Cleaner Waste Systems 3 (2022) 100049

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Cleaner Waste Systems

journal homepage: www.journals.elsevier.com/cleaner-waste-systems

Statistical optimization of biodiesel synthesis from waste cooking oil using

NaOH/ bentonite impregnated catalyst ]]
]]]]]]
]]

Wisdom C. Ulakpaa,b, , Ruth O.E. Ulakpac,b, Emmanuel O. Eyankwared,b,

⁎

Michael C. Egwunyengae,b
a
Department of Chemical Engineering, Delta State University of Science and Technology, Ozoro, Delta State, Nigeria
b
Department of Petroleum Chemistry, Delta State University of Science and Technology, Ozoro, Delta State, Nigeria
c
Department of Environmental Management and Pollution Control, Nigeria Maritime University, Okerenkoko, Warri, Delta State, Nigeria
d
Department of Gas Engineering, Faculty of Engineering, University of Port-Harcourt, P.M. B 5323, Rivers State, Nigeria
e
Department of Chemical Engineering, Delta State Polytechnic, Ogwashi-Uku, Delta State, Nigeria

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

Keywords: In the present study, bentonite clay supported on sodium hydroxide catalyst was synthesized and its performance
NaOH/Bentonite was evaluated for biodiesel synthesis from waste cooking oil. Impregnation procedure was used for the synthesis
Impregnation of NaOH/bentonite catalyst and the best catalyst was selected based on the yield of transesterification reaction.
Transesterification The catalyst characterization was done by Scanning electron microscope (SEM) to determine the morphology,
Waste cooking oil
and Fourier transform infrared (FTIR) analysis to determine the functional group. The synthesized catalyst was
Biodiesel
used to investigate the synthesis of FAME by varying the response parameters using central composite design of
Response surface methodology
randomized response surface methodology (RSM-CCD). The transesterification was conducted with 9:1 methanol
to oil, 4 wt% catalyst, reaction time of 4 h, temperature of 600 C, with stirring speed of 350 rpm. A biodiesel
yield of 91.2% was obtained in continuous stirring speed of 350 rpm at 60ºC for 4 h and 9:1 methanol/oil molar
ratio with 4 wt% of NaOH/bentonite catalyst. Investigations were done on how different reaction factors af-
fected the biodiesel yield. The developed catalyst was found to have good catalytic activity. The developed
catalyst was significant because it could be easily recovered and reused in successive cycles without significantly
losing catalytic activity. The RSM was found to be a reliable statistical method for creating a respectable em-
pirical model of the relationships between operational parameters and optimal operating conditions for future
prediction. The fuel's physical and chemical qualities were measured, and they were found to be within safe
ranges.

1. Introduction researchers all over the world have been looking at ecologically friendly
and cost-effective renewable energy sources that could substitute diesel
Global energy production is an important economic link that is as a fuel source (Arjun et al., 2019). The technological requirements of
powered by non-renewable energy sources such as fossil fuels (natural diesel fuel may be met by this alternative fuel (Wisdom et al., 2020b).
gas, petroleum, and coal) and nuclear power plants, which account for Fatty acid methyl ester also known as biodiesel is a biodegradable,
90% of non-renewable energy sources. However, there are some chal- non-toxic and renewable fuel manufactured from waste cooking oil,
lenges associated with the utilization of fossil fuels. One of these is vegetable oil, animal fats, and generated using a variety of methods
resource availability (Arjun et al., 2019). As a result of an expanding (Bibin et al., 2019; Jayakumar et al., 2021; Alagumalai et al., 2021; Eko
population and industrialization, energy resources are rapidly depleted, et al., 2021). Compared to diesel, it can cut emissions of carbon dioxide
and replacement takes a long time due to environmental concerns about by as much as 78% because it is a carbon-neutral fuel. The biode-
the harmful CO2 generated when fossil-based fuels are used. CO2 is a gradability of biodiesel is high, according to the studies, while that of
well-known greenhouse gas component, accounting for 72% of total normal diesel is only 24.5% (Syafiuddin et al., 2020; Wisdom et al.,
greenhouse gas emissions. These greenhouse gases absorb longwave 2021). Although, there is a wide range of results from study to study
radiation from the globe, raising atmospheric temperatures. As a result, due to variances in engine design and operating variables, the general

⁎
Corresponding author at: Department of Chemical Engineering, Delta State University of Science and Technology, Ozoro, Delta State, Nigeria.
E-mail address: [email protected] (W.C. Ulakpa).

https://doi.org/10.1016/j.clwas.2022.100049
Received 20 July 2022; Received in revised form 29 October 2022; Accepted 1 November 2022
2772-9125/© 2022 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

opinion is that biodiesel leads to reduced emissions of particulate concentration of free fatty acids, the rate of mixing, the type of alcohol
matter (PM), carbon monoxide (CO), and hydrocarbons (HC), and used, the length of time required for the reaction, the type of catalyst
nearly no sulfate emissions. The use of biodiesel, however, often results used, and the amount of catalyst used. Catalysts used in the transes-
in a 10% increase in NOx emissions (Aydın, 2020; Eko et al.,2021). terification process fall into three categories: homogeneous, hetero-
Diesel fuel is refined from crude petroleum oil, which consists of an geneous, and biocatalytic (Kambiz et al., 2015). Chemical catalytic
assortment of 8–21 carbon atom. On the other hand, biodiesel is made transesterification is commonly used in industry due to its better per-
up of long-chain hydrocarbons with an ester functional group formance and proficiency to catalyze second-generation feedstocks. The
(Hoekman and Robbins, 2012; Rizwanul et al., 2020). homogeneous approach presents significant challenges, such as limited
Biodiesel has many advantages over regular diesel, including its product recovery and unrecyclability of the catalyst. The use of het-
cheaper price, its lower environmental impact, and the fact that it is erogeneous catalyst support resolves these problems while decreasing
produced locally and thus helps the economy. the overall cost of the process (Wisdom et al., 2020a; Venkatesh and
The selection of a suitable raw material is the primary and fundamental Santhosh, 2021).
footprint in the biodiesel making process. High thermo-stability of the catalytic elements contained in sup-
However, non-edible feedstock has shown to be a significant aid in ported catalysts and uniformity of their intercropping distribution (total
this regard because it can be cultivated on a massive scale. Some volume of active surface) have led to their pervasive utilization.
widespread examples include jatropa, jojoba, neem, rubber seed tree, Bentonite clay was selected as the supporting catalyst due to its low cost
and tobacco seed (Sayfa et al., 2020). The food vs fuel question can be and wide accessibility. Bentonite is an aluminum phyllosilicate ad-
settled in favor of biodiesel because it can be produced from non-edible sorbent formed when volcanic activity is altered by the presence of an
feedstock (Aasma et al., 2021). Along with plants, animal fats and acid. Bentonite's high porosity can be attributed to its uneven dis-
leftover cooking oil have great potential as a cheap and efficient bio- tribution of particle sizes. Due to its high exchange capacity, large
diesel feedstock. Pre-treatment methods including alkaline trans ester- specific surface area, and relatively high net specific charge, bentonite
ification are used to lower the fatty acid concentration in these used clay is a popular material for a variety of applications. In order to
cooking oils with free fatty acids, preventing them from being con- achieve this, a micro catalytic site or channel was created using ben-
verted into soap. tonite as a supporting catalyst. A chemical solution (Sodium hydroxide)
The high-cost of biodiesel has been the focus of recent studies, with an was injected into the material to boost its performance (Noraini et al.,
emphasis on methods that aim to reduce the price of raw ingredients. Used 2021).
cooking oil is a cheap raw material that can be substituted for virgin oil to The response surface approach is a collection of mathematical and
produce biodiesel (Supple et al., 1999). Additionally, reusing waste cooking statistical techniques used to analyze data, create models, find optimal
oil could help with the waste oil discarding issue (Wiltsee, 1998). Waste conditions, and rank the importance of factors influencing a process
cooking oil (WCO) is a byproduct of repeated frying and is produced daily (Yucel, 2012). In the biodiesel industry, efficiency and cost-effective-
in a wide range of settings, including private homes, commercial kitchens, ness are paramount, so optimizing the production process is a top
and institutional food service operations. Water quality will be compro- priority for scientists (Wong et al., 2015).
mised if this trash is dumped in a body of water or another environmentally Several academics have studied response surface approach for fatty
sensitive region. Therefore, it must be treated and managed in a way that acid methyl ester(biodiesel) optimization (Mansourpoor and Shariati,
does not pose any risks to human health or the environment, such as by 2012).
being converted to biodiesel. The aim of the investigation presented in this research is synthesis of
Tadesse et al. (2019), studied biodiesel production from waste NaOH/bentonite catalyst, test its efficiency in producing biodiesel from
cooking oil and obtained a 96% conversion of WCO to biodiesel at used cooking oil, and identify the ideal conditions for production. The
optimized experimental conditions i.e., 50 °C, 1:8 WCO oil to methanol creation of a heterogeneous catalyst supported on bentonite for the
ratio, 1% by weight of catalyst loading rate and 90 min reaction time at synthesis of biodiesel is the unique contribution of this work. Despite
150 rpm agitation speed. Hoda et al. (2014), studied the optimization of being affordable and widely accessible, very little research has been
biodiesel from waste cooking oil a temperature of 65 °C, the catalyst done on the use of bentonite clay as a catalytic support in the synthesis
loading of 1.4 wt% and the MeOH/oil molar ratio of 7.5:1. The max- of biodiesel.
imum biodiesel yield under such conditions was 99.38 wt%, This catalyst, which consists of bentonite and sodium hydroxide, is
Fatty acid methyl ester can be created using different methods, in- stable and has been used by few researchers but not with catalyst se-
cluding transesterification/esterification, cracking, and pyrolysis lection as in this study. To get the most biodiesel out of the shortest
(Sánchez et al., 2019; Manish et al., 2021). Transesterification and es- amount of time, a heterogeneous catalyst supported by bentonite was
terification are the simplest and most popular methods for creating used. Utilizing used cooking oil from locally owned eateries, this study
biodiesel. It is possible to carry out these procedures by allowing a develops a high-quality biodiesel that satisfies ASTM criteria and can be
reaction to occur between any oil obtained from a feedstock and alcohol used as a non-petroleum diesel substitute to lessen emissions. Waste
in the presence of a suitable catalyst (Manish et al., 2021). An ester can cooking oil biodiesel has many benefits, including better recycling and
be trans esterified into another ester in the presence of an alcohol. The job creation, lower pollution, and a lower total cost of energy acquisi-
transesterification process, also known as alcoholysis, is the most tion. Using waste oil as a fuel source and in industrial applications like
popular method due to its many benefits over other production cosmetics helps small businesses achieve sustainability. The central
methods. These benefits include the ability to use a wider variety of composite design of the response surface methodology was also used to
feedstocks, better fuel characteristics achieved through reduced fuel optimize the biodiesel production in order to find the best candidate for
viscosity, the compatibility of biodiesel with any percentage of fossil biodiesel synthesis. As a result, the experimental research will be in
fuel, low production costs, and high conversion efficiency. When tri- accordance with institutional and international requirements.
glycerides and alcohol (methanol/ethanol) interact, esters and glycerol
are produced. As a result, biodiesel produced through transesterifica- 2. Materials and methods
tion or esterification is appropriately referred to as fatty acid mono-
alkyl ester derived from renewable feedstock that is either edible or 2.1. Materials
inedible. This process produces the high-value chemical glycerol as a
byproduct (Da Silva et al., 2015; Manish et al., 2021). The Sigma Aldrich Sodium hydroxide (NaOH) and methanol used in
The rate of transesterification can be modified by changing the re- this experiment were of analytical quality and were utilized in their
action temperature, the ratio of alcohol to oil, the relative humidity, the unrefined form. Bentonite clay, utilized throughout the study, was

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W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

acquired from a store in Wuse, Abuja; waste cooking oil and deionized Table 1
water were sourced in Onitsha, Anambra State and Zaria in Kaduna Experimental range and levels of the independent variables.
State, respectively. Factor Units Low level High level 0 level

2.2. Methods Methanol/oil Mol/mol 6(−1) 12(+1) 9

ratio. (A)
Catalyst conc.(B) wt% 3(−1) 5(+1) 4
2.2.1. Treatment of waste cooking oil Temperature (C) °C 45(−1) 75(+1) 60
The received oil sample was first filtered by sieve to remove any Reaction time (D) Hours 3(−1) 5(+1) 4
suspended food particles and inorganic residues, then heated to 110 °C Agitation speed Rpm 200(−1) 500(+1) 350
in a beaker at 15 min in an electric heater to evaporate the water. A (E)
beaker was used to hold the sample while it was heated at 110°C for
15 min in an electric boiler to evaporate/eliminate moisture. The pro-
concentration(B), reaction temperature (C), reaction time (D) and agi-
cess was allowed to settle for 4–6 days at ambient temperature. After
tation speed (D), were chosen as independent variables for this study as
the oil sample had cooled to room temperature, it was filtered using a
shown in Table 1. The Design of Expert software version 11.0.4.0 uti-
vacuum to eliminate any particles that might have been left behind
lizing central composite design (CCD) was used for the design of ex-
from the food preparation process or the filtration procedure. A glass
periments, plotting of response surfaces, and establishment of optimum
bottle was used to keep the pure sample from contamination (Tadesse
conditions. The study employed a 32-test, fractional factorial experi-
et al., 2019). Standard protocols set forth by the American Oil chemists
mental design with 16 factorial points, 10 axial points, and 6 central
Society (AOCS) were used to estimate the physicochemical properties;
points. According to their relative significance, their respective levels
acid value density, free fatty acid (FFA), kinematic viscosity, ash con-
were set.
tent, value, saponification value, and molecular weight of the sample,
A quadratic polynomial equation was created using a central com-
as shown in Table 3.
posite design to predict the response as a function of the independent
elements and their interactions (Razali et al., 2010). We used a math-
2.2.2. Preparation of catalyst
ematical model based on a second-order polynomial with interaction
The processes required to create a sodium hydroxide catalyst sup-
terms to predict the reaction. Response for quadratic polynomials is as
ported by bentonite are as follows: The sodium hydroxide concentra-
follows: (Montgomery, 2001).
tions in the bentonite clay combinations ranged from 1:1, 1:5, 1:10, and
1:15. The sodium hydroxide and bentonite solution was put into a Y= β0 + βiXi k i=1 + βiiX 2 i k i=1 + βij XiXj k j=i+1 k i=1 (2)
500 ml flask, which was then set on a heated plate with a magnetic
The number of factors studied and optimized in the experiment is
stirrer. Bentonite was impregnated with sodium hydroxide for 24 h at
denoted by k, and Y is the percent methyl ester yield; xi and xj are the
600 C and a constant 350 rpm stirring speed. Following the completion
independent study factors (coded variables); β0, βi, βii, and βij are the
of the impregnation procedure, the suspension was dried for 4 h at 1100
constant co-efficient, regression co-efficient of the linear terms, re-
C to remove any remaining moisture. The catalyst was then activated by
gression co-efficient of the quadratic terms, and regression co-efficient
being heated for 3 h in a furnace at 400°C. Biodiesel yields of 86.12%,
of the interaction terms, respectively (number of independent vari-
89.2%, 93.22%, and 80.42% were observed across four (4) different
ables).
bentonites to sodium hydroxide ratios in the experiments. The best
biodiesel yield, 93.22%, was attained with a bentonite to sodium hy-
3. Results and discussion
droxide (NaOH) ratio of 1:10, which was used for further experiment.
Scanning electron microscopy (SEM) and Fourier Transform-Infrared
3.1. Waste cooking oil characterization
(FTIR) analysis of the catalyst were performed to ascertain the mor-
phological structure and function groups of the catalyst, respectively.
As a result of various chemical activities such as material transfer
and hydrolysis between oil and food occur during the frying process,
2.2.3. Transesterification reaction
the chemical and physical features of the oil are altered. The physic-
The process was performed in a batch reactor. The reaction was
chemical variables of the waste cooking oil sample collected are listed
heated using a thermostatically controlled water bath heater. It was
in Table 2.
determined by adding a certain amount of catalyst (1–5 g) to a mea-
sured volume of methanol. The combination was then heated to the
3.2. Characterization of the catalyst
desired temperature (60 °C) in a water bath whose temperature could
be precisely regulated. At that point, used cooking oil was added while
3.2.1. Scanning electron microscope
the mixture was being mixed constantly (350 rpm). The reaction oc-
The SEM analysis was done to study the morphology of the raw and
curred between 1 and 5 h with molar ratio of methanol to oil 9:1. After
impregnated catalyst. Fig. 1(a) displays the SEM image of raw bento-
the reaction time had elapsed, the solution was centrifuged. Using
nite. The raw bentonite surface morphology has larger surface and
centrifugation, we were able to separate the glycerin and biodiesel
shows the coarse and porous structure which is important for the cat-
layers. The methanol and water were driven off by washing the bio-
alyst support material.
diesel phase with water, decanting it, and heating it to 100 °C. Layer
biodiesel output was measured as a percentage by comparing the
Table 2
amount of yield (biodiesel) produced to the volume of used waste
Physicochemical properties of waste cooking oil.
cooking oil was calculated.
Properties Waste cooking oil
Weight of FAME
Biodiesel yield = × 100
Weight of oil used (1) Moisture content wt% 0.065
Density (kg/m3) 928
Higher calorific value (MJ/kg) 36.2
2.2.4. Modeling and optimization by RSM Acid value (mgKOH/g) 0.86
To determine the optimal conditions for FAME synthesis and con- Kinematic viscosity (mm2/s) 32.5
FFA content (wt% of oil) 1.10
duct statistical analysis of variation (ANOVA) of the response model
Iodine value (cg/g) 105.56
with a two-level-five-factor -Methanol/oil molar ratio (A), Catalyst

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W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

Fig. 1. (a) SEM image of raw bentonite.

Fig. 1(b) shows SEM image of NaOH/Bentonite. The surface mor- respectively (Alberto et al., 2018).
phology of Fig. 1(b) appeared with a significant difference compared to The asymmetric and symmetric stretching vibration of the hydroxyl
Fig. 1(a). The impregnated bentonite catalyst shows the smooth surface in group present in bentonite clay lattice was observed at 3652.8 cm-1.
SEM image. This is due to the uniform distribution of sodium hydroxide The presence of water molecules was identified at 3652.8 cm-1 in both
catalyst on bentonite surface and also fills the bentonite pores. It appeared catalysts. The OH group attached to the interlayer of water molecules
to be formed by several flaky particles accumulated together in the form are observed at 2009.0 and 1114.5 cm-1, for raw and impregnated re-
of agglomerates. It also shows the existence of rod-like particles and has a spectively. In impregnated bentonite, a strong, wide band was observed
smoother surface than Fig. 1(a), which contains a few cavities and hair at 909.6 cm-1 due to symmetric bending. Accumulation of CH3ONa on
line breaks. This could be due to the activation process, which may have bentonite surface mainly affect the raw bentonite physical structure
filled in the holes and created a smooth surface. The SEM image of which is identified by presence of.
Fig. 1(b) indicated the disaggregation and decrease in the size of the Al-O-Na functional group. An addition of CH3ONa, changes the
bentonite structure after the base treatment (Ali et al., 2020). structure of Al (Mg)-O-H to Al-O-Na stretching group in the catalyst.
The changes in the functional groups provide the indication of the
3.2.2. Fourier transform infra-red analysis modifications that occurred during the impregnation process. The
Fourier transform infrared spectra (FTIR) of raw bentonite is shown major absorption bands/ FT-IR signals and their corresponding func-
in Fig. 2(a). The functional group of bentonite catalyst such as Al tional groups are summarized in Table 3.
(Mg)–O–H stretching vibration, H-O-H stretching, Al-OH- Mg, Si-O-Si
stretching, bounded Fe3 + and Si–O stretching, and Si-O stretching 3.3. Response surface method statistical analysis
were observed at 3693.8 cm-1, 3652.8, 2009.0 cm-1, 1640.0 cm-1,
1118.2 cm-1, 797.7 cm-1 and 678.4 cm-1, respectively. The outcomes of the CCD experimental design for employing RSM to
The FTIR spectra of the impregnated (NaOH/Bentonite) catalyst was transesterify waste cooking oil (WCO) to FAME are displayed in
carried out in the range from 1000 to 3500 cm-1 to study the catalytic Table 4. The actual yield was examined in order to develop a reliable
transesterification effect. The FTIR spectra observed in Fig. 2(b) is quite and useful regression model. A acceptable model was selected from a
characteristic for bentonites constituted mainly montmorillonite, re- range of possibilities, including mean, linear, quadratic, cubic, and
sponsible for the bending peak at 909 cm−1 (Al-Al-OH), 779 cm−1(Si- quartic models. By using a cubic regression model, the software was
O-Al) and 685 cm−1 (Si-O). The stretching of the –OH group of the able to foretell the optimal parameters for the transesterification of
trapped and adsorbed water can be observed at 3652 and 1114 cm−1, WCO to biodiesel. The best fit model for FAME yield is shown in Eq. (3).

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W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

Fig. 2. (a) Fourier transform infrared (FTIR) spectroscope of raw Bentonite (b). Fourier transform infrared (FTIR) spectroscope of modified bentonite (NaOH/
bentonite).

According to Table 4, the RSM regression model projected that the

A mathematical expression for Y is Y=87·70–5·07A-1·12B+2·23 C-
highest FAME yield of 91.2% would be produced with catalyst 4 wt%,
0·1467D-8·52E-3·77AB-5·74AC-6·40 CE+2·71AE+0·0862 BCE+4·01BD
reaction time 4 h, reaction temperature 600 C, methanol to oil molar
+1·66BE-2·73CD+0·8875CE+3·08DE-
ratio of 9:1, and agitation speed of 350 rpm. To evaluate the model
5·53A2–8·29B2–1·34C2–6·50D2–4·44E2 (3)
equation's statistical significance, the ANOVA test, R2, and Radj2 were
A, B, C, D, and E display the estimation of the trial/experimental applied.
variables. The word with a plus sign in front of it means that it increases The effectiveness and efficacy of the regression model in predicting
FAME yield synergistically, while the word with a minus sign means the response were performed using ANOVA, and the findings are shown
that it reduces FAME yield (Wisdom, 2021; Shuit et al., 2010). The in Table 5. At the 95% confidence level, the model's F-value and p-value
model regression's positive coefficients indicated a linear increase in were calculated to be 125.02 and 0.0001, respectively, indicating that it
FAME yield. On the other hand, the quadratic term had negative effects was statistically significant (p 0.05). In such case, the model terms A, C,
on the FAME yield. E, AB, AC, AD, AE, BD, CD, DE, A2, B2, D2, and E2 are statistically

Table 3
Major absorption peaks and their functional groups.

Wave number (cm-1) Functional group Vibration type Wave number (cm-1) Functional group Vibration type
Raw Bentonite NaOH/Bentonite

3693.8 Al (Mg)–O–H Stretching vibration 3893.8 -OH/Na Asymmetric stretching

3652.8 Al (Mg)-O-H Stretching vibration 3652.8 -C]O/Na-OH Stretching vibration
2009.0 H-O-H Symmetric bending 1114.5 -CH2 Symmetric bending
1640.0 Al-OH-Mg Symmetric bending 998.9 Al-OH-Na Symmetric bending
1118.2 Si-O-Si Symmetric bending 909.6 =C-O-C Symmetric stretching
797.7 Fe3 + and Si-O Symmetric bending 779.0 C-H Plane rocking vibration
678.4 Si-O Stretching vibration 685.8 Si-O-Na Stretching vibration

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W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

Table 4
Experimental results for the central composite design.

Run order Methanol to oil Catalyst weight Temperature (0C): C Time (h): Agitation speed Experimental yield Predicted yield
ratio: A (wt%): B D (rpm): E % %

1 9:1 6 60 4 350 50.90 52.29

2 15:1 4 60 4 350 54.03 55.43
3 12:1 5 45 5 200 57.89 57.19
4 9:1 4 30 4 350 76.47 77.86
5 12:1 5 75 3 200 60.51 59.81
6 12:1 3 75 3 500 62.12 61.42
7 12:1 3 75 5 200 48.72 48.02
8 12:1 3 45 5 500 52.59 51.89
9 9:1 4 60 4 650 51.50 52.89
10 6:1 5 45 3 200 62.49 61.79
11 9:1 4 60 4 350 86.00 87.70
12 6:1 3 75 5 500 63.19 62.49
13 12:1 5 75 5 500 43.46 42.76
14 12:1 5 45 3 500 47.46 46.76
15 9:1 4 60 4 500 85.56 86.96
16 9:1 4 60 4 350 89.00 87.70
17 9:1 2 60 4 350 55.36 56.75
18 9:1 4 60 6 350 60.03 61.42
19 6:1 3 45 3 500 34.98 34.29
20 9:1 4 60 2 350 60.62 62.01
21 3:1 4 60 4 350 74.32 75.71
22 9:1 4 60 4 350 89.00 87.70
23 6:1 5 75 3 500 58.77 58.08
24 9:1 4 60 4 350 89.00 87.70
25 6:1 5 45 5 500 67.57 66.88
26 6:1 3 45 5 200 72.49 71.79
27 9:1 4 90 4 350 85.39 86.78
28 6:1 5 75 5 200 91.20 90.50
29 9:1 4 60 4 350 87.00 87.70
30 6:1 3 75 3 200 88.15 87.45
31 12:1 3 45 3 200 84.97 84.27
32 9:1 4 60 4 350 89.00 87.70

significant, while B, D, BC, CE, and C2 are not. At the 99% confidence occur because to noise" will really happen. Significant lack of fit sug-
level, P-values less than 0.01 are considered statistically significant, gests that the model may be missing some contributions to the regressor
suggesting that the model is statistically significant (p-value 0.05). The response connection. Because considerable lack of fit suggests that the
lack of fit was not significant in comparison to the pure error, according model may be missing some contributions to the regressor response
to the lack of fit F-value of 2.69 and p-value of 0.1489 (p-value > 0.05 connection, insignificant lack of fit is most important. The model is
is not significant), and the model was well fitted to the experimental well-fitted as seen by the regression coefficient R2 of 0.9956, which
data. There is a 99.59% chance that a lack of fit F-value "this large may suggests that the experimental variables examined account for 99.56%

Table 5
ANOVA results: Test of significance.

Source Sum of Squares df Mean Square F-value p-value

Model 8479.06 20 423.95 125.02 < 0.0001

A-Methanol/oil ratio 617.12 1 617.12 181.99 < 0.0001
B-Catalyst conc. 29.88 1 29.88 8.81 0.0128
C-Temperature 119.35 1 119.35 35.20 < 0.0001
D-Time 0.5163 1 0.5163 0.1522 0.7038
E-Speed 1740.81 1 1740.81 513.36 < 0.0001
AB 227.26 1 227.26 67.02 < 0.0001
AC 527.62 1 527.62 155.60 < 0.0001
AD 656.13 1 656.13 193.49 < 0.0001
AE 117.51 1 117.51 34.65 0.0001
BC 0.1190 1 0.1190 0.0351 0.8548
BD 256.96 1 256.96 75.78 < 0.0001
BE 44.29 1 44.29 13.06 0.0041
CD 118.92 1 118.92 35.07 < 0.0001
CE 12.60 1 12.60 3.72 0.0801
DE 151.91 1 151.91 44.80 < 0.0001
A² 898.18 1 898.18 264.87 < 0.0001
B² 2018.23 1 2018.23 595.18 < 0.0001
C² 53.05 1 53.05 15.64 0.0023
D² 1237.82 1 1237.82 365.03 < 0.0001
E² 579.51 1 579.51 170.90 < 0.0001
Residual 37.30 11 3.39
Lack of Fit 28.47 6 4.74 2.69 0.1489
Pure Error 8.83 5 1.77
Cor Total 8516.36 31

6
W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

Table 6
Model summary statistics.

Source Std. Dev. R² Adjusted R² Predicted R² PRESS C.V.% Mean

Linear 15.20 0.2945 0.1588 -0.0124 8621.58

2FI 15.60 0.5426 0.1138 -2.9572 33,700.82
Quadratic 1.84 0.9956 0.9877 0.9221 663.15 2.70 68.12 Suggested
Cubic 2.49 0.9956 0.9774 -2.6296 30,910.88 Aliased

Table 7 attributes of the obtained biodiesel are shown in Table 7, along with
Properties of Produced Biodiesel (FAME) from WCO. comparisons to ASTM and EN standards. It can be shown that WCO's
density quickly drops after being turned into biodiesel, going from
Properties WCO ASTM D – EN14214
Biodiesel 6751 928 kg/m3 to 891 kg/m3. That the triglycerides are successfully
transformed into methyl esters can be inferred from this finding. The
Flash point (ºC) 166 > 130 – biodiesel produced in this condition was further analyzed to determine
Kinematic viscosity at 4.12 1.9 – 6.0 3.5 – 5.0
its viscosity and pour point in accordance with ASTM standards. As
30ºC (mm2 /s)
Pour point (ºC) -9 - 15–10 – required by ASTM D6751 and EN 14,214, the acid value, viscosity,
Acid value (mg KOH/g) 0.38 < 0.8 – density, pour point, and flash point all satisfied these requirements. The
Density at 32ºC (Kg/m3) 891 875 – 900 860 – 900 outcome of this investigation shows that the biodiesel produced will not
have an impact on the engine's ability to inject fuel efficiently
throughout the combustion process supported that it passes to the
of the total variation in biodiesel yield. According to Table 6, which
density required for biodiesel stipulated in ASTM and EN standards.
shows high values of projected R2 (0.9221) and adjusted coefficient of
determination (Radj2:0.9887), a standard deviation of 1.84, and a low
coefficient of variation (C.V:2.70%), the results of the quadratic model 3.5. Effects of process parameter on biodiesel yield
provided a strong indication of accuracy and dependability for the re-
lationship between the independent parameters and the corresponding 3.5.1. Effect of methanol/oil molar ratio on biodiesel yield
response. Methanol to oil ratio has a significant influence on biodiesel yield, as
shown in Fig. 3(a). The reported yield was 76.4% at molar ratio of
3.4. Physical property of produced Biodiesel methanol to oil of 9:1. Excess methanol is essential since it boosts the
speed of methanolysis. Since production of methoxyl species on the
The key characteristics of the biodiesel were used to describe the catalyst surface was stimulated by increase in methanol concentration,
biodiesel product. Acidity, flash point, and density are included. The an equilibrium shift toward the forward direction occurred, leading to

(c)

(d)

Fig. 3. (a). Effect of methanol/oil molar ratio on biodiesel yield (b). Effect of catalyst concentration on biodiesel yield (e). Effect of agitation speed on biodiesel yield.

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W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

Fig. 4. Predicted versus experimental yield (%).

an increase in biodiesel yield (Buasr et al., 2013). After methanol-to-oil 3.5.3. Effect of temperature on biodiesel yield
molar ratio of 9:1, further increases would reduce biodiesel production. Fig. 3(c) shows the biodiesel output from waste cooking oil trans-
This could be attributed to the reaction being stymied by a concentra- esterification at reaction temperatures ranging from 45° to 75°C. The
tion of methanol that is too high compared to what would be ideal. biodiesel yield rises with the reaction temperature until it reaches an
Glycerol, a byproduct of the reaction, would dissolve primarily in the ideal point of 60 °C, with an 89.0% biodiesel yield. The transester-
excess methanol, preventing the methanol from reacting with the re- ification required some thermal energy at first because the reaction was
actants and the catalyst. This would prevent the separation of glycerin endothermic. Because the reaction mixture is a three-phase system (oil,
and reduce the conversion by shifting the equilibrium in the opposite methanol, and catalyst), enough thermal energy was required to over-
direction. come the diffusion barrier between the phases (Liu et al., 2008).
However, the high temperatures are not preferable. When the tem-
3.5.2. Effect of catalyst concentration on biodiesel yield perature rises to the boiling point of methanol, the methanol quickly
Increasing the yield of the transesterification reaction, the catalyst vaporizes and forms a significant number of bubbles, inhibiting the
concentration is necessary. Fig. 3(b) demonstrates that the biodiesel yield process at the two-phase interface and reducing the biodiesel yield.
increases when catalyst concentration increases from 1 to 5, but the yield
somewhat drops as catalyst concentration goes further. The optimal cat- 3.5.4. Effect of time on biodiesel yield
alyst concentration was found to be 4 wt%, which resulted in a biodiesel Waste cooking oil transesterification yielding biodiesel throughout a
output of 86.0%. The biodiesel output has somewhat decreased as a result range of reaction periods (from 0.5 to 5 h) is depicted in Fig. 3(d). When
of soap production when there is a lot of catalyst present. Furthermore, the transesterification reaction first started, biodiesel production was
too much catalyst increases the viscosity of the reactants, lowering the quick until it reached equilibrium. Once the reaction has exceeded the
synthesis of biodiesel. Transesterification is catalyzed by the basic sites optimal point, it starts to turn against the reactants. This outcome was
created on the catalyst's surface as well as the soluble material that is brought about by the transesterification reaction's reversibility
leached from the catalyst (Granados et al., 2007). (Santana et al., 2012). Because the catalyst may soak up so much of the

Fig. 5. (a). 3D response surface plot for the interaction effect of methanol to oil molar ratio and catalyst concentration against yield (%). (b). Contour plot
representing the Effect of methanol to oil ratio and catalyst concentration against yield (%).

8
W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

Fig. 6. (a). 3D response surface plot for the interaction effect of methanol to oil molar ratio and temperature(°C) against yield (%) (b). Contour plot representing the
Effect of methanol to oil ratio and catalyst concentration against yield (%).

end product, the reaction period is too long to produce much biodiesel. runs designed by the CCD model served as the experimental values,
That's why it's so important to zero in on the optimum transesterifica- while the predicted values were calculated using the quadratic model
tion reaction time. In this case, a response time of 4 h resulted in a yield that had been established. Fig. 4 shows that the data points on the plot
of 89.0%. were adequately dispersed near the straight line (R2 = 0.9956), im-
plying a reasonable link (a good conformity) between the experimental
3.5.5. Effect of agitation speed on biodiesel yield and projected response values and that the analyses' underlying as-
The agitation rate is a significant reaction variable that affects sumptions were correct (data fit the model well).
biodiesel synthesis during the transesterification of triglycerides. As Fig. 5(a) and (b), showed the 3D response surface and the contour
shown in Fig. 3(e), the biodiesel yield increased with increasing agi- plots. Each curving contour represents an unlimited number of possible
tation speed, reaching a peak of 91.0% at 350 rpm. But beyond that combinations of two test variables, with the other two remaining at
optimum agitation speed, there was no appreciable gain in biodiesel zero. It is simple and convenient to comprehend the interactions be-
yield. This research found that the optimal agitation speed for max- tween two components and to determine their optimum levels using
imum biodiesel production was 350 rpm. This showed that agitation at contour plots. Fig. 5(a) demonstrate the response to the interaction
350 rpm was adequate to restrict the mass transfer of the process. between methanol oil ratio and catalyst weight versus yield. These
graphs show that better biodiesel yields occur when the methanol oil/
ratio is 9:1, the catalyst weight is 4%, the reaction temperature is 60 °C,
3.5.6. Three-dimensional response surface and the contour plots
and the reaction period at 4 h. The oil to methanol molar ratio had only
Fig. 4 shows the results of a correlation analysis of the experimental
a little effect on synthesis at low catalyst concentrations, however at
and anticipated FAME yields (%). The measured response data for the

Fig. 7. (a). 3D response surface plot for the interaction effect of methanol to oil molar ratio and time(hr) against yield (%) (b). Contour plot representing the Effect of
methanol to oil ratio and time (hr) against yield (%).

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W.C. Ulakpa, R.O.E. Ulakpa, E.O. Eyankware et al. Cleaner Waste Systems 3 (2022) 100049

high catalyst concentrations, the oil to methanol molar ratio was sig- the transformation of waste cooking oil (WCO) into biodiesel may
nificantly important for synthesis enhancement (Jeong et al., 2009). further be examined. For cost-effective biodiesel synthesis, choosing the
However, if the catalyst concentration is higher than the prescribed correct feedstock oil is essential. Food crops should not be affected by
levels, the product will not separate. In other words, the transester- the feedstock oil chosen. Finally, in order to decrease mass transfer
ification reaction would be difficult to complete. As a result, the resistance, significant energy use, and by-product utilization, techno-
transesterification reaction was hampered by low catalyst concentra- logical improvement is required in order to construct the reaction
tions and a higher methanol-to-oil ratio. When the catalyst was in- process on a big scale. As a result, there should be more investigation
creased to a specific level and the methanol to oil ratio was high, the into how to enhance catalyst support and opportunities for maintaining
yield merely improved. The contour plot Fig. 5(b) revealed that a high ideal reaction variables, which will increase biodiesel production.
biodiesel production (> 91.2%) may be achieved by using a combina-
tion of intermediate to high catalyst loading (3–5 wt%) and a high CRediT authorship contribution statement
methanol to oil molar ratio (6−12).
The impact of methanol to oil ratio and temperature on biodiesel Wisdom Chukwuemeke Ulakpa conceptualized the research idea.
yield is depicted in Fig. 6(a) and 6(b). Plot analysis revealed that 60°C All the authors make substantial contribution in this manuscript.
and a 9:1 methanol-to-oil ratio resulted in the highest yield (91%). As Analysis of experimental data was carried out with contribution and
the temperature rises, methanol becomes more soluble in the oil. When guidance from all the authors. Wisdom Chukwuemeke Ulakpa is the
the methanol to oil molar ratio was raised at low temperatures, bio- first author of the manuscript while other authors undertook the re-
diesel production first increased and then decreased. This might be view, correction, and commented on the manuscript. All authors have
because methanol evaporates, inhibiting the reaction at the three-phase read and approved the final manuscript.
contact (Boulifi et al., 2010; Sliva et al., 2010).
The influence of methanol quantity and reaction time on experi- Data Availability
mental yield is depicted in a 3D surface plot and a contour plot, re-
spectively, as shown in Fig. 7(a) and (b). The figures show that for the Data will be made available on request.
given methanol quantity (9:1), the yield increased with increased re-
action time. This is because when reaction time was less and less me- Declaration of Competing Interest
thanol was reacting, the biodiesel yield was very low since there was
incomplete reaction. This may be as a result of adequate time provided The authors declare that they have no known competing financial
for conversion of the triglyceride. Because the quadratic components of interests or personal relationships that could have appeared to influ-
the two parameters are more substantial and have a negative impact ence the work reported in this paper.
with increasing methanol and reaction times, the yield decreased (Sliva
et al., 2010; Math and Harshavardhan, 2016). Acknowledgements

4. Conclusions The authors are grateful to the reviewers for their constructive
comments/remarks and suggestions towards improving the quality of
The outcomes of the studies suggest that factors including reaction the manuscript. We also acknowledge the department of Chemical
time, the molar ratio of methanol to oil, and speed significantly influ- Engineering, Faculty of Engineering, Ahmedu Bello University and
enced the transesterification of WCO to methyl ester. The impacts of the National Research Institute of Chemical Technology (NARICT)for its
key operating factors on the development of biodiesel from used assistance in carrying out the analysis.
cooking oil were effectively studied using the response surface metho-
dology based on the central composite design (CCD). The methanol to References
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