Journal of Advanced Research (2010) 1, 309–314

Cairo University

Journal of Advanced Research

ORIGINAL ARTICLE

Production of biodiesel using the microwave technique

Shakinaz A. El Sherbiny, Ahmed A. Refaat, Shakinaz T. El Sheltawy *

Department of Chemical Engineering, Faculty of Engineering, Cairo University, Egypt

Received 30 October 2009; revised 28 January 2010; accepted 8 March 2010

Available online 15 September 2010

KEYWORDS Abstract Biodiesel production is worthy of continued study and optimization of production pro-
Microwave; cedures because of its environmentally beneficial attributes and its renewable nature. Non-edible
Biodiesel; vegetable oils such as Jatropha oil, produced by seed-bearing shrubs, can provide an alternative
Transesterification; and do not have competing food uses. However, these oils are characterized by their high free fatty
Non-edible oil acid contents. Using the conventional transesterification technique for the production of biodiesel is
well established. In this study an alternative energy stimulant, ‘‘microwave irradiation’’, was used
for the production of the alternative energy source, biodiesel. The optimum parametric conditions
obtained from the conventional technique were applied using microwave irradiation in order to
compare the systems. The study showed that the application of radio frequency microwave energy
offers a fast, easy route to this valuable biofuel with the advantages of enhancing the reaction rate
(2 min instead of 150 min) and of improving the separation process. The methodology allows for
the use of high free fatty acid content feedstock, including Jatropha oil. However, this emerging
technology needs to be further investigated for possible scale-up for industrial application.
ª 2010 Cairo University. Production and hosting by Elsevier B.V. All rights reserved.

Introduction degradable and non-toxic. Further, compared to petroleum-

Biodiesel has many merits as a renewable energy resource
including being derived from a renewable domestic resource,
thereby relieving the reliance on petroleum fuel, and being bio-
* Corresponding author. Tel.: +20 10 6044605.
E-mail address: chakinaz@hotmail.com (S.T. El Sheltawy).
2090-1232 ª 2010 Cairo University. Production and hosting by
Elsevier B.V. All rights reserved.
Peer review under responsibility of Cairo University.
doi:10.1016/j.jare.2010.07.003
Production and hosting by Elsevier
based diesel, biodiesel has a more favorable combustion emis-
sion profile, such as low emissions of carbon monoxide, partic-
ulate matter and unburned hydrocarbons [1]. Fuels derived
from vegetable oils, due to their agricultural origin, are able
to reduce net CO2 emissions to the atmosphere along with im-
port substitution of petroleum products [2]. They present a
very promising alternative to diesel oil since they are renewable
and have similar properties [3]. The use of non-edible vegetable
oils compared to edible oils is very significant because of the
tremendous demand for edible oils as food. Moreover, edible
oils are far too expensive to be used as fuel at present [4].
The interest in using Jatropha curcas as a feedstock for the
production of biodiesel is rapidly growing. The properties of
the crop and its oil have persuaded investors, policy makers
and clean development mechanism (CDM) project developers
to consider Jatropha as a substitute for fossil fuels to tackle the
310 S.A. El Sherbiny et al.

challenges of energy supply and GHG emission reduction [5].

Table 1 Fatty acid profile of feedstock.
The oil produced by this crop can be easily converted to liquid
biofuel that meets the American and European standards [6]. Fatty acid Composition (wt.%)
Additionally, the press cake can be used as a fertilizer and Palmitic (16:0) 18.22
the organic waste products can be digested to produce biogas Stearic (18:0) 5.14
(CH4) [5]. The plant itself is believed to prevent and control Oleic (18:1) 28.46
soil erosion or can be used as a living fence or to reclaim waste- Linoleic (18:2) 48.18
land [7].
Microwave irradiation, an unconventional energy source,
has been used for a variety of applications including organic Table 2 Main characteristics of feedstock.
synthesis, wherein chemical reactions are accelerated because
Parameter Unit Value
of selective absorption of MW energy by polar molecules,
non-polar molecules being inert to the MW dielectric loss [8]. Viscosity mm2/s 46.6
Pour point C 3
Microwaves, representing a non-ionizing radiation, influence
Cloud point C 2
molecular motions such as ion migration or dipole rotations
Flash point C 235
without altering the molecular structure. Because the mixture Acid value mg KOH g 1
6.2
of vegetable oil, methanol, and potassium hydroxide contains Iodine value mg iodine g 1
101
both polar and ionic components, rapid heating is observed Calorific value MJ kg 1 39.54
upon microwave irradiation, and because the energy interacts
with the sample on a molecular level, very efficient heating
can be obtained. Microwave heating compares very favourably Helium was used as the carrier gas with a flow rate 1 mL/
with conventional methods, where heating can be relatively min and also as an auxiliary gas for FID. One micrometer of
slow and inefficient because transferring energy into a sample each diluted sample with analytical grade dichloromethane
depends upon convection currents and the thermal conductiv- from BDH (England) was injected. The viscosity of the origi-
ity of the reaction mixture [9]. To allow for a strict comparison nal oil and the produced biodiesel was measured using the
between microwave irradiation and conventional heating under Brookfield viscometer model DV-II.
similar conditions (reaction medium, temperature and pres- As evident from the tables, the fatty acid composition of the
sure), a monomode microwave reactor should be used. This en- oil is dominated by oleic acid (29%) and linoleic acid (48%)
sures wave focusing (reliable homogeneity in the electric field) i.e., the oil contains about 77% unsaturated fatty acid, which
and accurate control of the temperature (using an optical fibre is reflected on its pour and cloud points ( 3 and 2 C,
or infrared detection) throughout the reaction [10]. Reflux sys- respectively).
tems have been developed in an effort to use solvents in micro- Methanol (Analytical) El-Nasr Pharmaceutical Chemicals
wave assisted organic synthesis without the risk of explosion. Co. (ADWIC) Mwt. 32.04 Assay 99.8% was used. KOH was
Reflux systems are at minimal risk of explosion because they used in this study: KOH pellets purified Thann-Fransu.
are operating at atmospheric pressure and because flammable
vapors cannot be released into the microwave cavity. Production methodology
Several examples of microwave irradiated transesterifica-
tion methods have been reported incorporating adapted Biodiesel production was performed in two-step reaction
domestic ovens for use as flow systems [11] or batch laboratory mechanisms:
ovens [12] but only moderate conversions were obtained. A
more recent study used homogeneous catalysis, both in a batch  Acid-catalyzed esterification.
and in a flow system [13]. Leadbeater and Stencel reported the  Base-catalyzed transesterification.
use of microwave heating as a fast, simple way to prepare bio-
diesel in a batch mode [14]. This was followed by a continuous
flow approach allowing for the reaction to be run under atmo- Acid-catalyzed pretreatment
spheric conditions and performed at flow rates of up to 7.2 L/
min using a 4 L reaction vessel [15].
The Jatropha oil used had an initial acid value of 6.2 mg
KOH/g corresponding to a free fatty acid (FFA) level of
Experimental 3.1%, which is above the 1% limit for a satisfactory transeste-
rification reaction using an alkaline catalyst [16]. Therefore,
Materials FFAs were first converted to esters in a pretreatment process
with methanol (molar ratio methanol/oil = 6.5:1) using
The main oil treated in this investigation is Jatropha oil. The H2SO4 as catalyst (0.3%) in 90 min reaction time at 60 C [6].
fatty acid composition of the Jatropha oil used as a feedstock
for biodiesel production is given in Table 1 and the oil charac- Base-catalyzed transesterification using the conventional
teristics are given in Table 2. technique
Determination of the composition of the oil was by gas
chromatograph (Auto system XL, PerkinElmer type) using The method applied for the production of biodiesel from
fused silica capillary column 60 m · 0.32 mm (ID) at the split Jatropha oil in this research is base-catalyzed transesterifica-
ratio 1:5. The oven temperature was planned to remain at tion in a laboratory-scale setup. The reaction was performed
150 C for one min, then heated at 30 C/min up to 240 C. using methanol as alcohol and KOH as catalyst. The transeste-
Microwave biodiesel
rification process was studied at two catalyst loadings (1 and
1.5 wt.% KOH) and three alcohol to oil molar ratios (4.5:1,
6:1, and 7.5:1).
One of the most important variables affecting the yield of an
ester is the molar ratio of alcohol to triglyceride. The stoichiom-
etric ratio for transesterification requires three moles of alcohol
and one mole of triglyceride to yield three moles of fatty acid al-
kyl esters and one mole of glycerol. However, transesterification
is an equilibrium reaction in which an excess of alcohol is re-
quired to drive the reaction to the right [17]. However, an exces-
sive amount of alcohol makes the recovery of the glycerol
difficult, so that the ideal alcohol/oil ratio has to be established
empirically [18]. Most of the studies on the base-catalyzed
transesterification of WVO reported that maximum conversion
to the ester occurred with a molar ratio of 6:1 [19–22]. Transeste-
rification of pretreated waste rapeseed oil carried out by Yuan
and co-workers showed a maximum conversion at 6.5:1 of meth-
anol to oil ratio [23], whereas an earlier study by Leung and Guo
found a maximum conversion at a ratio of 7:1 [24].
Catalyst concentration is closely related to the free acidity
of the oil. When there is a large free fatty acid content, the
addition of more potassium hydroxide, or any other alkaline
catalyst, compensates this acidity and avoids catalyst deactiva-
tion [16]. The addition of an excessive amount of catalyst,
however, gives rise to the formation of an emulsion, which in-
creases the viscosity and leads to the formation of gels. These
hinder the glycerol separation and, hence, reduce the apparent
ester yield. The result of these two opposing effects is an opti-
mal catalyst concentration of about 1.0–1.5%.
Reviewing the literature indicated that it was most efficient
to fix the reaction temperature at 65 C, which is slightly above
the boiling point of methanol (64.7 C). When the reaction
temperature exceeds the boiling point of methanol, the metha-
nol will vaporize and form a large number of bubbles which
may inhibit the reaction [22,25,26]. The agitation rate was kept
at 400 rpm. Since this reaction can only occur in the interfacial
region between the liquids and also due to the fact that fats
and alcohols are not totally miscible, transesterification is a rel-
atively slow process. As a result, vigorous mixing is required to
increase the area of contact between the two immiscible phases
[27]. Stamenković and co-workers studied the effect of agita-
tion intensity on methanolysis of sunflower oil and reported
that by using the microphotographic technique, drop size dis-
tributions were found to become narrower and shift to smaller
sizes with increasing agitation speed as well as with the pro-
gress of the methanolysis reaction at a constant agitation speed
[28]. Berchmans and Hirata used an agitation intensity of
400 rpm for the two-step methanolysis of Jatropha oil [25].
All the reactions were carried out in the reaction conical flasks,
which were immersed at 65 C in a thermostatic water bath
equipped with a magnetic stirrer at 400 rpm.
Potassium methoxide solution was freshly prepared by dis-
solving the fresh KOH pellets in the predetermined amount of
methanol. Mixing was performed by continuous stirring for 5–
10 min. Warm oil was then added to the catalyst/alcohol mix-
ture and the reaction mix was kept at 65 C throughout the
reaction time. Once the reaction was completed, the reaction
mixture was poured into a 200 mL separating funnel and the
solution was allowed to settle overnight before the glycerol
layer was removed from the bottom of the separating funnel
to get the ester layer (biodiesel) to the top. In practice, the sep-
arated biodiesel layer should have been water-washed to re-
311
move the excess catalyst, alcohol and other impurities.
However, due to the small size of the oil samples used in the
glass reaction tubes, the refinement stage on this experiment
was omitted. The experiments were run in triplicate; each set
of operation conditions was conducted three times and the
average was recorded.
Microwave-assisted technique
The optimum parametric conditions that were obtained from
the conventional technique were applied using the micro-
wave-assisted technique in order to compare the systems. In
order to verify the advantages of microwave irradiation, the
technique was applied on the oil without pretreatment.
A scientific microwave with advanced vessel technology was
used. This allowed fast vessel heating with homogeneous
microwave distribution throughout the cavity. The oven used
was the Start S (Milestone), manufactured by Milestone Inc.,
USA. A normal pressure glass reactor is equipped with a
500 mL flask and a reflux condenser. The oven is supplied with
a colour touch screen controller that enables the creation, stor-
age and use of time vs. temperature or time vs. power reaction
profiles. The output microwave power is variable up to 1200
watts, controlled via a microprocessor.
The optimum parametric conditions obtained from the con-
ventional technique were applied again using microwave irra-
diation in order to compare the systems. The temperature
was adjusted to 65 C, and the oil was preheated to the desired
temperature of 65 C using the microwave unit. The alcohol–
catalyst mixture was then fed into the flask through the con-
denser, and the mixture was irradiated under reflux for differ-
ent reaction times of 1, 2 and 3 min.
Results and discussion
Results obtained by using the mechanical conventional technique
The effect of process variables on biodiesel yield
The base-catalyzed transesterification result of Jatropha oil
was investigated by changing catalyst (KOH) to oil ratios
(% w/w) and alcohol to oil ratios (% w/w). The highest con-
version was obtained with 1.5% of catalyst (KOH) to oil ratio
and 7.5:1 of methanol to oil molar ratio for 60 min, and under
these condition, the Jatropha oil methyl ester (JOME) yield
was 99.8%. Figs. 1 and 2 show biodiesel yield% with time
for KOH 1% and KOH 1.5% at different alcohol/oil molar
ratios.
One of the most important variables affecting the yield of
ester is the molar ratio of alcohol to triglyceride. In this study,
a molar ratio of 7.5:1 has given a yield of over 98%.
Biodiesel with the best properties was obtained using potas-
sium hydroxide as the catalyst in many studies [29–32]. Meth-
anolysis with 1 wt.% KOH catalyst resulted in successful
conversion giving the best yields and viscosities of the esters
in most of the literature reviewed. However, using a concentra-
tion of 1.5% showed better results in this study.
Results obtained by using the microwave-assisted technique
Applying the microwave technique as previously described in
the Experimental section showed that the application of radio
312
Fig. 1 Effect of alcohol/oil molar ratios on biodiesel yield using
KOH 1% as catalyst.
Fig. 2 Effect of alcohol/oil molar ratios on biodiesel yield using
KOH 1.5% as catalyst.
frequency microwave energy enhances the reaction rate for the
conversion of Jatropha oil to biodiesel, and drives the reaction
equilibrium toward the production of biodiesel. Highest bio-
diesel yield (97.4%) was obtained by applying microwave irra-
diation for two minutes compared to 1 h with the conventional
technique. The results are depicted in Fig. 3.
It should be pointed out, however, that these results were
achieved by using Jatropha oil without pretreatment. It was
also evident that exceeding the optimum reaction time will lead
to deterioration of biodiesel yield. The interpretation of these
results requires further investigation. The most accepted inter-
pretation is that the exceeded time favours the equilibrium in
the reverse direction. Attributing the decrease in yield after
exceeding the optimum time to cracking followed by oxidizing
of the formed fatty acid methyl esters to aldehydes, ketones
and lower chained organic fractions could be excluded because
the GC results do not show peaks of oxygenated compounds
[33].
Quality assessment of produced biodiesel
Quality assessment was performed using physical parameters
such as viscosity, flash point and calorific value, as shown in
Table 3.
The viscosity difference forms the basis of an analytical
method, viscometry, applied to determine the conversion of
vegetable oil to methyl ester. The viscosity difference between
S.A. El Sherbiny et al.
Fig. 3 Effect of time on biodiesel yields from Jatropha oil using
microwave irradiation.
Table 3 Quality assessment of biodiesel production from
Jatropha oil.
Property JOME ASTM D 6751 EN 14214
Viscosity (mm2/s) 5.8 1.9–6.0 3.5–5.0
Flash point (C) 185 P130 P120
component triacylglycerols of vegetable oils and their corre-
sponding methyl esters resulting from transesterification is
approximately one order of magnitude [34]. Kinematic viscos-
ity has been included in biodiesel standards (1.9–6.0 mm2/s in
ASTM D6751 and 3.5–5.0 mm2/s in EN 14214) [35].
The viscosity of the produced biodiesel was calculated using
the Brookfield viscometer Model DV-II and was found to be
5.8 mm2/s. The result obtained is compatible with the reports
from other studies on biodiesel from Jatropha oil. Kumar
and Sharma reported a value of 5.65 mm2/s [36].
The flash point of the produced biodiesel was estimated to
be 185 C. This flash point is quite high compared to diesel.
Hence, biodiesel is extremely safe to handle. The high flash
point was referred to in many previous literature; Agarwal
and Agarwal reported a flash point of 191 C compared to
71 C for mineral diesel [2], and Kumar and Sharma reported
a flash point of 170 C for Jatropha oil methyl ester (JOME)
[36].
The calorific value (MJ/Kg) for the produced Jatropha bio-
diesel is 39.632 compared to 45.343 for mineral diesel.
Comparing the results with those obtained from neat and waste
edible oils
The results obtained from this study on Jatropha-based biodie-
sel are confirming the results obtained in a previous study con-
ducted by Refaat and co-workers on neat and waste edible
vegetable oils [33] which also showed that no substantial differ-
ences were obtained from different oil origins. Hence, it can be
concluded that biodiesel produced from Jatropha oil is at least
not inferior to that produced from edible oils.
Conclusion
From the obtained results, using the conventional technique,
the best yield % for the production of biodiesel from Jatropha
oil was obtained using a methanol/oil molar ratio of 7.5:1,
potassium hydroxide as catalyst (1.5%), and a reaction time
Microwave biodiesel
of one hour with the reaction temperature maintained at
65 C. The study also showed that the quality of the produced
biodiesel satisfies the international American and European
standards; hence, inedible vegetable oils such as Jatropha oil,
produced by seed-bearing shrubs, can provide an alternative,
and they do not have competing food uses.
The results showed that application of radio frequency
microwave energy offers a fast, easy route to this valuable bio-
fuel with advantages of enhancing the reaction rate and
improving the separation process. The reaction time was re-
duced to 2 min instead of 150 minutes (90 min for the pretreat-
ment process and 60 min for transesterification), because, by
using the microwave technique, no pretreatment is required.
The methodology also allows for the use of high free fatty acid
content feedstock, including Jatropha oil. However, this will
need time control, otherwise the yield may be affected.
Acknowledgements
Sincere thanks are due to both Prof. Dr. Guzine El-Diwani
and Dr. Nahed Kamal of the Chemical Engineering Depart-
ment – National Research Center – Dokki – Egypt, for gener-
ously offering the oil and equipment. Thanks are also due to
M.A. Refaat, A.M. Hanafy, M.M. Hassen and M.S. Sakr,
the undergraduate students in the Department of Chemical
Engineering, Cairo University, for their efforts.
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