C
heating. Meanwhile, pyrolysis of oil under conventional electric heating
of 54.39 wt.% for WCO and 400 ◦ C of 52.41 wt.% for FCO raw materials.
tended to have more amounts of heavy hydrocarbon fractions. This
showed that microwave irradiation intensity might be contributed in
enhancing cracking reactions that could not be attained with

Table 5
Comparison of fuel fractions in the bio-oil from different oil feedstocks.
Heating method Oil feedstock Gasoline (wt.%) Kerosene/Jet fuel (wt.%) Diesel (wt.%) Heavy oil (wt.%) Reference

Microwave Waste cooking oil 10 44 43 3 Present study

Electric resistance Waste cooking oil 40 – 34 2 [23]
Microwave Waste automotive engine oil 69 16 15 4 [18]
Electric resistance Waste machinery oil 38 1 14 53 [31]
Electric resistance Scrap tire + waste lubricant oil 40 18 13 34 [32]
Electric resistance Used sunflower oil 23 – – 45 [33]
Electric resistance Waste cooking oil – – – 75 [34]

9
S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Table 7
Energy consumption and energy recovery evaluation in bio-oil production from pyrolysis of WCO under microwave irradiation.
EWCO EPy EBO EPy/EWCO EBO/EWCO EP,ratio EP,in EP,loss EP,recovery
Process condition
(kJ/h) (kJ/h) (kJ/h) (%) (%) (kJ/h) (kJ/h) (kJ/h) (%)

Temperature (oC)
400 4009 1248 2563 31 64 2.1 5257 2694 2563 49
450 4009 1560 2993 39 75 1.9 5569 2575 2993 54
500 4009 1872 3593 47 90 1.9 5881 2287 3593 61
550 4009 2340 3378 58 84 1.4 6349 2971 3378 53
WCO feed rate (kg/h)
0.051 2004 936 1466 47 73 1.6 2940 1474 1466 50
0.102 4009 1560 2993 39 75 1.9 5569 2575 2993 54
0.204 8017 1755 6015 22 75 3.4 9772 3757 6015 62
0.306 12,026 2574 8713 21 72 3.4 14,600 5887 8713 60

conventional heating [17]. These results indicate that the application of 3.5. Energy consumption and recovery
microwave heating for thermochemical decomposition of materials
could solve the limitation of conventional heating, in which The assessment of energy consumption and energy recovery provides
microwave-heated pyrolysis can enhance cracking reactions to break valuable information that illustrates the energy efficiency of the process,
longer hydrocarbon chains into shorter ones. Moreover, the type of oil including WCO pyrolysis and bio-oil distillation under microwave irra­
raw material used also affects the composition of the bio-fuels fraction as diation used in this study. In addition, this information can also be used
they actually have different hydrocarbon content. to evaluate whether the process is feasible to be applied on a larger scale.
The green-diesel fraction was then analyzed for obtaining its fuel For this purpose, a microwave input power (MPin) of 1.3 kW was used as
properties such as density, kinematic viscosity, total acid number, flash a basis for calculating electrical energy consumption and only the HHV
point, etc. Table 6 shows green-diesel fraction properties and its com­ of bio-oil and green-diesel products were included in the assessment.
parison with two grade of fossil diesel fuels that are commercially Table 7 shows estimates of the energy recovery compared with the
available in Indonesia called Pertamina Dex (high grade diesel fuel) and energy consumption in bio-oil production through WCO pyrolysis under
Solar (low grade diesel fuel). microwave irradiation both at various temperatures and feed flow rates.
According to Table 6, the green-diesel fraction originated from waste It should be noted that the effects of temperature on WCO pyrolysis were
cooking oil showed good fuel properties agreement to that of the fossil performed at a fix feed flow rate of 0.102 kg/h, while the effects of feed
diesels. The density, viscosity, and pour point of the green-diesel frac­ flow rate were studied at a constant temperature of 450 ◦ C. Assessment
tion were found within the prescribed range of diesels given by PT. of the energy content of WCO (EWCO), the electrical energy needed for
Pertamina, Indonesia. The flash point of the green-diesel fraction was pyrolysis process (EPy), and the energy content of bio-oil (EBO) were
found to be higher than that of Solar and quite close to that of Pertamax adapted from previous studies [18,19] as the following equations:
Dex. The relatively high flash point suggests that most of the components
EWCO = HHVWCO × WCO feed rate (4)
with lower boiling point in the bio-oil had been removed, although the
final boiling point of the green-diesel fraction was quite lower than that
EPy = MPin × ˝on˝ duration of magnetron during pyrolysis process (5)
of Pertamax Dex and Solar.
Another important fuel property of the fuel is heating value that is YBO
also listed in Table 6 in term of higher heating value (HHV). The HHV of EBO = HHVBO × WCO feed rate × (6)
100
fuels represents the gross energy output of combustion in the engine
Equations above were then used to calculate the energies involved in
combustion chamber. As shown in the table, the HHV of green-diesel
pyrolysis process as follows:
fraction was relatively lower compared to that of the fossil diesels.
The lower HHV of green-diesel fraction might be due to the fuel con­ EBO
EP,ratio = (7)
stituent compounds being dominated by lighter hydrocarbons which EPy
have low heating values. This also closely related to the final boiling
point of compounds in the green-diesel fraction which is lower than that EP,in = EWCO + EPy (8)
of fossil diesel fuels.
Total acid number figures the quantity of acidic chemicals in the fuel EP,loss = EP,in − EBO (9)
oils and normally used as an indicator of the quality of fuel oils. The
acidity of fuel oils is also represented by the presence of oxygen in fuel EP,recovery = EP,in − EP,loss (10)
oils. Lower acid content is needed to avoid severe corrosion in the fuel As shown in Table 7, on the one side, the electrical energy needed for
supply system and in the combustion chamber. In this work, total acid pyrolysis process (EPy) increased with the increase of reaction temper­
number of the green-diesel fraction was found to be relatively low which ature, ranging from 2563 kJ/h to 3378 kJ/h that is equivalent to 31 %–
is comparable to that of Pertamax Dex, showing it has good fuel quality 58 % of the HHV of WCO. At higher pyrolysis temperature, more elec­
of total acid number property. Moreover, cetane index of the green- trical energy was consumed as it needed to supply sufficient heat to
diesel fraction was higher than that of Pertamax Dex and Solar. The sustain the reaction temperature. On the other side, the electrical energy
quality of diesel fuels is also highly associated to the cetane index. The usage for pyrolysis process with regard to HHV of WCO decreased with
cetane index illustrates how fast fuel can be ignited in the compression the increase of feed flow rate under the investigated condition. The
chamber. This shows that the fuel which has a high cetane index will lower electrical energy usage at higher feed flow rates might be due to
generally combust faster in the engine combustion chamber. As such, the heat generated by the microwave can be more effectively used to
engine working conditions are usually quieter and smoother and pro­ heat the feed of WCO to be converted into bio-oil. The result also showed
duce less harmful emissions. that the energy content of waste cooking oil can be recovered well as
indicated by the high energy content of bio-oil which is proportional to
the increase in the yield of bio-oil products. In general, the bio-oil
products contained about 64 %–90 % of the energy content of waste

10
S. Anis et al. Journal of Analytical and Applied Pyrolysis 154 (2021) 105014

Table 8
Energy consumption and energy recovery evaluation in green-diesel production under microwave irradiation.
WCO feed No EWCO EPy EBO EDis EGD EGD/EBO ED,ratio ED,in ED,loss ED,recovery
rate (kg/h) of runs (kJ/h) (kJ/h) (kJ/h) (kJ/h) (kJ/h) (%) (kJ/h) (kJ/h) (kJ/h) (%)

0.051 16 32,069 14,976 23,460 3120 9029 39 2.9 73,625 64,596 9029 12
0.102 8 32,069 12,480 23,948 3120 9217 39 3.0 71,617 62,400 9217 13
0.204 4 32,069 7020 24,061 3120 9260 39 3.0 66,269 57,009 9260 14
0.306 3 36,077 7722 26,139 3120 10,060 39 3.2 73,059 62,999 10,060 14

cooking oil. heat integration and recovery are also carried out. This is certainly ex­
Table 7 also shows that the bio-oil products produced from the pected to increase the amount of energy that can be recovered from the
applied pyrolysis process have much higher energy content than the pyrolysis and distillation system. Thereby, the pyrolysis and distillation
electrical energy used to carry out the pyrolysis process. This is indicated processes of WCO under microwave irradiation appear feasible to be
by a good energy ratio in the range of 1.4–3.4, where the energy ratio applied in producing high energy content of liquid bio-fuels.
increased significantly with the increase of feed flow rate. In addition,
the estimation results showed that although in small-scale equipment, 4. Conclusion
the energy recovery was quite high in the range of 49 %–62 % of the
input energy involved in the pyrolysis process. Thus, regardless of the Liquid bio-fuels from waste cooking oil were successfully produced
assumptions used in this energy estimation, the pyrolysis process of under microwave-assisted pyrolysis and distillation. In contrast to the
WCO using a microwave reactor appears to be able to produce high effect of feed flow rate, pyrolysis temperature and type of cooking oils
energy content of bio-oil and high energy recovery in the system. played a prominent role in the yield and composition of bio-oil. Both
Table 8 shows estimates of the energy recovery compared with the WCO and FCO required higher pyrolysis temperatures to effectively
energy consumption for green-diesel production. In this work, there break the long-carbon chain of the liquid sample. Compared to 500 ◦ C,
were two main processes applied for the production of green-diesel from although pyrolysis temperature of 450 ◦ C provided a relatively lower
WCO, namely microwave-assisted pyrolysis of WCO to produce bio-oil, bio-oil yield, the bio-oil product contained more amounts of jet fuel and
and microwave-assisted distillation of pyrolytic bio-oil to separate green-diesel fractions. The fuel properties of green-diesel fraction
green-diesel fraction. So, these two processes are involved in the esti­ showed good agreement to that of the fossil diesels. Based on energy
mation of energy consumption and energy recovery. It should be noted estimates, application of microwave irradiation for pyrolysis and
that each distillation process used about 500 g of bio-oil, so that a distillation processes showed high benefit for converting waste cooking
minimum of 800 g of WCO feed is needed for bio-oil production in the oil into liquid bio-fuels, in particular for the production of green-diesel.
pyrolysis processes. In this evaluation, the pyrolysis process is assumed
to be carried out several times depending on the feed flow rate used. As a CRediT authorship contribution statement
consequence, the EWCO, EPy, and EBO values in the table are then
multiplied by the number of runs. While the electrical energy needed for Samsudin Anis: Supervision, Conceptualization, Methodology,
distillation process (EDis), the energy content of green-diesel (EGD) and Writing - review & editing. Rais Alhakim: Investigation, Data curation,
others are calculated based on the following equations: Writing - original draft. Wahyudi: Visualization, Validation. Ahmad
EDis = MPin × ˝on˝ duration of magnetron during distillation process (11) Mustamil Khoiron: Methodology, Formal analysis. Adhi Kusumastuti:
Validation, Writing - review & editing.
( )
YBO × GD Fraction
EGD = HHVGD × WCO feed rate × no. of runs ×
100
Declaration of Competing Interest
(12)

EGD The authors report no declarations of interest.

ED,ratio = (13)
EDis
Acknowledgements
ED,in = EWCO + EPy + EBO + EDis (14)
The authors gratefully acknowledge the Applied Research Grant (No.
ED,loss = ED,in − EGD (15) 87.18.3/UN37/PPK.3.1/2019) awarded by the Directorate of Research
and Community Service (DRPM) of the Directorate General of Research
ED,recovery = ED,in − ED,loss (16) and Development Strengthening, Ministry of Research, Technology and
As shown in Table 8, the green-diesel fuel produced from the applied Higher Education of the Republic of Indonesia to carry out this work.
distillation process has a much higher energy content than the electrical
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