Environmental Science and Pollution Research

https://doi.org/10.1007/s11356-020-09068-6

SHORT RESEARCH AND DISCUSSION ARTICLE

Feasibility of biodiesel production from waste cooking oil: lab-scale

to pilot-scale analysis
Kubendran Devaraj 1 & Yuvarani Mani 1 & Salma Aathika Abdur Rawoof 1 & Amudha Thanarasu 1 &
Anuradha Dhanasekaran 2 & Sivanesan Subramanian 1

Received: 24 May 2019 / Accepted: 27 April 2020

# Springer-Verlag GmbH Germany, part of Springer Nature 2020

Abstract
In the last few decades, consciousness of fossil fuel resources and increased environmental concerns have given the need for
emergence of alternative fuel. Biodiesel is one of the potential renewable energies produced from edible and non-edible biomass
which could be a potential alternative for petrol-derived diesel. In this work, initially the process of biodiesel production from
waste cooking oil using potassium hydroxide as catalyst and the process parameters were studied in laboratory. The maximum
biodiesel yield of 97% was attained at 75 °C with 1 wt% catalyst concentration and oil-methanol molar ratio of 1:06 at 350 rpm
and 90 min. Also, these process conditions were used for biodiesel production in the pilot plant and obtained 97% yield. Overall,
mass balance for the pilot plant was studied to analyze the product yield loss. The fatty acid methyl ester formation in the plant
was confirmed by characterization with FTIR and 1H NMR. Further, the quality of biodiesel produced was compared for its
physiochemical properties with the ASTM standards.

Keywords Potassium hydroxide . Transesterification . Fatty acid methyl ester . Free fatty acid

Introduction The raw material costs and limited availability of vegetable

Rapid industrialization and urbanization lead to the depletion
of fossil fuel and therefore attract researchers on alternative
fuels (Periyasamy et al. 2016). Biodiesel is a realistic alterna-
tive of diesel fuel which is produced by transesterification of
animal fat, algae oil, microbial lipid, and non-edible and edi-
ble oils (Aathika et al. 2018; Yuvarani et al. 2017).
Comparatively, it has lower emission profile than petroleum
diesel and could be used in engines without major modifica-
tion. Also, it is renewable and biodegradable and reduces
emission of greenhouse gases in the atmosphere
(Nilavunesan et al. 2017).
Responsible editor: Ta Yeong Wu
* Kubendran Devaraj
devakubendran@gmail.com
* Sivanesan Subramanian
sivanesh1963@gmail.com
1
Department of Applied Science and Technology, Alagappa College
of Technology, Anna University, Chennai 600025, India
2
Department of Biotechnology, Alagappa College of Technology,
Anna University, Chennai 600025, India
oil feedstock are some of the critical issues for biodiesel pro-
duction (Devaraj et al. 2017). Biodiesel produced from virgin
edible and non-edible vegetable oils has increased the total
manufacturing cost up to 75%, resulting in an increase in the
cost to approximately 1.5 times higher than the commercially
available diesel (Sinha and Murugavelh 2016). Alternatively,
the cost of used waste cooking oil (WCO) is 2–3 times lower
than of virgin vegetable oils. Utilizing the WCO for biodiesel
production has reduced the total manufacturing cost hugely
(Wang et al. 2019). Eighty percent of WCO is produced from
restaurants, food industry, and household use. The disposal of
WCO to the environment causes pollution; for example, a
million liters of fresh water can be contaminated by just a liter
of WCO and the reuse of fried oil leads to health issues for
humans. Thus, biodiesel from waste cooking oil can eliminate
the environmental issues and provide many options for waste
management (Kubendran et al. 2017).
The availability and potential of WCO bring attention to-
wards large-scale biodiesel production worldwide. According
to Indian statistics, 20% of biodiesel production is from WCO.
Some of the major producers of WCO are the following:
135,000 tons from Canada; 200,000 tons from the UK; and
700,000–1,000,000 tons from EU countries annually,

whereas, in India, WCO biodiesel production capacity is
600,000 tones/year (Enweremadu and Mbarawa 2009). The
WCO below 3% FFA can be directly used for base catalysis
transesterification process. The homogeneous catalyst has the
advantages of faster conversion, lower catalyst requirement,
and higher product formation (Enweremadu and Mbarawa
2009). Still, in many countries, the process of biodiesel pro-
duction is in lab-scale due to uncertainty of process for the
large-scale industrial process that includes the raw materials
and refining cost, ineffective conversion, and low quality of
biodiesel (Devaraj et al. 2018). When compared with other
raw materials, waste cooking oil has an advantage to be used
in large-scale biodiesel production due to its low cost as well
as high conversion percentage with resource availability.
According to previous studies, Bilgin et al. (2015) reported
96% conversion with 1.25% NaOH concentration, 1:12 oil to
alcohol molar ratio, for 120 mins at 70 °C. Also, the maximum
of 96% yield was reported by Encinar et al. (2005) with 1% of
KOH concentration, 1:6 oil to methanol molar ratio for 120
mins at 65 °C. The conversion percentage of triglycerides to
methyl ester is widely determined by 1H NMR (Goyal et al.
2012; Tantirungrotechai et al. 2013; Naureen et al. 2014).
However, all the above processes were done under lab-scale
process conditions. In this study, various process parameters
were studied to obtain maximum conversion of fatty acid
methyl ester (FAME) from waste cooking oil with potassium
hydroxide as a base catalyst in lab-scale and the results were
scaled up to pilot plant.
Methodology
Reagents required
The WCO of 10 L was collected from Anna University can-
teen (13.012936° N, 80.239784° E). To remove the impurities
in the WCO, phosphoric acid (0.3% v/v) pretreatment was
carried out which precipitates solid particle, gums, phospho-
lipids, and wax materials, and further, it was purified by fil-
tration with filter cloth (Kubendran et al. 2017). During the
Table 1 Basic fuel properties of pretreated WCO, biodiesel, and petro-diesel
Parameters Waste cooking oil
Density (30 °C, kg m−3) 890
Kinematic viscosity (20 °C and 40 °C, mm2 s−1) 54.8 and 26.2
Acid number (mg KOH g−1) max 0.9
Cloud point (°C) 5 3
Flash point (°C) 251
Water % volume, max 0.5
Carbon residue % mass, max 0.20
Environ Sci Pollut Res
process, the residual moisture content was removed from
WCO by heating. Though there is only very small quantity
of (0.3% v/v) phosphoric acid in the degumming of oil, it does
not much affect the FFA value. Since the waste cooking oil has
FFA ≤ 0.5, the pretreated oil can be directly used for
transesterification reaction. The chemicals used are phospho-
ric acid (SRL) 98%, methanol (Global Chem) 99.5%, and
KOH (MERCK) 99.9%.
Transesterification
The acid value and FFA value of pretreated WCO oil were
found to be 0.99 mg KOH/g and 0.5%. Fat and oils
consisting of FFA less than 3% can be subjected to direct
base catalyzed transesterification process. A total of 100 mL
of pretreated oil taken in a 250-mL flat bottom flask was
connected with reflux condenser and placed on a hot plate
with a magnetic stirrer. Then, potassium methoxide solution
was prepared by adding 1 wt% of KOH in 30 mL of meth-
anol. The process parameters of catalyst concentration, oil to
methanol ratio, temperature, and time were studied for the
maximum biodiesel yield.
Warnquist 3/27 for biodiesel confirmation
The FAME formation in the transesterification process was
observed by the following simple method from laboratory
analysis. In this method, the biodiesel was separated from
glycerol and dissolved in methanol by 1:09 oil to methanol
volume ratios and was homogenized. Then, the mixture was
allowed to precipitate without interruption for 30 mins. The
uncovered tri-, di-, and mono-glycerides present in the biodie-
sel get settle down as precipitate. The FAME was completely
dissolved in methanol to form homogenized mixture. The
amount of precipitate formed directly reflects the unconverted
oil in the biodiesel. The results obtained by this experiment
was confirmed with a previous study done by Kubendran et al.
(2017).
WCO biodiesel Petro-diesel ASTM B100
(Sandhya et al. 2016) (Jindal et al. 2015)
839 834–860 860 to 900
3.0 1.9 to 3.8 1.9 to 6.0
0.03 0.5 0.5
− 8 to 5 − 3.0 to 12
150 60–70 100–170
< 0.01 0.05 0.05
0.01 - 0.050
Environ Sci Pollut Res
Characterization of biodiesel
The basic fuel properties like density, kinematic viscosity, acid
value, flash point, cloud point, water content, and carbon res-
idue were determined to analyze the fuel quality of the oil and
biodiesel. All these properties were tested and the resulting
values were compared with the petro-diesel in accordance
with the ASTM standards as shown in Table 1. The Fourier
transform infrared spectrometry (FTIR BRUKER) and 1H nu-
clear magnetic resonance (1H NMR BRUKER AVANCE III
500 MHz) were used to analyze the chemical changes in the
functional groups and biodiesel conversion percentage,
respectively.
Results and discussions
Effect of various process parameters on biodiesel
production
Direct transesterification process was carried out as the FFA
value of WCO is within the limit. In the transesterification
process, the important process parameters such as oil to meth-
anol ratio (1:03–1:06), catalyst concentration (0.5–1.25 wt%),
temperature (35–75 °C), and stirring speed (250–400 rpm)
were studied to obtain the maximum biodiesel yield. The se-
lected parameter range played a crucial role in obtaining better
conversion of triglycerides into fatty acid methyl esters.
Conversion of FAME will take place by replacing CH2-O−
group in the oil with CH3-O− group in methanol, therefore
maintaining the oil to alcohol molar ratio, an important param-
eter in biodiesel production. Hence, the effect of oil to meth-
anol molar ratio needs to be studied for the maximum conver-
sion. The maximum yield (94%) was obtained at 1:06
oil:methanol ratio for 1 wt% catalyst, 75 °C temperature,
300 rpm, and 90-min reaction time as shown in Fig. 1a. The
required stoichiometric oil to alcohol molar ratio for the
transesterification is 1:03; however, to increase the miscibility
of alcohol molecules with the triglycerides, excess alcohol is
added to keep the reaction in forward direction (Musa 2016).
The catalyst concentration is one of the important parame-
ters in the transesterification process to obtain maximum yield
by varying the catalyst concentration from 0.5 to 1.25 wt% at
300 rpm, temperature 75 °C, and 1:06 oil to methanol ratio.
The maximum of 95% biodiesel yield was achieved with
1 wt% of KOH at 90 min as shown in Fig. 1b. However, lower
catalyst concentration gives lower biodiesel yield due to in-
complete conversion of triglycerides to fatty acid methyl es-
ters. Also, KOH is a cheaper alkaline catalyst with higher
conversion efficiency compared with other catalysts. A com-
parison of the results obtained by previous researchers with
different types of catalyst is given in Table 3. Catalyst concen-
tration more than 1 wt% causes soap formation with oil and
increases the viscosity and decreases the biodiesel yield, there-
by increasing the biodiesel refining cost (Bouaid et al. 2005).
The soap formation can be reduced by removing the moisture
content of oil by heat pretreatment before initiation of
transesterification process. The oil and fat consisting of more
FFA require more catalyst. Similarly, transesterification of oil
followed by esterification requires more catalyst compared
with oil consisting of low FFA value.
Temperature plays an important role in increasing the mis-
cibility of oil with methanol by reducing the viscosity of oil.
During the reaction, the temperature was maintained close to
the boiling point (64.7 °C) of methanol. The reaction has been
carried out in liquid state with use of reflux condenser
equipped with the reactor to avoid the volatility of methanol.
At critical temperature (240 °C) and pressure (78.5 atm),
methanol converts to gaseous phase. Initially, the effect of
temperature (35 °C, 45 °C, 55 °C, 65 °C, 75 °C) was analyzed
with 1:06 oil to methanol ratio, 1 wt% catalyst concentration,
and 350 rpm for 90 mins. From Fig. 1c, it was observed that a
rise in the temperature from 35 to 75 °C led to an increase in
the yield from 68 to 97% after 90 min. Further increasing the
temperature more than 75 °C leads to rapid volatilization of
methanol from the reaction mixture, causing reduction in bio-
diesel yield (Ho et al. 2014). At lower temperature, oil is
highly viscous and therefore, the contact between the oil and
catalyst gets reduced causing lower biodiesel conversion
(Kawentar and Budiman 2013).
The effect of stirrer speed with respect to time on biodiesel
in the range of 250–400 rpm was evaluated with the above
studied conditions as shown in Fig. 1d. The biodiesel yield
was found to be increased from 80 to 97% with increase in the
stirrer speed from 200 to 350 rpm at 90 mins. The results in
Fig. 1d indicates that effective mass transfer takes place be-
tween the oil to methanol and catalytic mixture by increasing
the stirrer speed. The maximum yield was obtained at 350
rpm. No significant increase was obtained in the biodiesel
yield with increased stirring speed of more than 350 rpm.
Biodiesel production in pilot plant and cost analysis
The conditions for biodiesel production in the preliminary
investigation in laboratory were used as a factorial design of
experimental procedure for pilot plant. The process conditions
of temperature 75 °C, catalyst 1 wt%, oil to methanol ratio
1:06, 350 rpm, and time 90 min were maintained during the
transesterification reaction. A schematic diagram of the pilot
plant is shown in Fig. 2. 7 L of WCO, 70 g of KOH, and 2.1 L
of CH3OH were mixed in a 15-L stirred tank reactor (0.6 mm
thick and 26 cm diameter) covered with a steel lid. The system
temperature (75 °C) for the reactor was maintained by digital
thermocouple connected with immersion type heating coil
(3 kW electric heater). The reactor is also fixed with turbine
agitator connected with the digital speed controller for
 Environ Sci Pollut Res

Fig. 1 Effect of biodiesel yield. a Oil to methanol ratio. b Catalyst concentration. c Temperature. d Stirring speed

uniform mixing of reactants and 350 rpm was maintained. To formation, 4 baffles were installed with dimensions of 20 cm
increase the miscibility of reactants and to avoid vortex height, 5 cm breadth, and 3 mm width inside the vessel.
During the transesterification process, the conversion process
Inlet portal
was monitored with warnquist analysis. After 90 mins of
transesterification process, excess methanol from the reaction
Impeller axis
mixture was distillated and recovered. The reaction was
Thermocouple
stopped and glycerol was collected from FAME based on
20 cm

density, from the bottom of the reactor vessel. Residual glyc-

Baffles erol, methanol, and unreacted catalyst should be removed by
31 cm

Impeller washing with warm water to improve the quality of biodiesel.

When cold water is used for purification, emulsification and
Heating coil saponification of biodiesel lead to separation problem. Finally,
Reactor vessel the biodiesel was dried over rotary evaporator to remove the
moisture content and filtered to remove the traces of impuri-
Out let valve ties to improve the overall quality of biodiesel. The overall
biodiesel production process in pilot plant is shown in Fig. 3.
26 cm The mass balance for the pilot plant biodiesel production
Fig. 2 Schematic view of pilot plant process is related with molar weight of vegetable oil including
Environ Sci Pollut Res

Fig. 3 Process flow of biodiesel

production in pilot plant

the molar yield of biodiesel and the molar yield losses pro- human labor, and energy which give income of 2.5 $/L with
duced by molar yields of glycerol and saponification of tri- net profit about 52%. Also, the cost can be further reduced by
glyceride (Bouaid et al. 2005). To calculate the yield loss of government subsidies as WCO is cheaper than petro-diesel.
the process, mass balance of overall process of biodiesel pro- The Ministry of New and Renewable Energy (MNRE) 2018
duction was carried out. By conservation law, process balance has fostered the importance of biofuel blending and has set the
and product yield are calculated and tabulated in Table 2, target as 5% biodiesel blending with diesel by 2030. The min-
showing biodiesel conversion of about 97% and residual istry also focused on (a) improving the domestic production of
losses up to 3%. The results obtained in this study showed biodiesel and bioethanol; (b) developing 2G (second-
better conversion compared with the previous work done in generation) bio-refineries; (c) identifying new biomass for
lab and pilot-scale as shown in Table 3. biofuel generation; (d) developing new technologies for bio-
fuel production; and (e) implementing biofuel blending with
conventional fuel. Additionally, the Indian Government has
Techno-economical cost analysis and government launched biodiesel production program from waste cooking
policies in biodiesel production oil in 100 cities across the country in collaboration with Bharat
Petroleum, IndianOil, and Hindustan Petroleum.
According to survey, the total production cost will get reduced
about 20–45% when the biodiesel is produced from waste
cooking oil rather than edible and non-edible oil, fat, and oil Characterization of WCO and FAME
from waste material (Demirbas et al. 2016; Razon et al. 2020).
The mass balance of biodiesel pilot plant was calculated and FTIR analysis
the input and output are given in Table 2. Mohammadshirazi
et al. (2014) calculated the total cost for the production as 1.2 The changes in the functional group during the conversion of
$/L considering the costs involved with machinery, electricity, WCO into FAME were confirmed by FTIR spectra as shown
in Fig. 4. The functional groups of CH, CH2, and CH3
Table 2 Material balance for pilot plant process stretching vibrations were observed at 3006 cm−1, 2921
cm−1, and 2854 cm−1 and bending vibration of these groups
Reactant Amount (kg) Product Amount (kg)
was found at 1454 cm−1 and 1157 cm−1 (Shankar et al. 2016).
Crude waste cooking oil 6.23 Biodiesel 6.043 Whereas in oil, the strong absorption peak of ester stretches
Methanol 1.512 Glycerol 1.435 from carbonyl C=O and C-O signals at 1742 (Abdul Raqeeb
KOH 0.07 Unconverted oils 0.137 2015). The peak at 717 cm−1 indicates the methylene func-
Soaps 0.05 tional groups (-(CH2)n-). Break down of glycerol back bone
Methanol 0.144 from WCO during transesterification process, reduction of
Water (kg) traces 0.001 CH2-O− group in oil, and formation of functional -O-CH3
Total 7.81 Total 7.81 group in FAME were identified from the changes in charac-
teristic peak at 1157 to 1171 cm−1 in biodiesel confirming the
 Environ Sci Pollut Res

Table 3 Waste cooking oil to biodiesel production

Source Scale Process condition % Conversion Reference

Waste cooking oil Lab Molar ratio 1:05 93.8 (Sodhi et al. 2017)
(Oil to methanol) temperature 60 °C
Catalyst 1 wt% KOH
Time 30–35 min
Waste cooking oil Pilot Molar ratio 1:08 91.0 (Wang et al. 2019)
(Oil to methanol) temperature 45 °C
Catalyst 1.04 wt% CH3ONa
Time 2h
Waste cooking oil Pilot Volume ratio 3:1.7 93.4 (Aghel et al. 2019)
(Oil to methanol) temperature 61.7 °C
Catalyst 8.87 wt% Limescale
Time 2h
Waste cooking oil Pilot Molar ratio 1:06 96 (Devaraj et al. 2018)
(Oil to methanol) temperature 80 °C
Catalyst 3 wt% A-CaO
Time 2h
Chicken fat Pilot Molar ratio 1:06 81 (Alptekin et al. 2014)
(Oil to methanol) temperature 60 °C
Catalyst 1 wt% KOH
Time 2h

conversion. The peaks at 1454 to 1447 cm−1 also confirm the
transformation of ester groups of the waste oil sample into
methyl esters (CO-O-CH 3 ) of the produced biodiesel
(Maqbool 2011).
1 proton intense peck was observed at 3.665 ppm, and the triplet
H NMR analysis for biodiesel
The 1H NMR spectra of biodiesel are given in Fig. 5, which
was analyzed by a Bruker Avance III 600 MHz NMR spec-
trometer. This NMR spectrometer was accredited by both
ISO/IEC 170251 and also ISO Guide 34 for the certification
of organic reference materials. The peaks 1.35 ppm and
1.632 ppm corresponded to a strong signal of methylene pro-
ton and β-carbonyl protons signal, respectively. The peak at
5.32 ppm indicates the olefinic hydrogens. A singlet methoxy
peak at 2.287–2.317 ppm corresponds to alpha methylene
proton (α-CH2). From these results, the presence of methyl
esters was confirmed in biodiesel. The biodiesel conversion
efficiency of 97% was calculated by the following equation:

Oil 2AMe
C ¼ 100 
3CH 2

where C is the conversion percentage of methyl esters from

WCO. From the equation, 2Ame corresponds to methoxy pro-
tons of FAME and 3CH2 is for α-methylene proton.
Biodiesel
T%

Conclusion

The lower cost and good quality fuel produced through waste
cooking oil using KOH as homogenous catalyst were accom-
plished. The suitable conditions for maximum yield are 1 wt%
catalyst concentration, 75 °C temperature, 1:06 oil to metha-
4000 3500 3000 2500 2000 1500 1000 500 nol molar ratio, 90 min reaction time, and 350 rpm. The max-
Wave number cm-1 imum yield of 97% biodiesel was obtained in both lab-scale
Fig. 4 FTIR spectra of WCO and biodiesel and pilot plant. Material balance of the overall process was
Environ Sci Pollut Res
Fig. 5 1H NMR analysis of
biodiesel
also calculated to identify the yield losses. The functional
groups and conversion efficiency are confirmed by FTIR
and 1H NMR spectroscopy. The comparable physiochemical
properties of WCO, diesel, and biodiesel showed biodiesel as
a potential substitute for diesel fuels.
Funding information This research was financially supported by the
Council of Scientific & Industrial Research (CSIR-RA/09/468/0536/
2019 EMR-I), India.
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