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Energy Sources, Part A: Recovery,

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Potassium Ion Impregnated Calcium

Oxide as a Nanocrystalline Solid Catalyst
for Biodiesel Production from Waste
Cotton Seed Oil
a a
D. Kumar & A. Ali
a
School of Chemistry and Biochemistry, Thapar University, Patiala,
India
Published online: 26 Mar 2014.

To cite this article: D. Kumar & A. Ali (2014) Potassium Ion Impregnated Calcium Oxide as a
Nanocrystalline Solid Catalyst for Biodiesel Production from Waste Cotton Seed Oil, Energy
Sources, Part A: Recovery, Utilization, and Environmental Effects, 36:10, 1093-1102, DOI:
10.1080/15567036.2010.545797

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 Energy Sources, Part A, 36:1093–1102, 2014
Copyright © Taylor & Francis Group, LLC
ISSN: 1556-7036 print/1556-7230 online
DOI: 10.1080/15567036.2010.545797

Potassium Ion Impregnated Calcium Oxide as a

Nanocrystalline Solid Catalyst for Biodiesel
Production from Waste Cotton Seed Oil
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D. Kumar1 and A. Ali1

1
School of Chemistry and Biochemistry, Thapar University, Patiala, India

Vegetable oil and animal fat derived fatty acid methyl esters are commonly known as biodiesel and
provide an environment friendly and renewable substitute for the conventional diesel fuel. The present
work demonstrates an easy preparation of potassium ion impregnated calcium oxide in nano crystalline
form (supported by powder X-ray diffraction and transmission electron microscopic studies) and its
application as a solid catalyst for the transesterification of waste cottonseed oil with methanol. The
catalyst prepared by impregnating 3.5 wt% of potassium in CaO support was found to show the
best catalytic activity among the prepared catalysts. The same catalyst was found to be effective
for the complete transesterification of less expensive feedstock, waste cotton seed oil, even in the
presence of 10.26 wt% moisture and 4.35 wt% free fatty acid contents. The selected catalyst has also
been reused successfully for three catalytic cycles. Few physicochemical properties of the prepared
biodiesel sample have been studied and found to be within the acceptable limits of EN 14214
standards.

Keywords: nano particles, solid catalyst, transesterification, waste cotton seed oil and biodiesel quality

INTRODUCTION

The diminishing traditional mineral diesel fuel resources, increasing crude oil price, and environ-
ment concerns have encouraged the search for a diesel fuel alternate. In this contest, biodiesel
being renewable, ecofriendly, and carbon neutral was found to be a promising diesel fuel substitute
(Ma and Hanna, 1999). The transesterification of vegetable oil or animal fat with methanol in the
presence of acid or alkali or enzyme catalyst yielded glycerol and a mixture of fatty acid methyl
esters commonly known as biodiesel (Lopez et al., 2008).
Homogeneous alkali or acid catalyzed transesterification reactions are usually faster and do not
require harsh reaction conditions; however, major drawbacks of such catalysts include the contami-
nation of biodiesel and glycerol, deactivation of alkali catalysts by high free fatty acid and moisture
contents, deactivation of acid catalysts by high moisture contents, and their nonrecyclability (Ma

Address correspondence to Dr. Amjad Ali, School of Chemistry and Biochemistry, Thapar University, Patiala 147004,
India. E-mail: amjadali@thapar.edu

1093
 1094 D. KUMAR AND A. ALI

and Hanna, 1999; Demirbas, 2007). In the recent past, to overcome the problems associated with
homogeneous catalysts, efforts have been directed by researchers to develop solid catalysts for the
transesterification reaction. A variety of heterogeneous chemical catalysts for the transesterification
reactions of triglycerides were reported in the literature, including calcium carbonate (Suppes
et al., 2001), alkali earth oxides (Demirbas, 2007) and transition metal oxides (Stern et al.,
1999), sulphated zirconia (Charusiri et al., 2006), zeolites (Brito et al., 2007), alkylguanidines
heterogenized on organic polymers (Schuchardt et al., 1995), and supported mesoporous materials
(Li and Rudolph, 2008). Due to ease of preparation, being less costly, and non toxic, pure and
alkali metal supported CaO (Meher et al., 2006; Watkins et al., 2004; Kumar and Ali, 2010),
MgO (Ilgen and Akin, 2009), and ZnO (Xie et al., 2007) have been studied extensively as solid
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catalysts for the transesterification reaction of a variety of triglycerides.

Kumar and Ali (2010) have recently reported the preparation of Li/CaO in nano particle form
and successfully demonstrated its application as solid catalyst for the complete transesterification
of waste cotton seed oil even in the presence of high free fatty acid (15 wt%) and moisture
contents (6 wt%).
In continuation to the authors’ earlier work and to study the effect of KC impregnation on CaO
activity, the present study demonstrates the preparation of KC impregnated CaO in nano-sized
form and its characterization by powder X-ray diffraction (XRD), scanning electron microscopy
(SEM), transmission electron microscopy (TEM), and surface area measurement studies. The
prepared catalyst has been used as solid catalyst for the transesterification of waste cotton seed
oil, and a few physicochemical properties of the prepared biodiesel were also studied.

EXPERIMENTAL

Materials and Methods

Waste cooking oil was collected from local restaurants located in Patiala. Palmitic acid, KNO3 ,
and silica gel for thin layer chromatography (TLC), of reagent grade quality were purchased from
Loba Chemie, India and used as such without further purification. Methanol (99.8%) used in the
present study was obtained from Merck, India and methyl oleate (99%) used as biodiesel standard
was procured from Sigma-Aldrich, USA.
The catalyst characterization has been performed using the instruments and procedures for
powder XRD, Brunauer-Emmett-Teller (BET) surface area, SEM, TEM, and Hammett indicators
studies as reported earlier (Kumar and Ali, 2010).

Preparation of Catalyst
The nanocrystalline potassium metal ion impregnated calcium oxide was prepared by the wet
impregnation method as reported in the literature (Watkins et al., 2004) with a slight modification.
In a typical preparation, CaO (10 g) was suspended in 40 mL of deionized water and to this 10
mL aqueous solution of desired potassium nitrate concentration was added to obtain KC loading
in CaO in the range of 1.5–4.5 wt%. The resulted slurry was stirred for 3 h, then evaporated to
dryness and heated at 180ıC for 24 h and the solid thus obtained was characterized by flame
photometry, powder XRD, BET surface area measurement, a Hammett indicator test, FESEM and
TEM techniques.
The prepared catalysts were designated as K-CaO-XX, where XX represents the potassium
concentration (wt%) in CaO, e.g., K-CaO-3.5 represents the catalyst prepared by impregnating
3.5 wt% of KC (using KNO3 ) in CaO.
 BIODIESEL PRODUCTION FROM WASTE COTTON SEED OIL 1095

Transesterification of Waste Cottonseed Oil

All transesterification reactions were performed in a 100-mL, two-neck round bottom flask equipped
with a water-cooled condenser, oil bath, and a magnetic stirrer. In a typical transesterification
reaction, 10 g of waste cottonseed oil, different molar concentrations of methanol, and catalyst
were heated up to 65ıC till the completion of the reaction.
To monitor the progress of the reaction, the samples from the reaction mixture have been
withdrawn after every 15 min with the help of a glass capillary, and subjected to TLC analysis
using hexane/ethyl acetate/acetic acid (90:9:1, v/v) as mobile and silica gel on a glass plate as the
stationary phase. Biodiesel shows higher mobility .Rf D 0:65/ than vegetable oil .Rf D 0:26/
with the selected solvent system, and complete conversion of vegetable oil to biodiesel was
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supported by the disappearance of vegetable oil spot on the TLC plate.

After the completion of the reaction, the reaction mixture was filtered through the ordinary
filter paper and excess methanol from the same was recovered with the help of a rotary evaporator.
The reaction mixture thus obtained was kept in a separating funnel for 12 h to separate the lower
glycerol layer from the upper biodiesel layer. Biodiesel, thus obtained, was further characterized
by 1 H NMR (Figure S1 in electronic supporting information) and the same technique has also been
used for the quantification of biodiesel by following the literature reported procedure (Knothe,
2001).

RESULTS AND DISCUSSION

Catalyst Preparation and Characterization

The basic strength (H_) of the pure CaO was found to be in the range of 9.8–10 and the same
was found to increase from 10.1–11.1 to 11.1–15.1 as the potassium ion concentration in CaO
was increased from 1.5 to 3.5 wt% as given in Table 1. Further increases in potassium ion
concentration (4.5 wt%) were not found to increase the basic strength of the calcium oxide
support. The enhancement of the basic strength of CaO after potassium ion impregnation could
be due to the formation of strong basic sites on the CaO surface (Kumar and Ali, 2010).
The surface area of pure calcium oxide and K-CaO-3.5 was measured by BET method and
the same was found to be decreased marginally after impregnating the CaO with 3.5 wt% of
potassium as shown in Table 1. It could be due to the plugging of the pores of the solid support
upon potassium impregnation (Meher et al., 2006).
The comparisons of the powder XRD patterns of pure CaO with 1.5–4.5 wt% potassium
impregnated CaO are shown in Figure 1. The pure CaO shows that intense peaks at 2 D 37:37,

TABLE 1
Comparison of BET Surface Area and Basic Strength of CaO with
That of Potassium Ion Impregnated CaO

BET Basic
Catalyst Surface Strength,
S. No. Type Area, m2 /g H_

1 CaO 3.9630 9.8 < H_ < 10.1

2 K-CaO-1.5 — 10.1 < H_ < 11.1
3 K-CaO-2.5 — 10.1 < H_ < 11.1
4 K-CaO-3.5 3.8973 11.1 < H_ < 15.0
5 K-CaO-4.5 — 11.1 < H_ < 15.0
 1096 D. KUMAR AND A. ALI
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FIGURE 1 Comparison of powder XRD patterns of (a) pure CaO with (b) K-CaO-1.5, (c) K-CaO-2.5, (d) K-
CaO-3.5, and (e) K-CaO-4.5.

53.89, and 32.18 correspond to the d-values of 2.39, 1.69, and 2.78, respectively, of calcium oxide
in cubic form (JCPDS No. 821691), while peaks at 2 D 34:11, 18.11, and 47.19 correspond
to the d-values of 2.60, 4.88, and 1.90, respectively, of calcium hydroxide in hexagonal form
(JCPDS No. 841276), as shown in Figure 1. The absence of the diffraction patterns of KNO3
could be either due to its high degree of dispersion on the CaO surface or its concentration being
smaller than those detectable by the powder XRD technique. The particle size of the K-CaO-3.5
catalyst was determined by Debye-Scherrer method (Qadri et al., 1999) using powder XRD data
and found to be about 48 nm.
FESEM studies of K-CaO-3.5 show that it has hexagonal and irregular shaped clusters of 2–5
m-sized particles as shown in Figure 2a. The TEM analysis of the same particles shows that
these are the clusters of further smaller particles with an average size of about 30 nm as shown
in Figure 2b.

Transesterification Reactions and Biodiesel Characterization

The transesterification reaction of waste cottonseed oil (10 g) with varying molar concentrations
of methanol, and catalyst amounts were performed at the desired temperature. All reactions have
been carried out till the completion of the reaction by varying one parameter at a time in order
to optimize the reaction conditions for complete transesterification of waste cotton seed oil in
minimum time.
Fatty acid methyl esters (biodiesel) produced during the transesterification reaction were quan-
tified and characterized by 1 H NMR spectroscopy. The conversion of the cotton seed oil to
corresponding biodiesel was determined by measuring the areas under the –OCH3 (X) and ˛-CH2
(Y) proton signals in 1 H NMR spectrum of biodiesel and using the literature reported formula
(Knothe, 2001) as given below:

% conversion of oil to biodiesel D f2X=3Y g  100:

 BIODIESEL PRODUCTION FROM WASTE COTTON SEED OIL 1097
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FIGURE 2 (a) SEM and (b) TEM images of K-CaO-3.5.

During the course of study, the effect of the following parameters on catalytic activity have been
studied: (i) impregnated potassium ion concentration, (ii) catalyst concentration, (iii) reaction
temperature, (iv) methanol/oil molar ratio, (v) the presence of moisture content (0.26–10.26 wt%),
and (vi) the presence of free fatty acid content (0.35–4.35 wt%).

Effect of Catalyst Concentration and Reaction Temperature

A series of transesterification reactions were performed at 65ıC using 18:1 molar ratio of methanol
to oil in the presence of 1–15 wt% (catalyst/oil) of nanocrystalline K-CaO-3.5 in order to determine
the optimum catalyst concentration. The time required for the complete conversion of vegetable
oil to biodiesel decreases from 7 to 2.5 h as the catalyst concentration was increased from 1 to 10
wt% (Figure S2 in electronic supporting information). Further increase in catalyst concentration
does not reduce time required for the complete transesterification of waste cottonseed oil.
Similarly, to optimize the reaction temperature, a series of transesterification reactions were
conducted in the temperature range of 35 to 75ıC using 10 wt% (catalyst/oil) of catalyst and
18:1 molar ratio of methanol to oil. The time required for the complete transesterification of oil
to biodiesel decreases from 7.5 to 2.5 h as the reaction temperature was increased from 35 to
65ı C. Further increase in reaction temperature does not reduce the time required for the complete
transesterification of oil to biodiesel (Figure S3 in electronic supporting information). Hence, all
transesterification reactions in the present study have been performed at 65ıC using 10 wt% of
catalyst.

Effect of Impregnated Potassium Ion Concentration

To determine the optimum potassium ion concentration in CaO for the best catalytic activity, a
series of catalysts was prepared by varying the amount of potassium in the range of 1.5–4.5 wt%
(K/CaO). The transesterification reaction of waste cottonseed oil was performed with methanol
(methanol/oil D 18:1, m/m) at 65ıC in the presence of prepared catalysts. Reaction time required
for the complete transesterification was found to decrease from 3.5 to 2.5 h as the amount of
potassium ion in CaO were increased from 1.5 to 3.5 wt%. However, further increase in KC
 1098 D. KUMAR AND A. ALI
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FIGURE 3 Effect of potassium ion concentration in CaO on the time required for complete transesterification
of waste cottonseed oil to biodiesel.

ion concentration does not reduce the reaction time as shown in Figure 3 and, hence, K-CaO-
3.5 catalyst was selected for optimizing other parameters to achieve the minimum time for the
complete transesterification reaction.

Effect of Methanol/Oil Molar Ratio

The methanol/oil molar ratio used during the transesterification reaction is one of the important
parameters that determines the methyl ester yield as well as cost of the biodiesel production.
Theoretical minimum methanol to oil molar ratio should be 3:1 for the complete conversion of
vegetable oil to biodiesel. Heterogeneous catalysts usually catalyzed the transesterification reaction
at a slower rate and often required higher methanol to oil (up to 275:1) molar ratios as reported
in the literature (Xie et al., 2005).
To determine the optimum methanol/oil molar ratio in the present study, the reactions were
performed with 9:1 to 27:1 molar ratios at 65ıC using 10 wt% of K-CaO-3.5 catalyst. The rate of
transesterification reaction increases as methanol/oil molar ratio was increased from 9:1 to 18:1
and reactions were found to be completed in 2.5 h when 18:1 molar ratio of MeOH and oil was
used. Further increase in methanol/oil molar ratio does not decrease the reaction time significantly,
as shown in Figure 4.

Effect of Moisture Content

The presence of water (>0.3 wt%) in vegetable oil, used as feedstock for the transesterification
reaction, leads to the formation of soap instead of biodiesel in the presence of homogenous
catalyst. The waste cotton seed oil used in the present study was found to have 0.26% moisture
contents, and transesterification reaction of the same using NaOH or KOH as the catalyst leads
to the saponification reaction. However, the same reaction when catalyzed by nanocrystalline
K-CaO-3.5 yielded the complete conversion of oil to biodiesel. In order to determine the max-
imum moisture resistance of K-CaO-3.5 catalyst, transesterification reactions were performed in
the presence of 0.26–10.26 wt% (water/oil) water. The catalyst was found to be effective for
 BIODIESEL PRODUCTION FROM WASTE COTTON SEED OIL 1099
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FIGURE 4 Effect of methanol/oil molar ratio on the time required for complete transesterification of waste
cottonseed oil to biodiesel.

the complete transesterification of cotton seed oil in 10 h even when 10.26 wt% of moisture
contents were present in the reaction mixture as shown in Figure 5. The addition of >10.26 wt%
moisture contents in the reaction mixture was found to cause the saponification of the cotton
seed oil.

Effect of Free Fatty Acid (FFA) Content

Like moisture contents, presence of FFAs (>0.5 wt% of oil) leads to the saponification instead of
transesterification when the reaction is catalyzed by a homogeneous catalyst. Waste cotton seed

FIGURE 5 Effect of moisture contents on the time required for complete transesterification of used cottonseed
oil to biodiesel.
 1100 D. KUMAR AND A. ALI
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FIGURE 6 Effect of free fatty acid contents on the time required for complete transesterification of waste
cottonseed oil to biodiesel.

oil used in the present study was found to have 0.35 wt% FFAs, and transesterification reaction
of the same using NaOH or KOH as homogenous catalyst leads to the formation of soap instead
of biodiesel. However, the same reaction when catalyzed by nanocrystalline K-CaO-3.5 yielded
the complete conversion of oil to biodiesel in 2.5 h. In order to determine the maximum FFA
tolerance of the prepared catalyst, transesterification reaction of the waste cotton seed oil was
performed in the presence of 0.35–4.35 wt% FFA by adding palmitic acid in the reaction mixture.
The catalyst K-CaO-3.5 was found to be effective for the complete transesterification of waste
cotton seed oil in 10.25 h even when 4.35 wt% of FFA were present in the reaction mixture as
shown in Figure 6. Further addition of FFAs (>4.35 wt%) in the reaction mixture resulted in
partial transesterification of the cotton seed oil, could be due to the deactivation of the catalyst
by high FFA amount.

Reusability of the Catalyst

To test the reusability of K-CaO-3.5 catalyst, it was recovered from the reaction mixture by
filtration, washed with hexane, and dried at 100ıC. The catalyst thus recovered was used for
the second and third catalytic run, respectively, under the same experimental condition and
regeneration method. The reused catalyst was also found to complete (>99% conversion) the
transesterification of waste cotton seed oil though it required 4.3 and 5.8 h of reaction period
when reused for the second and third catalytic cycle respectively, as shown in Figure 7.

Physicochemical Properties of Prepared Biodiesel

Determination of the physicochemical properties of the fuel is important to ensure its quality.
Hence, key physicochemical properties of the biodiesel prepared from waste cotton seed oil have
been studied, and measured values were found within the acceptable limits of European Standard
EN 14214, as shown in Table 2.
 BIODIESEL PRODUCTION FROM WASTE COTTON SEED OIL 1101
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FIGURE 7 Reusability of the catalyst for the transesterification of the waste cotton seed oil.

CONCLUSIONS

The present work demonstrates the preparation of a KC impregnated CaO catalyst in nano particle
form and its application towards the transesterification of used cottonseed oil. The catalyst prepared
by impregnating 3.5 wt% of KC in CaO was found to be most effective and required 2.5 h of
reaction period for the complete transesterification of used cottonseed oil when 18:1 molar ratio
of methanol to oil was used at 65ı C. The same catalyst has been reused for three catalytic cycles
and found to be effective for the complete transesterification of oil, even in the presence of 10.26
wt% moisture and 4.35 wt% of FFA contents. Hence, the reported catalyst has the potential to
convert the low quality and cheap feedstock into biodiesel. The physicochemical properties of the
prepared biodiesel sample have been tested, and observed values were found within the limits of
EN 14214 specifications.

TABLE 2
Physicochemical Properties of the Biodiesel Prepared from Waste Cottonseed Oil Using
K-CaO-3.5 as Catalyst

S. No. Parameters CBD EN 14214 Test Method

1 Ester content (wt%) >99 96.5 1 H-NMR

2 Flash point (ı C) 110 100–170 ASTM D 93

3 Pour point (ı C) 6 — ASTM D 2500
4 Kinematic viscosity at 40ı C 3.94 1.9–6.0 ASTM D 445
5 Calorific value (MJ/kg) 40 — IS 1350 P:2
6 Iodine value 84 <120 EN 14111
7 Ash (%) 0.02 0.02 ASTM D 874
8 Density at 31ı C (g/ml) 0.80 0.86–0.89 IS 1448 P:32
9 Water (%) 0.05 0.5 ASTM D 2709
10 Acid number (mg KOH/g) 0.12 0.8 ASTM D 664
11 K (ppm) 1.5 <5 ASTM D 1318
 1102 D. KUMAR AND A. ALI

ACKNOWLEDGMENTS

A. A. acknowledges the School of Chemistry and Biochemistry, Thapar University for providing
the necessary research facilities. The authors also wish to acknowledge SAIF (Punjab University)
for powder XRD, NMR, and TEM; Matter Lab (Thapar University) for FESEM and EDS; and
Kunash Instruments for surface area measurement studies.

FUNDING
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D. K. acknowledges the JRF from DST. A. A. acknowledges the DST, New Delhi (Ref. No.:
SR/FTP/CS-30/2007), and DRDO (Ref. No.: ERIP/ER/0803708/M/01/1175) for the financial
support.

SUPPLEMENTAL MATERIAL

Supplemental data for this article can be accessed on the publisher’s website.

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