Hindawi Publishing Corporation

The Scientific World Journal

Volume 2013, Article ID 460923, 7 pages
http://dx.doi.org/10.1155/2013/460923

Research Article
Calcium Oxide Derived from Waste Shells of Mussel,
Cockle, and Scallop as the Heterogeneous Catalyst for
Biodiesel Production
Achanai Buasri,1,2 Nattawut Chaiyut,1,2 Vorrada Loryuenyong,1,2
Phatsakon Worawanitchaphong,1 and Sarinthip Trongyong1
1

Department of Materials Science and Engineering, Faculty of Engineering and Industrial Technology, Silpakorn University,
Nakhon Pathom 73000, Thailand
2
National Center of Excellence for Petroleum, Petrochemicals and Advanced Materials, Chulalongkorn University,
Bangkok 10330, Thailand
Correspondence should be addressed to Achanai Buasri; achanai130@gmail.com
Received 27 August 2013; Accepted 1 October 2013
Academic Editors: H. Noritomi and H. Yahiro
Copyright 2013 Achanai Buasri et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
The waste shell was utilized as a bioresource of calcium oxide (CaO) in catalyzing a transesterification to produce biodiesel
(methyl ester). The economic and environmen-friendly catalysts were prepared by a calcination method at 7001,000 C for
4 h. The heterogeneous catalysts were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron
microscopy (SEM), and the Brunauer-Emmett-Teller (BET) method. The effects of reaction variables such as reaction time, reaction
temperature, methanol/oil molar ratio, and catalyst loading on the yield of biodiesel were investigated. Reusability of waste shell
catalyst was also examined. The results indicated that the CaO catalysts derived from waste shell showed good reusability and had
high potential to be used as biodiesel production catalysts in transesterification of palm oil with methanol.

1. Introduction
Recently, alternative energies have been focused worldwide
because of recent energy crisis. Biodiesel is one of the
interesting alternative fuels which can be produced from
renewable sources [1]. It can be easily synthesized through
transesterification of oil or esterification of fats using basic
or acidic catalysts with heating functions [2]. Conventional
homogeneous catalysts are expected to be replaced by heterogeneous catalysts mainly in the near future because of
environmental constraints and simplifications in the existing
processes. Solid catalysts could be easily separated from the
reaction mixture by filtration and then reused [3]. Heterogeneous base catalysts eliminate the need for the neutralization
of homogeneous base catalysts with acids and the removal
of water in the commercial production of biodiesel, thereby
lowering its production cost [4]. Among the heterogeneous
catalysts that are being used in transesterification, calcium
oxide (CaO) has a promising place, and many reports have

been published on CaO-catalyzed transesterification using

laboratory grade. It is cheap, abundantly available in nature
(as limestone), and some of the sources of this compound are
renewable (waste material consisting of calcium carbonate,
CaCO3 ) [5]. However, the utilization of waste materials as
heterogeneous catalysts has been of recent interest in the
search for a sustainable process [6].
The catalyst synthesized with the waste shells opens door
for renewable catalyst and at the same time recycles the
waste generated. Utilization of these waste materials not only
reduces the catalyst cost but also promotes environmentally
benign process. These shells may also find their utility in other
base catalyzed important organic reactions which will add
value to the waste generated [7]. Mussel, cockle, and scallop
are found in several parts of Thailand. The production of
mussel, cockle, and scallop is quite large and the processing of
this food also produces significant amounts of shell waste. In
this paper, we utilized waste mussel, cockle, and scallop shells
as the source of CaO for transesterification of palm oil into

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Mussel

Cockle

Scallop

Natural shell

Calcined

Crushed

Figure 1: Preparation of CaO catalyst derived from waste shell (1,000 C).

biodiesel. The effects of reaction time, reaction temperature,

methanol/oil molar ratio, catalyst loading, and reusability of
catalyst were systematically investigated.

2. Experimental
2.1. Materials. Palm oil was purchased from Morakot Industries Public Company Limited, Thailand. The molecular weight and density of the oil were measured to be
851.06 g/mole and 0.868 g/cm3 , respectively. The mussel,
cockle, and scallop shells were collected as wastes from
university cafeterias. The waste shells were rinsed with water
to remove dust and impurities and were then dried in an oven.
All chemicals were analytical-grade reagents (Merck, >99%
purity) and were used as received.

2.2. Catalysts Preparation. The catalysts were prepared by

a calcination method. The dried waste shells were calcined
at 7001,000 C in air atmosphere with a heating rate of
10 C/min for 4 h [2]. The solid result was crushed and sieved
to pass 100200 mesh screens. The products (3875 m)
were obtained as white powder. All calcined samples were
kept in the close vessel to avoid the reaction with carbon
dioxide (CO2 ) and humidity in air before being used. Figure 1
illustrated the preparation process of waste shell-derived
catalyst.

2.3. Catalysts Characterization. The X-ray diffraction (XRD)

characterization of the waste shell-derived catalyst was performed on a Rigaku (MiniFlex II, England) based generator
X-ray diffractometer using CuK radiation over a 2 range
from 20 to 80 with a step size of 0.04 at a scanning speed
of 3 /min.

The elemental chemical compositions of the materials

were analyzed by X-ray fluorescence spectroscopy (XRF
Oxford, ED-2000, England) under energy dispersive mode
for precise measurement of both light and heavy elements.
The microstructures of the calcined waste shells were
observed by a scanning electron microscope (SEM). The
SEM images of the representative sample were obtained from
a Camscan-MX 2000 (England) equipped with an energy
dispersive spectroscope (EDS).
To evaluate the surface area, mean pore diameter, and
pore volume, adsorption-desorption of nitrogen (N2 ) at 77 K
was carried out by a Quantachrome Instrument (Autosorb-1
Model No. ASIMP.VP4, USA). Before taking adsorption data,
degassing at 120 C and a residual pressure of 300 m Hg for
24 h was performed using the degas port. The surface area was
calculated using the Brunauer-Emmett-Teller (BET) equation
and the mean pore diameter and pore volume was obtained
by applying the Barret-Joyner-Halenda (BJH) method on the
desorption branch [8].

2.4. Transesterification of Palm Oil. The synthesis of biodiesel

from palm oil and methanol was carried out in a 500 mL glass
reactor equipped with condenser and mechanical stirrer at
atmospheric pressure. The effects of reaction time (2 to 6 h),
reaction temperature (50 to 70 C), methanol/oil molar ratio
(6 to 18), catalyst loading (5 to 25 wt.%), and reusability of
catalyst (1 to 4 times) on the conversion to biodiesel were
studied. After a certain period of time, a known amount
of sample was taken out from the reactor for analysis. All
experiments were repeated 3 times and the standard deviation
was never higher than 7% for any point.
Composition of the fatty acid methyl ester (FAME) was
analyzed with gas chromatograph-mass spectrometry (GCMS QP2010 Plus, Shimadzu Corporation, Japan) equipped
with a flame ionization detector (FID) and a capillary column

The Scientific World Journal

1000 C

Mussel shell
Intensity (a.u.)

Intensity (a.u.)

900 C
800 C

Cockle shell

700 C

Scallop shell

Natural

20

30

40

50
2 (deg)

60

70

20

80

30

40

50

60

70

80

2 (deg)

Figure 2: XRD patterns of natural and calcined mussel shell (:

CaCO3 , : CaO).

Figure 3: XRD patterns of waste mussel, cockle, and scallop shell

calcined at 1,000 C (: CaO).

30 m 0.32 mm 0.25 m (DB-WAX, Carbowax 20 M). Yield

of FAME was calculated by:

Table 1: Chemical compositions of waste shell-derived catalyst.

Yield (%) =

100,

(1)

where is the mass of internal standard added to the

sample, is the peak area of internal standard, is the
mass of the biodiesel sample, and is the peak area of the
biodiesel sample [9, 10]. The physical and chemical properties
of FAME including kinematic viscosity, density, flash point,
cloud point, pour point, acid value, and water content were
analyzed according to ASTM methods [11].

3. Results and Discussions

3.1. Characterization of Waste Shell and CaO Catalyst. The
XRD patterns of natural and calcined mussel shell are given in
Figure 2. XRD results revealed that the composition of natural mussel shell mainly consists of CaCO3 with the absence of
CaO peak, as indicated by diffraction peak at 2 around 29.2
[5]. However, with the increase in calcination temperature,
CaCO3 completely transforms to CaO by evolving the carbon
dioxide (CO2 ). The composition of calcined catalyst at and
above 900 C mainly consists of the active ingredient (CaO).
Narrow and high intense peaks of the calcined catalyst define
the well-crystallized structure of the CaO catalyst [6]. The
major component of the calcined waste shell at 1,000 C for
4 h was CaO species (Figure 3). The result reveals sharp XRD
reflections with (1 1 1), (2 0 0), (2 2 0), (3 1 1), and (2 2
2) orientations, implying that the calcined material was well
crystallized during the heat treatment process [2].
The chemical compositions of the catalyst are presented
in Table 1. The major mineralogical component is CaO. The
waste mussel, cockle, and scallop shells-derived catalysts
have concentration of CaO 98.37, 99.17, and 97.53 wt.%,
respectively.
The morphology of waste mussel, cockle, and scallop
shell calcined at 1,000 C was examined by SEM (Figure 4).

Compound
CaO
Na2 O
SO3
P2 O5
SrO
ZrO2
Cl
Fe2 O3

Mussel shell
98.367
0.937
0.293
0.163
0.158
0.046
0.037

Concentration (wt.%)
Cockle shell
Scallop shell
99.170
97.529
0.438
0.565
0.117
1.568
0.096
0.204
0.132
0.107

0.027

0.026

Table 2: The physical properties of waste shell-derived catalyst.

Derived catalyst
Mussel shell Cockle shell Scallop shell
Surface area (m2 /g)
89.91
59.87
74.96
0.130
0.087
0.097
Pore volume (cm3 /g)

Mean pore diameter (A)

34.55
25.53
30.55
Physical property

The natural shell displays a typical layered architecture

[12]. With the calcination temperature rising from 700 to
1,000 C, the microstructures of natural shell are changed
significantly from layered architecture to porous structure
[13]. The calcined cockle shell and scallop shell showed
similar particle morphology with the calcined mussel shell.
The calcined waste shells were irregular in shape, and some
of them bonded together as aggregates. However, the smaller
size of the grains and aggregates could provide higher specific
surface areas. Since all samples are considered to be lessporous or even nonporous, the size of the particle should
directly respond to the surface area [14].
The physical properties of the CaO catalyst are summarized in Table 2. The waste mussel shell-derived catalyst
had a large surface area (89.91 m2 /g) and pore volume
(0.130 cm3 /g), and presented a uniform pore size. The cockle

The Scientific World Journal

(a)

(b)

(c)

Figure 4: SEM images of (a) mussel shell, (b) cockle shell, and (c) scallop shell calcined at 1,000 C.

3.2. Effect of Reaction Variables. The yield of biodiesel was

affected by reaction variables, such as reaction time, reaction
temperature, methanol/oil molar ratio, catalyst loading, and
reusability of catalyst. The reaction variables were associated
with the type of catalysts used [16]. Therefore, the effect of
reaction variables was studied in the presence of waste shellderived catalyst. For the following reactions, all the catalysts
were prepared by calcinning waste shells at 1,000 C for
4 h.
The effect of reaction time on the conversion of palm
oil to biodiesel was investigated. Reaction time is one of the
key parameters during the transesterification carried out in
glass reactor. Figure 5 shows an increase in the yield with
time from 2 to 3 h with a catalyst amount of 10 wt.% relative
to oil and a methanol/oil molar ratio of 9 : 1. The maximum
yields of 97.23, 94.47, and 96.68% were obtained in 4 h at
65 C for mussel, cockle and scallop shell, respectively. In the
initial stages of the transesterification reaction, production
of biodiesel was rapid, and the rate diminished and finally

100
95
Yield of biodiesel

and scallop shell-derived catalysts present lower values for

surface area (59.87 and 74.96 m2 /g, resp.) and pore volume
(0.087 and 0.097 cm3 /g, resp.) related to mussel shell. It can
be seen that the heterogeneous catalyst resulted in a strong
increase in the active sites [15]. This assumption is supported
by the SEM images of catalyst.

90
85
80
75
70
1

4
5
Reaction time (h)

Mussel shell
Cockle shell
Scallop shell

Figure 5: Effect of reaction time on % yield of biodiesel.

reached equilibrium [17] in about 4 h. This can be explained

by that transesterification reaction between oil and alcohol is
reversible, when the reaction time is long enough [18].
In general, the reaction temperature can influence the
reaction rate and yield of biodiesel. The transesterification of
triglyceride (TG) with methanol to methyl ester was carried

100

100

90

90

Yield of biodiesel

Yield of biodiesel

The Scientific World Journal

80

70

70

60

80

60
45

50

55
60
65
Reaction temperature ( C)

70

75

Mussel shell
Cockle shell
Scallop shell

out over the catalysts of CaO at reaction temperature 50

70 C. The % yields of biodiesel after 3 h of reaction time are
shown as a function of temperature in Figure 6. The yields
of biodiesel were obviously rising from 76.85 to 95.90% for
mussel shell, 63.83 to 94.13% for cockle shell, and 70.14 to
95.44% for scallop shell with the increasing temperature from
50 to 65 C. The effect of reaction temperature on promoting
transesterification can be explained due to endothermic
reaction [18]. The highest yield rate was obtained at the
reaction temperature of 65 C. When the reaction temperature
continued to increase over 65 C, the yield of biodiesel was
decreased. The reaction temperature consumedly exceeds the
boiling point of methanol such as 70 C, and the methanol
will quickly vaporize and form a large number of bubbles,
which inhibits the reaction on the two-phase interface [19].
Moreover, in order to save energy, it is necessary to choose the
relative low temperature. Therefore, the optimum reaction
temperature for the transesterification of TG to methyl ester
is considered to be around 65 C.
The excess of methanol is necessary because it can
increase the rate of methanolysis. Normally, stoichiometric
molar ratio of methanol to TG is near 6 : 1 when the alkalicatalyzed process is used. However, it increases to 30 : 1, even
50 : 1, in the acid-catalyzed one to ensure high conversion
[20]. The methyl ester content increased significantly when
the methanol/oil molar ratio was changed from 6 to 18
(Figure 7). The high amount of methanol promoted the
formation of methoxy species on the CaO surface, leading
to a shift in the equilibrium in the forward direction, thus
increasing the rate of conversion up to 95.90, 94.13, and
95.44% for mussel, cockle and scallop shell, respectively.
However, further increases in the methanol/oil molar ratio,
did not promote the reaction. It is understood that the
glycerol would largely dissolve in excessive methanol and
subsequently inhibit the reaction of methanol to the reactants
and catalyst, thus interfering with the separation of glycerin,
which in turn lowers the conversion by shifting the equilibrium in the reverse direction [21]. Therefore, the optimum

9
12
15
Methanol/oil molar ratio

18

21

Mussel shell
Cockle shell
Scallop shell

Figure 7: Effect of methanol/oil molar ratio on % yield of biodiesel.

100
80
Yield of biodiesel

Figure 6: Effect of reaction temperature on % yield of biodiesel.

60
40
20
0
0

10
15
20
Catalyst loading (wt.%)

25

30

Mussel shell
Cockle shell
Scallop shell

Figure 8: Effect of catalyst loading on % yield of biodiesel.

molar ratio of methanol to oil was 9, which is more than

the practical methanol to oil molar ratio for homogeneous
transesterification [22].
Figure 8 reveals the effect of catalyst loading on the
methyl ester formation in the transesterification of palm oil
over waste shell-derived catalyst. In the absence of catalyst,
there was no methyl esters formed in the reaction. Applying
the catalyst amount of 10 wt.%, the highest yields of 95.90,
94.13, and 95.44% were obtained within 3 h for mussel,
cockle and scallop shell, respectively. Reducing the catalyst
loading to 5 wt.% decreased the methyl ester content to ca.
50.9265.45%. This result implies that the transesterification
of TG is strongly dependent on the amount of basic sites [23].
The loadings of 1525 wt.% created catalyst accumulation
on the wall of the glass reactor, possibly contributing to
diffusional problems during reaction and, therefore, lowering
the activity [24]. From this study, we can conclude that the

The Scientific World Journal

Table 3: The fuel properties of biodiesel.

Fuel property

Kinematic viscosity (mm /s) at 40 C

Density (g/cm3 ) at 80 C
Flash point ( C)
Cloud point ( C)
Pour point ( C)
Acid value (mg KOH/g oil)
Water content (%)

Yield of biodiesel

Scallop shell
4.5
0.878
164
11
8
0.55
0.02

4. Conclusions

100
80
60
40
20
0

Derived catalyst
Cockle shell
4.6
0.878
165
12
8
0.67
0.03

Mussel shell
4.4
0.877
164
11
7
0.47
0.02

Number of catalyst reusability

Mussel shell
Cockle shell
Scallop shell

Figure 9: Effect of reusability of catalyst on % yield of biodiesel.

Using cost-effective and environment-friendly catalysts is

particularly useful for the production of biodiesel. The waste
shells are used as the catalyst for this process. This catalyst
contains CaCO3 which is converted to CaO after calcination
at temperatures 1,000 C for 4 h. The optimum conditions,
which yielded a conversion of palm oil of nearly 95% for all
waste shell-derived catalysts, were reaction time 3 h, reaction
temperature 65 C, methanol/oil molar ratio 9, and catalyst
loading 10 wt.% with pressure 1 atm in glass reactor. The
experimental results show that CaO catalyst had excellent
activity and stability during transesterification. The catalyst
was used for 4 cycles and apparent low activity loss was
observed. The fuel properties of the biodiesel so obtained
meet all biodiesel standards. As a solid catalyst, CaO can
decrease the cost of biodiesel and the steps of purification.
It has potential for industrial application in the transesterification of palm oil to methyl ester.

Conflict of Interests
suitable amount of CaO required for the transesterification
of palm oil is 10 wt.%.
The reusability of catalyst is examined by carrying out
reaction cycles. When transesterification reaction finished,
the catalyst is separated from the mixture and used again
without any subsequent treatment in a second reaction
under the same conditions as before. It is found that the
prepared catalyst is active for 3 reaction cycles, with yield
above 90%. After 3 reaction cycles, the biodiesel yield lowers
to 90% (Figure 9). Catalyst deterioration is probably due
to the change of catalyst surface structure. Calcium oxide
is transformed to calcium hydroxide gradually due to the
moisture in the reactants, which deteriorate the activity of
catalyst [25, 26]. However, the activity can be recovered after
calcination in air at 600 C [13].

3.3. Fuel Properties of Methyl Ester. The fuel properties of

methyl ester obtained in this work are summarized in Table 3.
It can be seen that most of its properties are in the range of fuel
properties as described in the latest standards for biodiesel
[27].

The authors declare that there is no conflict of interests

regarding the publication of this paper.

Acknowledgments
The authors acknowledge sincerely the Department of Materials Science and Engineering (MATSE), Faculty of Engineering and Industrial Technology, Silpakorn University,
(SU), and National Center of Excellence for Petroleum,
Petrochemicals, and Advanced Materials (PPAM), Chulalongkorn University (CU) for supporting and encouraging
this investigation.

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Hindawi Publishing Corporation

http://www.hindawi.com

Chemical Engineering
Hindawi Publishing Corporation
http://www.hindawi.com

Volume 2014

Volume 2014

Active and Passive

Electronic Components

Antennas and
Propagation
Hindawi Publishing Corporation
http://www.hindawi.com

Aerospace
Engineering

Hindawi Publishing Corporation

http://www.hindawi.com

Volume 2014

Hindawi Publishing Corporation

http://www.hindawi.com

Volume 2014

Volume 2014

International Journal of

International Journal of

International Journal of

Modelling &
Simulation
in Engineering

Volume 2014

Hindawi Publishing Corporation

http://www.hindawi.com

Volume 2014

Shock and Vibration

Hindawi Publishing Corporation
http://www.hindawi.com

Volume 2014

Advances in

Acoustics and Vibration

Hindawi Publishing Corporation
http://www.hindawi.com

Volume 2014