Fuel Processing Technology 111 (2013) 105–110

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Fuel Processing Technology

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Optimization of biodiesel production from castor oil using factorial design

Murat Kılıç a, Başak Burcu Uzun a, Ersan Pütün b,⁎, Ayşe Eren Pütün a
a
Anadolu University, Department of Chemical Engineering, 26555 Eskisehir, Turkey
b
Anadolu University, Department of Materials Science and Engineering, 26555 Eskisehir, Turkey

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

Article history: In this study, optimization of biodiesel production from castor oil using full factorial design was investigated.
Received 27 December 2011 The biodiesel production was carried out in a batch laboratory scale reactor by alkaline-catalyzed
Received in revised form 25 April 2012 transesterification process. Experimental design was used in the evaluation of process variables. Effects of
Accepted 2 May 2012
temperature, methanol/oil molar ratio and catalyst concentration were optimized according to the 2 3 full fac-
Available online 15 March 2013
torial central composite design (CCD). For determining the influence of purification methods on biodiesel
Keywords:
yield, different purification methods were applied to the product after transesterification reaction. Second-
Castor oil order model was obtained to predict biodiesel yield as a function of these variables. According to the exper-
Transesterification imental results this process gave an average yield of biodiesel more than 90%.
Biodiesel © 2013 Elsevier B.V. All rights reserved.
Optimization
Experimental design

1. Introduction followed by the conversion of diglycerides to monoglycerides and of

New and renewable alternative fuels as a substitute for petroleum-
based fuels have become increasingly important, due to environmental
concerns, unstable costs and transportation problems [1,2]. For this rea-
son the possibility of developing alternative energy sources to replace
traditional fossil fuels has been receiving a large interest in the last
few decades. Biodiesel is a source of renewable energy that is made
from biological sources such as vegetable oils and animal fats and is
an attractive alternative to petro-diesel fuel because of its environmen-
tal benefits. It is biodegradable, non-toxic with a low emission profile
and can be used directly or mixed with conventional fuel for diesel en-
gines, and as a heating fuel [3,4].
The most common way to produce biodiesel is transesterification.
In this reaction, triglycerides, as the main components of vegetable
oils, react with an alcohol to produce fatty acid mono-alkyl esters
and glycerol as a by-product. Methanol is the most commonly used
alcohol because of its low price compared to other alcohols. In this
case, the reaction is referred to as methanolysis. Generally, this reac-
tion is catalyzed by a basic or an acid catalyst. The alkali catalysts are
the most commonly used, because they make the process faster and
the reaction conditions are more moderated. The stoichiometry of
methanolysis reaction requires 3 mol of methanol and 1 mol of tri-
glyceride to give 3 mol of fatty acid methyl ester (FAME) and 1 mol
of glycerol. This is the general transesterification reaction, because it
consists of a number of consecutive reversible reactions. The first
step is the conversion of triglycerides to diglycerides, which is
⁎ Corresponding author. Tel.: +90 2223213550x6352.
E-mail address: eputun@anadolu.edu.tr (E. Pütün).
monoglycerides to glycerol, yielding one methyl ester molecule
from each glyceride at each step [5,6].
There are many parameters affecting the transesterification reac-
tion. The ones known as greatly influencing the reaction are: tempera-
ture, methanol/oil molar ratio, catalyst type and amount of catalyst.
The optimization of the production process should take into account
such parameters. Considering homogeneous alkali catalytic systems:
(i) optimum temperature tends to be the one which is the closest to
the boiling point of the alcohol used; (ii) excess alcohol is necessary to
promote a good conversion (6:1 is considered as the best methanol/
oil molar ratio by many authors); (iii) catalysts normally used are sodi-
um and potassium hydroxides, sodium and potassium methoxides as
well as sodium and potassium carbonates; (iv) amount of catalyst
used might vary from 0.2 to 2 (wt.%) [7].
Like other vegetable oils, castor oil is constituted mainly by tri-
glycerides which consist of three fatty acids and one molecule of glyc-
erol. The fatty acids of this oil consist of approximately 80–90%
ricinoleic, 3–6% linoleic, 2–4% oleic, and 1–5% saturated fatty acids.
Castor oil is a viscous, pale yellow nonvolatile and non-dry oil. Due
to this particular chemical composition castor oil is a raw material
in great demand by the pharmaceutical and chemical industry. Its
use as fuel for internal combustion engines, however, can become
complicated because of its extremely high viscosity and high water
content. Thus a better method to use castor oil in engines as fuel is
its transesterification.
Most of the studies on the transesterification for optimization of re-
action parameters were based on changing one separate factor at a time
(COST). However, reaction system was influenced simultaneously by
more than one factor, due to this fact it is important to investigate the

0378-3820/$ – see front matter © 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.fuproc.2012.05.032
106 M. Kılıç et al. / Fuel Processing Technology 111 (2013) 105–110

effects of interactions between reaction parameters. Although some Table 2

studies can be found about the optimization of biodiesel production The physical and chemical properties of castor oil.

from castor oil in literature, they are generally based on different exper- Property Value ASTM limits Test method
imental design methodologies and ethanolysis [8–11]. For instance,
Density (15 °C) 965 kg/m3 957–968 kg/m3 AOCS Cc 10a-25
Cavalcante et al. [8] studied transesterification of castor oil with ethanol Refractive index (20 °C) 1.478 1.467–1.490 AOCS Cc 7-25
using a central composite rotatable design. They determined the opti- Acid index 0.64 mg KOH/g 0.4–4.0 AOCS Cd 3a-63
mum reaction conditions as oil:ethanol molar ratio of 1:11, catalyst Iodine index 86 g I−/100 g 82–88 g I−/100 g AOCS Cd 1-25
Saponification index 182 mg KOH/g 175–187 mg KOH/g AOCS Cd 3-25
amount of 1.75% KOH, and reaction time of 90 min and obtained
Unsaponifiable 0.11 0.3–0.7 AOCS Ca 6a-40
≈86.0% of biodiesel yield. Ramezani et al. [9] used Taguchi method matter (%)
for optimization of castor oil transesterification. Optimum reaction con- Viscosity (25 °C) 6.6 St 6.3–8.8 St AOCS Tq 1a-64
ditions were determined as methanol:oil molar ratio of 8:1, catalyst HHV 40.83 MJ/kg –
amount of 0.5% CH3OK, reaction time of 120 min, reaction temperature Molecular weight 926 kg/mol –
Fatty acid composition – AOCS Ce 1-62
of 65 °C and mixing intensity of 400 rpm. According to the optimum
Ricinoleic acid 89.08 wt.%
reaction conditions they obtained the biodiesel yield as ≈87.0% by Palmitic acid (C16:0) 0.42 wt.%
using the Taguchi method. Silva et al. [10] studied alkali ethanolysis of Stearic acid (C18:0) 0.33 wt.%
castor oil and optimized the process parameters by using factorial Oleic acid (C18:1) 2.83 wt.%
Linoleic acid (C18:2) 4.03 wt.%
design adding central points and axial points as star points. They used
Linolenic acid (C18:3) 2.10 wt.%
bioethanol obtained from sugar cane as alcohol for transesterification Lignoceric acid (C24:0) 1.21 wt.%
reaction. 99.0% of ethyl ester and 93.0% of biodiesel yield were
obtained by using optimum reaction conditions which were deter-
mined as ethanol:castor oil molar ratio of 16:1, catalyst amount of were determined according to the ASTM D 6751, EN 14214 and
1.0% C2H5ONa, reaction time of 30 min, and reaction temperature AOCS standard test methods.
of 30 °C with mechanic stirrer. Jeong and Park [11] optimized the
biodiesel production from castor oil using response surface method-
ology. They determined the optimum process parameters as the re- 2.3. Experimental procedure
action time of 40 min, reaction temperature of 35.5 °C, oil:methanol
molar ratio of 1:8.24, and catalyst concentration of 1.45% KOH. 92.0% The system used for transesterification reactions consisted of tem-
biodiesel yield was obtained by using the determined conditions. perature bath, reaction flask with reflux condenser and rpm con-
With the above considerations, in this study biodiesel production trolled mechanical stirrer. Experiments were carried out in a
from castor oil has been optimized by application of the full-factorial 500 cm 3 two necked batch reactor, one for condenser and the other
design. 2 3 full factorial central composite design (CCD) was used to op- for samples. The temperature bath was capable of maintaining the re-
timize the reaction parameters and determine the relationship between action temperature to within ±0.01 °C. A thermometer was used to
reaction parameters. Different alkali catalysts were used to determine measure the reaction temperature. Castor oil was preheated until
the optimum alkali catalyst and different purification methods were ap- the desired temperature was reached. Then, a mixture of methanol
plied to the product to determine the optimum purification type. Effects and catalyst was added to the oil and the transesterification reaction
of the other process parameters such as reaction temperature, metha- began. The stirrer was set at 600 rpm to avoid the mass transfer lim-
nol/oil molar ratio and catalyst concentration on biodiesel yield were itations and a magnetic bar was used for stirring [13]. The reaction
optimized by using experimental design. was timed as soon as the methanol/catalyst mixture was added and
continued for 10 min. After the reaction, product was kept overnight
for cooling down and separation of the phases. The upper phase
2. Materials and methods
consisted of methyl esters, and the lower phase consisted of glycerol,
remaining catalyst, excess methanol, formed soaps and some
2.1. Materials
entrained methyl esters. Fewer amounts of catalyst, glycerol and
methanol were in the upper methyl ester phase. After removing the
Castor oil was obtained from a local market. Methanol, potassium
glycerol from the methyl ester phase with separation funnel, the
hydroxide, sodium hydroxide, potassium methoxide and sodium
upper methyl ester phase was purified and then dried over sodium
methoxide were purchased from Merck Chemicals. Reference standards
sulfate and filtered under vacuum.
for gas chromatography (GC) were obtained from Sigma-Aldrich. All
To find out the suitable alkali catalyst for the castor oil
chemicals used in experiments were analytical reagent grade and
transesterification a comparison is made of various alkali catalysts
used without further purification.

2.2. Analytical methods

100
Properties of castor oil were determined according to the AOCS
standard test methods of oil and fat analyses [12]. Fatty acid compo- 90
Biodiesel Yield (%)

sition of the oil was determined using Hewlett–Packard 7890 Series

II Gas Chromatography. Fuel properties of the final biodiesel product 80

70
Table 1
Experimental range and levels of the independent variables.
60
Variables Symbol coded Range and levels

−1 0 +1 50
KOH NaOH CH3ONa CH3OK
Temperature (°C) X1 25 45 65 Catalyst type
Catalyst concentration (wt.%) X2 0.5 1.0 1.5
Methanol/oil molar ratio X3 5:1 6:1 7:1
Fig. 1. Effect of catalyst type on biodiesel yield.
 M. Kılıç et al. / Fuel Processing Technology 111 (2013) 105–110 107

Table 4
100 ANOVA for the model.

Sources of Degree of Sum of Mean F-value P-value

90
Biodiesel Yield (%)

variations freedom squares square

80 Model 7 129.10 18.44 55.30 0.001

Linear 3 117.90 39.30 117.83 0.000
Square 1 7.57 7.57 22.71 0.009
70 Interaction 3 3.70 1.21 3.64 0.122
Residual error 4 1.33 0.33
60 Lack-of-fit 1 0.87 0.87 5.65 0.098
Pure error 3 0.46 0.15
Total 11 130.41
50
silica gel phosphoric acid water S = 0.5774, R2 = 0.990, Adj. R2 = 0.972.

Fig. 2. Effect of purification type on biodiesel yield.

errors. In this way, the arithmetical averages were calculated for all
such as NaOH, KOH, CH3ONa, and CH3OK. Because, dissolving NaOH the results.
(or KOH) in the anhydrous methanol produces water according to
the following equilibrium equation [14]: 2.4. Statistical analysis

CH3 OH þ NaOHðorKOHÞ→CH3 ONaðorCH3 OKÞ þ H2 O:
Formed water reacts with oils in the reaction system and lead to
form soaps. This saponification reaction reduces the final biodiesel
yield. Using CH3ONa and CH3OK cannot form any water as side
product, because these catalysts can only dissociate CH3O − and Na +
(or K +) leading to obtain a higher biodiesel yield [14].
Predojevic [15] reported the importance of purification type on
biodiesel yield and fuel characteristics. The refining step of the prod-
ucts obtained by the transesterification is very important because the
purity level of the biodiesel has strong influence on its fuel properties.
The amount of glycerides and triglycerides present in the fuel can
cause serious problems in application. Another factor that must be
taken into account is that the fuel must be almost free of water, alco-
hol, glycerin and catalyst; thus, the ester layer has to be treated.
According to the European Union standards for alternative diesel
fuel, the contents of free fatty acids, methanol, glycerin, and water
in the biodiesel are restricted and biodiesel must be at least 96.5%
pure [15]. Therefore, three different methods were applied for the pu-
rification of the product mixture: washing the mixture with (a) silica
gel, (b) 5% phosphoric acid, and (c) hot distilled water.
Product yield is defined as the weight percentage of the final prod-
uct (transesterified and purified oil) relative to the weight of oil at the
start. Product yield equation is expressed as follows:
The statistical design chosen for the development and optimiza-
tion of biodiesel production from castor oil was 2 3 full factorial cen-
tral composite design (CCD). Application of this methodology
requires the appropriate selection of responses, factors and levels.
Biodiesel yield was selected as response. Range and levels of the
investigated variables are listed in Table 1. Factors were temperature
(X1), catalyst concentration (X2) and methanol/oil molar ratio (X3).
The upper temperature level, 65 °C, was chosen for being the boiling
point of methanol. The lower level was, 25 °C, as being the room tem-
perature, since lower temperatures would require a cooling system,
which would increase the cost of the process [4]. Catalyst concentra-
tion levels were 0.5 and 1.5% by weight of oil. Methanol/oil molar
ratio levels were 5:1 and 7:1. Central values (zero level) for the
experiments were: 45 °C for reaction temperature, 1.0% for catalyst
concentration and 6:1 for methanol/oil molar ratio.
Once the experiments are performed, the response variable (bio-
diesel yield) was fitted a second-order model in order to correlate
the response variable to the independent variable. The general form
of the second degree polynomial equation is as follows:
k k k k
2
Y ¼ b0 þ ∑ bi X i þ ∑ bij X i þ ∑ : ∑ bij X i X j þ e ð2Þ
i¼1 i¼1 ii>j j

Weight of biodiesel
ProductYieldð% Þ ¼ : ð1Þ where i and j are the linear and quadratic coefficients, respectively, b
Weight of raw oil
is the regression coefficient, k is the number of factors studied and op-
timized in the experiment and e is the random error [16].
All the experiments were carried out at least three times in order to
determine the variability of the results and to assess the experimental 3. Results and discussion

3.1. Properties of castor oil

Table 3
Experiment matrix of three variables and experiment results.
Physical and chemical properties of castor oil were analyzed and
Point Run X1 X2 X3 T (°C) Catalyst Methanol/ Biodiesel
given in Table 2. The oil is mainly ricinoleic acid and the properties
type number concentration oil molar yield (%)
(wt.%) ratio

Fact 1 −1 −1 −1 25 0.5 5:1 88.10 Table 5

2 +1 −1 −1 65 0.5 5:1 91.60 The least-squares fit and parameter estimates.
3 −1 +1 −1 25 1.5 5:1 91.85
Model term Coefficients estimated Standard error t-value P-value
4 +1 +1 −1 65 1.5 5:1 95.68
5 −1 −1 +1 25 0.5 7:1 95.46 Intercept 93.33 0.30 323.24 0.000
6 +1 −1 +1 65 0.5 7:1 99.10 X1 1.61 0.21 7.90 0.001
7 −1 +1 +1 25 1.5 7:1 98.18 X2 1.37 0.21 6.71 0.003
8 +1 +1 +1 65 1.5 7:1 99.81 X3 3.20 0.21 15.70 0.000
Center 9 0 0 0 45 1.0 6:1 92.80 X12 1.70 0.35 4.77 0.009
10 0 0 0 45 1.0 6:1 93.75 X12 −0.25 0.21 −1.21 0.292
11 0 0 0 45 1.0 6:1 93.35 X13 −0.22 0.21 −1.08 0.342
12 0 0 0 45 1.0 6:1 93.40 X23 −0.60 0.21 −2.90 0.045
108 M. Kılıç et al. / Fuel Processing Technology 111 (2013) 105–110

Fig. 3. Response surface plot and contour plot of biodiesel yield as a function of temperature and catalyst concentration. Methanol/oil molar ratio of 6:1.

of oil are in the range of limits. Therefore it can be used for biodiesel transesterification of castor oil. Therefore, all the experiments were
production. purified with using silica gel.

3.3. Statistical analysis

3.2. Effect of catalyst and purification type
According to the experimental design program MINITAB 16, cen-
tral values were 45 °C for reaction temperature, 1 wt.% for catalyst
concentration, and 6:1 for methanol:oil ratio. In this part of the
study, these values were kept constant in order to determine the ap-
propriate catalyst and purification type, before starting the experi-
mental design. Fig. 1 shows the effect of catalyst types on castor oil
biodiesel yield. It is shown that CH3ONa and CH3OK catalysts gave a
higher biodiesel yield than NaOH and KOH catalysts. After the
transesterification reaction it is seen that both upper and lower
phase contents formed soaps while using NaOH and KOH catalysts.
This soap formation decreased when CH3ONa and CH3OK catalysts
were used. During purification of the upper phase these sodium
soaps formed foams and reduced the biodiesel yield. There was no
foam formation during washing the upper methyl ester phase when
using CH3ONa and CH3OK catalysts. The maximum biodiesel yield
was obtained by using CH3OK catalyst. Therefore, CH3OK catalyst
was used as optimum catalyst in experimental design studies. Fig. 2
shows the purification results of produced biodiesel using center
point reaction conditions. Purification results showed that silica gel
is more suitable for the purification of biodiesel obtained from the
The experimental matrix for the factorial design and results are
shown in Table 3. The first three columns of data give ± 1 coded fac-
tor levels in the dimensionless co-ordinate, and the next three give
the factor levels on a natural scale. Four experiments were carried
out at the center point level for experimental error estimation.
A statistical analysis was carried out with these experimental
values and the main effects of the variables were calculated. Table 4
shows the analysis of the main effects and interactions in the form
of analysis of variance (ANOVA) for the chosen response together
with the test of statistical significance, a two-sided test with a 95%
confidence level. The P-values are used as a tool to check the signifi-
cance of the corresponding coefficient. The smaller the P-values are,
the bigger the significance of the corresponding coefficient. As it can
be seen, the P-value of the model, found by ANOVA, was 0.001
which indicates that the model is very suitable. The “Lack-of-Fit”
was insignificant, due to high P-value (0.098) and lower F-value
(5.65). In addition, the coefficient determination (R 2) and adjust coef-
ficient of determination (Adj. R 2) indicated that, the accuracy and
general availability of the polynomial model were adequate.
The significance of each coefficient was determined by t-values and
P-values which are listed in Table 5. The larger the magnitude of the

Fig. 4. Response surface plot and contour plot of biodiesel yield as a function of temperature and methanol/oil molar ratio. Catalyst concentration of 1.0%.
 M. Kılıç et al. / Fuel Processing Technology 111 (2013) 105–110 109

Fig. 5. Response surface plot and contour plot of biodiesel yield as a function of catalyst concentration and methanol/oil molar ratio. Temperature of 45 °C.

t-value and smaller the P-value, the more significant is the corresponding
coefficient [17]. This implies that the variable with the largest effect was
the term of methanol/oil molar ratio. Also it is shown that the t-values
and P-values of interactions indicate that interactive effects are not sig-
nificant on biodiesel, however they have a small negative effect on bio-
diesel yield. The linear effects of temperature, catalyst concentration
and methanol/oil molar ratio are more significant than the squared
term of temperature and they have a positive effect on biodiesel yield.
Experimental results were fitted to a linear model, and the following
second-order polynomial equation was obtained as:
3.4. Fuel properties of produced biodiesel
For commercial fuel, the finished biodiesel must be analyzed using
analytical equipment to ensure that it meets the international stan-
dards. Analytical methods were applied on the final biodiesel product
to determine the fuel characteristics and the results were compared
with the diesel standards of EN 14214 and ASTM D 6751. As seen
from Table 6 the properties of produced biodiesel are in accordance
with the ASTM D 6751 and EN 14214 standards.
4. Conclusions

Y ¼ 93:33 þ 1:61X 1 þ 1:37X 2 þ 3:20X 3 2 3 full factorial central composite design (CCD) was used to opti-
2
þ 1:70X 1 –0:25X 12 –0:22X 13 –0:60X 23 : ð3Þ mize the biodiesel production from castor oil. This design procedure
has been followed to optimize the variables to determine a maximum
biodiesel yield and a second-order response equation obtained for the
The three-dimensional response surface and two-dimensional con- biodiesel yield as a function of three variables. CH3OK catalyst was
tour plots are general for the graphical representations of the regression found the optimum catalyst for castor oil transesterification and silica
equation. Fig. 3 shows the response surface and contour plots for the gel is determined more suitable for purifying the obtained product.
predicted values of the biodiesel yield as a function of temperature Experimental design studies showed that linear effects of temper-
and catalyst concentration at a 6:1 methanol/oil molar ratio. Fig. 4 ature, catalyst concentration and methanol/oil molar ratio are more
shows the response surface plot and contour plot of biodiesel yield as significant than the squared term of temperature and they have a
a function of temperature and methanol/oil molar ratio at a catalyst positive effect on biodiesel yield. Temperature and methanol/oil
concentration of 1.0%. Fig. 5 shows the response surface plot and con- molar ratio were more effective on biodiesel yield than catalyst con-
tour plot of biodiesel yield as a function of catalyst concentration and centration. Interactive effects were not significant on biodiesel, how-
methanol/oil molar ratio at a temperature of 45 °C. By analyzing these ever they have a small negative effect on biodiesel yield. With a short
three figures, it can be concluded that increasing the reaction parame- reaction time (10 min), the maximum biodiesel yield was obtained as
ters result in an increased biodiesel yield. 99.81% at the temperature of 65 °C, catalyst concentration of 1.5% and
methanol/oil molar ratio of 7:1.
It is proved that a three-factorial design was an effective study for de-
termining the influence of the temperature, catalyst concentration and
Table 6
Some fuel properties of castor oil biodiesel. methanol/oil molar ratio on the material balance of transesterification
reaction. It can be concluded that castor oil is quite suitable for biodiesel
Property Value EN 14214 ASTM D 6751 production, but the usage in transportation vehicles should be also
Density (kg/m3,15 °C) 898.00 860–900 a
investigated.
a a
Refractive index (20 °C) 1.46
Acid index (mg KOH/g) 0.21 b0.50 b0.80
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