Biodiesel Production from Used Cooking Oil Using Coal Low Rating

as Environmentally Friendly Heterogeneous Catalyst

Mustafa

1,3

, Pramila Tumanaidu

2,3

and Muh. Irwan

Department of Chemical Engineering, Politeknik Negeri Samarinda, Jalan Dr. Cipto Mangunkusumo,

Kampus Gunung Lipan Samarinda, 75131, Kalimantan Timur Province, Indonesia

Malaysia-Japan International Institute of Technology (MJIIT), Universiti Teknologi Malaysia,

Jalan Sultan Yahya Petra, 54100 UTM Kuala Lumpur, Malaysia

Razak Faculty of Technology and Informatics, Universiti Teknologi Malaysia, Jalan Sultan Yahya Petra,

54100 UTM Kuala Lumpur, Malaysia

Keywords: Biodiesel, Catalyst, Low Rank Coal, Used Cooking Oil.

Abstract: The increasing need for fossil fuels encourages efforts to meet these needs, by developing alternative fuels

made from renewable raw materials, such as cooking oil from palm oil. Cooking oil is an important

commodity at this time which is quite widespread in Indonesia. The repeated use of cooking oil can produce

used cooking oil that cannot be re-consumed and has a negative impact on the environment. The purpose of

this study was to identify the characteristics of low rank coal with thermal assistance as a heterogeneous

catalyst to produce biodiesel and to study the effect of biodiesel product quality parameters on the

esterification and transesterification processes. Therefore, in this study the production of biodiesel from used

cooking oil was carried out using a low rank coal catalyst, to determine the effect of the amount of catalyst

on the yield and quality of the biodiesel produced. Biodiesel is obtained by reacting oil and methanol, then

low rank coal catalyst is added with various mass additions of 3, 5, 7, 9, and 11 grams. Based on this study,

the best results were obtained with the addition of 7 grams of catalyst, with biodiesel yield reaching 82.20%,

density 864.43 kg/m3, kinematic viscosity 3.60 cSt, water content 0.20%. , the acid number is 0.99 mgKOH/g,

and the methyl ester content is 97.48%. In general, the biodiesel produced has met the requirements of SNI

7182:2015, except for the parameters of water content and acid number.

1 INTRODUCTION

Indonesia is a country with various natural

resources, one of which is oil palm. Based on

statistics from the Directorate General of Indonesian

Plantations, the Volume and Value of Palm Oil

Exports (CPO) 2015-2017 showed a decline from

26,467,564 tons in 2015 to 24,150,232 tons in 2016.

It is estimated that this is due to the large

consumption of domestic palm oil. from the

excessive use of palm oil is the production of waste

palm oil or what is known as used cooking oil or

used cooking oil. To overcome this problem, efforts

are needed to convert used cooking oil into more

viable products, such as biodiesel (Efendi et al,

2018).

Used cooking oil is used cooking oil for frying

which is used repeatedly, with the production and

consumption of cooking oil, the availability of

cooking oil is abundant. Cooking oil is a waste and

when viewed from its chemical composition, used

cooking oil contains carcinogenic compounds that

occur during the frying process. The use of cooking

oil in a sustainable manner can damage human

health, cause cancer, and further reduce the

intelligence of the next generation (Siswani et al,

2012).

For this reason, proper handling is needed so that

this used cooking oil waste can be useful and not

cause harm from aspects of human health and the

environment through a conversion from used

cooking oil into biodiesel (Darmawan, 2013).

Biodiesel is a fuel made from vegetable oil or

animal fat. Biodiesel is a fuel consisting of a mixture

of mono-alkyl esters derived from long-chain fatty

acids, which are renewable sources from nature.

Biodiesel is also known as an environmentally

friendly fuel because it produces relatively cleaner

1072

Mustafa, ., Tumanaidu, P. and Irwan, M.

Biodiesel Production from Used Cooking Oil Using Coal Low Rating as Environmentally Friendly Heterogeneous Catalyst.

DOI: 10.5220/0012064500003575

In Proceedings of the 5th International Conference on Applied Science and Technology on Engineering Science (iCAST-ES 2022), pages 1072-1078

ISBN: 978-989-758-619-4; ISSN: 2975-8246

exhaust emissions than diesel. In addition, the use of

biodiesel is generally easy, because there is no need

to modify the diesel engine (Aziz et al, 2012).

Biodiesel has advantages over petroleum diesel.

Biodiesel fuel is renewable. In addition, it can also

strengthen the country's economy and create jobs.

Biodiesel is an ideal fuel for the transportation

industry because it can be used in various diesel

engines, including agricultural machinery.

According to the Indonesian Palm Oil

Association (Gapki), domestic palm oil

consumption in 2020 was 17.35 million tons or grew

3.6% compared to 2019 of 16.75 million tons. The

development of biodiesel based on used cooking oil

has the opportunity to be marketed, both

domestically and for export. Throughout 2020,

domestic biodiesel consumption increased by about

24% from 5.83 million tons in 2019 to 7.23 million

tons.

In addition, the use of biodiesel as a fuel has

many advantages, including being renewable and

environmentally friendly (reducing vehicle

emissions), being able to lubricate the engine as well

as being a fuel so as to increase the life of the

vehicle, it is safe to store and transport because this

fuel does not toxic and biodegradable and can

reduce dependence on fossil fuels (Balat et al, 2010).

The use of biodiesel as a renewable and

environmentally friendly fuel (reducing vehicle

emissions) is a treatment in the biodiesel

manufacturing process by adding a catalyst and with

ultrasonic assistance in order to increase the

conversion and yield produced.

To make it as a catalyst, thermal assistance is

needed so that the binding mechanism becomes a

simpler hydrocarbon. In line with that, in improving

the quality of biodiesel by using a catalyst, it is also

possible to break the bonds in this case using an

ultrasonic device. Ultrasonic waves can increase the

rate of transesterification of used cooking oil into

biodiesel so that the conversion of used cooking oil

into biodiesel with the use of ultrasonic waves is

higher than other uses.

In the research of Pasae et al., (2019), biodiesel

was produced from used cooking oil using a

heterogeneous catalyst in the form of shells, with

variations in temperature in the calcination and

transesterification processes. The amount of oil and

methanol used was 200 mL of oil and 600 mL of

methanol (1:3 v/v), with the addition of 2 grams of

clam shells as a catalyst. The best results in this

study were transesterification for 3 hours, with a

yield of 66.09%, a density of 853 kg/m

, a kinematic

viscosity of 2.77 mm

/s, an acid number of 0.56

mgKOH/g, and a saponification rate of 201

mgKOH/g. These results have met SNI Biodiesel

7182: 2015 except for the number of acids produced.

In the research of Saputri et al., (2016), biodiesel

methyl esters were made from used cooking oil and

methanol using a heterogeneous catalyst in the form

of rubbing ash with variations of 2, 4, 6, 8, and 10

grams. The best results in this study were achieved

using 10 grams of rubbing ash as a catalyst, with an

acid number of 0.71 mg KOH/g, a total glycerol

content of 0.01%, a density of 0.88 g/cm3, a

viscosity of 47.94 cSt, an iodine number. 66.83 g

/100, water content 0.06%, flash point 249.33ºC,

saponification number 154.84 mg KOH/g, and

methyl ester content 99.5%. The results obtained

have met the biodiesel standard SNI 7182: 2015,

except for the viscosity and water content of the

biodiesel produced.

In the research of Khoiruummah et al., (2020),

activated carbon from acacia wood was impregnated

using KOH and NaOH, then used as a heterogeneous

catalyst in the manufacture of biodiesel from used

cooking oil. This study used variations in the amount

of KOH catalyst/activated carbon, namely 1,3, and

5% w/w oil, as well as variations in temperature,

namely 45, 55, 65, and 75ºC, with an oil-methanol

molar ratio of 1:6. In addition, this study also used

variations in the amount of NaOH catalyst/activated

carbon, namely 3, 4, and 5% w/w oil, with variations

in transesterification temperature of 50, 55, 60, and

65ºC.

The best results on the use of KOH/activated

carbon catalyst is the catalyst variation of 3% w/w

with a transesterification temperature of 65ºC,

which produces a yield of 87.51%. The use of KOH

catalyst/activated carbon produces biodiesel with a

density of 0.7724-0.8585 g/mL, viscosity 4.5485-

5.3672 cSt, acid number 1.1222-2.2444 mgKOH/g,

water content 0.034-0.246% , and a flash point of

150-170ºC.

Meanwhile, the best results on the use of

NaOH/activated carbon catalyst are catalyst

variations of 3% w/w with a transesterification

temperature of 60ºC. In this variation, a yield of

88.35% was obtained. Overall, variations in the

amount of NaOH catalyst/activated carbon produced

biodiesel with a density of 0.89282-0.90722 g/mL,

kinematic viscosity 2.3439-4.1601 cSt, acid number

0.84165-2.2444 mgKOH/g, content water

0.000592-0.071963%, and a flash point of 128-

153ºC. In general, the biodiesel produced has

complied with SNI 7182:2015 on the parameters of

viscosity and flash point. As for the water content

and density parameters, some do not meet SNI

Biodiesel Production from Used Cooking Oil Using Coal Low Rating as Environmentally Friendly Heterogeneous Catalyst

1073

7182:2015. While for the acid number parameter, all

of them do not meet SNI 7182:2015.

Meanwhile, in the research of Oko et al., (2021)

the process of making biodiesel from used cooking

oil was carried out through two reaction stages,

namely esterification and transesterification

reactions. The esterification reaction was carried out

for 1 hour with 100 grams of used cooking oil as raw

material, then 52 grams of methanol and 1 gram of

catalyst were added. Then, in the

transesterification reaction, the mass ratio of CaO

and C was varied in the NaOH/CaO/C catalyst. The

best result of this research is the mass ratio of CaO/C

1:1 with a catalyst of 3% (w/w), with a yield of

83.45% (w/w), kinematic viscosity 2.3 cSt, density

0.8612 g/ mL, water content 0.0273% (w/w), and

acid number 0.2516 mgNaOH/g. All of these results

have met the biodiesel standard of SNI 7182:2015.

In this research, the process of making biodiesel

is carried out through two reaction stages, namely

the esterification reaction which refers to the

research of Oko et al., (2021), and the

transesterification reaction, with a fairly large

oil:methanol ratio of 1:3 (v/v). referring to the

research of Pasae et al., (2019). The addition of large

amounts of methanol is expected to increase the

yield of biodiesel and prevent the kinematic

viscosity from being too high in the final product. In

addition, in this study a different heterogeneous

catalyst was used, namely activated carbon catalyst

from low rank coal impregnated with NaOH. By

using this catalyst, it is expected that the biodiesel

produced is able to meet several criteria in SNI

7182:2015.

2 METHODOLOGY

There are two stages in this research, namely the

production of catalysts from low rank coal and the

production of biodiesel.

 For the production of catalysts from low

rank coal, first prepare low rank coal, then

analyze coal samples with analysis of

proximate, total sulfur, and calorific value,

then carry out the carbonization process in a

furnace at a temperature of 600 º C for 2

hours. After that the carbon is cleaned and

then cooled in a desiccator. Then do physical

activation on the catalyst with a temperature

of 950ºC for 2 hours. Then cool the catalyst

in a desiccator. Then puree the catalyst using

a blender, then filter the catalyst with a size

of -100 +120 mesh. After that, a proximate

analysis was carried out on the low rank coal

catalyst.

 Biodiesel production is the first collected

used cooking oil. Then analyzed the used

cooking oil which includes water content,

density at 40 º C, kinematic viscosity at

40ºC, FFA content, and acid number. If the

FFA level exceeds 1%, then an esterification

reaction is carried out (Hadrah et al., 2018),

which is to react 100 grams of used cooking

oil with 52 g of methanol and 1 g of H2SO4

(Oko et al., 2021). The reaction was

maintained at a temperature of 50-60ºC for

1 hour (Arifin et al., 2016). Then separate the

esterification product in a separatory funnel

for 1 hour, then take the bottom layer for use

in the transesterification reaction (Oko et al.,

2021).

Then carry out a transesterification reaction by

reacting the esterified oil with a catalyst-methanol

mixture at a temperature of 60-70ºC for 1 hour 30

minutes, where the variations of the added catalyst are

3, 5, 7, 9, and 11 grams (Saputri et al., 2016) . The

ratio of oil:methanol used was 1:3 v/v (Pasae et al.,

2019). Then filtering the catalyst while separating the

transesterification results in a separating funnel for 12

hours (Pasae et al., 2019). Then take the top layer and

heat it on a hot plate at a temperature of 60-70ºC for

± 1 hour to remove the remaining methanol

(Khoiruummah et al., 2020). Then wash the biodiesel

produced using aquadest at a temperature of 70-80ºC

until the water becomes clear (Khoiruummah et al.,

2020). After that, the biodiesel is put in the oven for

± 3 hours to reduce the water content (Khoiruummah

et al., 2020). Then save the obtained biodiesel.

The procedure of the process can be described as

shown in the figure below, namely in Figure 1 and

Figure 2.

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1074

Research Procedure

Figure 1: Catalyst Production from Low Rank Coal.

3 RESULT AND DISCUSSION

3.1 Analysis Results

In this study, biodiesel was made from used cooking

oil using a low rank coal activated carbon catalyst,

with variations in the addition of a catalyst of 3, 5, 7,

9, and 11 grams which aims to determine the effect of

the catalyst on the yield of biodiesel produced.

The initial stage of making biodiesel is collecting

used cooking oil, then analyzing the oil with the

parameters of free fatty acid content, color, density at

40ºC, kinematic viscosity at 40ºC, and acid number.

This analysis aims to determine the condition of used

cooking oil before it is used as raw material, as well

as to determine the reaction stage used in the

manufacture of biodiesel.

Figure 2: Biodiesel Production.

Table 1: Results of Low Rank Coal Analysis.

Parameter Analysis Results

Total Moisture, % 37.40

Inherent Moisture, % 14.02

Ash Content, % 2.86

Volatile Matter, % 45.61

Fixed Carbon, % 32.51

Total Sulphur, % 0.98

Calorific Value, kcal/kg 4714

Finish

Catalyst proximate analysis

Proximate analysis of low rank

coal samples

Carbonization (T = 600ºC; t = 2 hours)

Refining and sieving catalyst up to -100 +120 mesh

Physical activation (T = 950ºC; t = 2 hours)

Start

Esterification

T=50-60ºC

t = 1 hour

oil = 100 g

mmethanol = 52 g

m H

= 1 g

FFA < 1%

Yes

Transesterification

T = 60-70ºC

t = 1 hour 30 minutes

Ratio of oil: methanol = 1:3 (v/v)

Variation of catalyst = 3, 5, 7, 9, 11

grams

Separation of

esterification results

(t = 1 hour)

Catalyst and

glycerol

Separation of transesterification results

(

t = 12 hours

)

Methanol

Analysis of the quality of used

cooking

oil

Collecting used cooking oil

Reduction of residual methanol

(T = 60-70ºC; t = ±1 hour)

Aquadest

(T = 70-80ºC)

Biodiesel washing

(T=70-80ºC)

Water va

Reduction of water content

(T = 105-110ºC; t = ±3 hours)

Biodiesel Yiel

Biodiesel characteristic test

Finish

Biodiesel Production from Used Cooking Oil Using Coal Low Rating as Environmentally Friendly Heterogeneous Catalyst

1075

Table 2: Results of Low Rank Coal Analysis (Physical

Activation).

Parameter Analysis Results

Inherent Moisture, % 3.13

Ash Content, % 38.23

Volatile Matter, % 6.64

Fixed Carbon, % 55.13

Table 3: Results of Analysis of Used Cooking Oil

Characteristics.

Parameter Analysis Results

Free fatty acid content, % 4.34

Warna Color

Abnormal (clear

brown)

Density, 40ºC, kg/m3 896.04

Kinematic viscosity, 40ºC, cSt 35.39

Acid number, mgKOH/g 12.57

Table 3 above shows that with the use of 7 grams of

catalyst, the highest yield was obtained at 82.20%.

The quality of the biodiesel produced is as follows:

density: 864.43 kg/m3, kinematic viscosity: 3.60 cSt,

water content: 0.20%, and acid number: 0.99

mgKOH/g.

Table 4: Results of Biodiesel Analysis.

Parameter

Analysis Results

SNI

7182:2015

Catalyst

3 grams

Catalyst

5 grams

Catalyst

7 grams

Catalyst

9 grams

Catalyst

11 grams

Density,

40ºC,

kg/m3

865.18 865.91 864.43 859.42 858.07 850-890

Kinematic

viscosity,

40ºC, cSt

3.59 3.64 3.60 3.58 3.34 2.3-6,0

Moisture

content, %

(v/v)

0.94 0.04 0.20 0.18 0.17 0.05

Acid

number,

mgKOH/g

1.22 1.23 0.99 1.00 0.89 0.5

Yield, % 21.97 35.22 82.20 61.46 69.13 -

4 DISCUSSION

• Effect of Catalyst Amount on Biodiesel Yield

Variations in the addition of catalysts as much as 3, 5,

7, 9 and 11 grams in the transesterification reaction

have a significant effect on the amount of

biodiesel produced, as shown in the figure below:

Figure 2: Graph of the Effect of Catalyst Amount on

Biodiesel Yield.

Based on Figure 2 above, the addition of catalyst

in the range of 3 to 7 grams showed a significant

increase in yield, where the highest yield was

obtained at the addition of 7 grams of catalyst, which

was 82.04%. The addition of a catalyst can reduce the

activation energy, where the more catalyst is added,

the activation energy decreases, so the reaction rate

will increase. With the increase in the reaction rate,

the conversion of used cooking oil into biodiesel is

also getting bigger (Prihanto & Irawan, 2018).

Meanwhile, the addition of 9 and 11 grams of

catalyst actually reduced the amount of biodiesel

produced. This is caused by the formation of soap that

occurs through a saponification reaction, where the

formation of soap can hinder the conversion of oil

into methyl esters. In addition, with the addition of 9

grams of catalyst, the yield of biodiesel produced is

actually lower than that of 11 grams of catalyst.

This is due to imperfect filtering of the catalyst, so

that the catalyst is carried into the product and

increases the amount of impurities. This increase in

the amount of impurities makes the washing process

more difficult, so that a lot of biodiesel is wasted

during the washing process.

According to Bintang et al., (2015), the washing

process and water separation after washing can

reduce the amount of biodiesel produced. The

purification process needs to be carried out properly

because the remaining impurities can affect the

quality of biodiesel, especially on the density

parameter (Faizal et al., 2013)

• Biodiesel Quality

The quality of biodiesel produced can be seen in table

4 with analytical parameters including: density at

40ºC, kinematic viscosity at 40ºC, water content, and

acid number. For the variation of the catalyst with the

highest yield (7 grams), additional analysis was

carried out in the form of methyl ester content to

determine the purity level of the biodiesel produced.

357911

Biodiesel Yield (%)

Amount of Catalyst (grams)

iCAST-ES 2022 - International Conference on Applied Science and Technology on Engineering Science

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Based on table 4, the obtained biodiesel density

ranges from 858.07-865.91 kg/m3. These results have

met the density standard of SNI 7182: 2015 which is

between 850-890 kg/m3.

According to Hadrah et al., (2018), biodiesel with

a density according to SNI standards is able to

produce perfect combustion. In addition to density,

the kinematic viscosity parameter also meets SNI

7182:2015, where the results obtained are in the range

of 3.55-3.87 cSt. These results are within the range

allowed by SNI, namely 2.3-6.0 cSt. The water

content parameters in general do not meet SNI

7182:2015, except for the 5 gram catalyst variation.

High water content can be caused by an incomplete

evaporation process (Kusumaningtyas & Bachtiar,

2012).

Meanwhile, the acid number parameter in general

does not meet SNI 7182:2015. The high acid number

in biodiesel indicates the presence of free fatty acids

in biodiesel produced by the hydrolysis reaction

between oil and water (Zamhari et al., 2021). In

addition, the acid number is also closely related to the

pH of biodiesel (Faizal et al., 2013).

Therefore, to reduce the acid number, the

evaporation process of the water content can be

carried out to prevent the hydrolysis reaction, as well

as carry out neutralization until the biodiesel pH is

close to 7. The parameters of the methyl ester content

were only reviewed for biodiesel with the highest

yield of 82.20% (7 grams of catalyst variation).

Methyl ester analysis was carried out using an FT-

IR instrument, with the resulting IR spectrum as

follows:

Figure 3: IR Spectrum on Biodiesel.

In the spectrum above, it is seen that there is a

sharp absorption at wavelengths 1169.46, 1741.85,

2853.07 and 2922.45 cm-1. Based on the book

Dachriyanus, (2004), the absorption at 1169.46 cm-1

indicates the presence of C-O bonds (1300-1000 cm-

1). Meanwhile, the absorption at 1741.85 cm-1

indicated the presence of an ester group, namely C=O

(1900-1650 cm-1). Then the absorption at 2922.45

cm-1 and 2853.07 cm-1 indicated the presence of C-

H bonds (3000-2700 cm-1). The C=O, C-H and C-O

bonds in biodiesel prove the presence of methyl ester

compounds contained in it. The types of methyl esters

in biodiesel can be identified using the IR spectrum

comparison as follows:

Figure 4: Comparison of the IR Spectrum of Methyl Oleate

(Blue) with Biodiesel (Red).

In Figure 4 above, it can be seen that there is a

comparison between the IR spectrum of biodiesel and

the IR spectrum of methyl oleate under the same

conditions. The IR spectrum of methyl oleate is the

standard spectrum used as a comparison.

According to Siswani et al., (2012), to identify an

unknown compound, a comparison can be made

between the IR spectrum of the compound and the IR

spectrum of a standard compound under the same

conditions. The similarity between the two spectra

being compared indicates that the compound is

identical. The results of the analysis show that

biodiesel has an IR spectrum that is identical to the IR

spectrum of methyl oleate. Therefore, it can be seen

that the methyl ester compound in the biodiesel

produced is predominantly methyl oleate.

Meanwhile, to determine the methyl ester content

in detail, additional analysis was performed using the

FT-IR ATR-PLS-FAME Quantification method,

which refers to the ASTM D7371 and EN 14078

methods. From this analysis, the methyl ester content

was obtained with an estimate of 97.48%. This level

has exceeded the minimum limit determined by SNI

7182:2015 which is 96.5%. Thus, the methyl ester

content in biodiesel has met the SNI 7182:2015

standard.

Biodiesel Production from Used Cooking Oil Using Coal Low Rating as Environmentally Friendly Heterogeneous Catalyst

1077

5 CONCLUSION

1. The more catalyst added to the reaction, the greater

the yield of biodiesel produced, but the yield of

biodiesel will decrease if the addition of catalyst has

reached the optimum condition.

2. The best result of this research is the use of 7 grams

of catalyst, with a yield of 82.20%. The quality of the

biodiesel produced is as follows:

• density: 864.43 kg/m3

• kinematic viscosity: 3.60 cSt

• water content: 0.20%

• acid number: 0.99 mgKOH/g

• methyl ester content: 97.48%.

3. Parameters of density, kinematic viscosity, and

methyl ester content in the biodiesel produced have

complied with SNI 7182:2015. Meanwhile, the

parameters of water content and acid number do not

meet SNI 7182:2015.

ACKNOWLEDGEMENTS

The authors would like to thank the Samarinda State

Polytechnic Research and Community Service Center

(P2M POLNES) which has provided the opportunity

to research, and obtain research funds under the State

Polytechnic Lecturer Research scheme and all parties

who have supported the smooth implementation of

this research. And special thanks to Razak Faculty of

Technology and Informatics, Universiti Teknologi

Malaysia, UTM Kuala Lumpur, Malaysia who helped

push this article.

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