ABSTRACT
In this work, Transesterification of waste vegetable oil has been carried out using Anthill as the
catalyst. Anthill was utilized as raw material for catalyst production for biodiesel preparation.
During calcination process, the calcium carbonate content in the anthill was converted to CaO with
Al₂O₃ as the promoter and SiO₂ as the support. This calcium oxide was used as catalyst for
transesterification reaction between waste cooking oil and methanol to produce biodiesel. The
biodiesel preparation was conducted under the following conditions: the mole ratio between
methanol and palm oil was 6:1 and with catalyst of 7wt %. The catalyst activation temperature,
reaction temperature and reaction time was varied at 600-1000°C, 60-70°C and 1-3h respectively.
The maximum yield of biodiesel was 63.14%, obtained at 3h of reaction time and 70°C. Anthill
has potential application as a source of catalyst for synthesis of biodiesel of high purity. The
catalyst was obtained by calcinations of anthill at 600-1000°C for 3h. The maximum yield of
biodiesel produced by transesterification of waste cooking oil with methanol was 63.14%. The
operating condition to achieve the maximum biodiesel yield is: the ratio of oil to methanol 1:6, the
amount of catalyst 7%, reaction time 3h, reaction temperature 70°C.
vi
TABLE OF CONTENTS
CERTIFICATION ………………………………………………………………………………………………………….. ii
DEDICATION……………………………………………………………………………………………………………….iii
ACKNOWLEDGEMENT………………………………………………………………………………………………. iv
ABSTRACT…………………………………………………………………………………………………………………… v
LIST OF FIGURES ……………………………………………………………………………………………………… viii
LIST OF TABLES………………………………………………………………………………………………………….. x
NOMENCLATURE ………………………………………………………………………………………………………. xi
CHAPTER ONE…………………………………………………………………………………………………………….. 1
1.0 INTRODUCTION …………………………………………………………………………………………………….. 1
1.1 Research Background ………………………………………………………………………………………….. 1
1.2 Problem Statement………………………………………………………………………………………………. 3
1.3 Aim…………………………………………………………………………………………………………………… 3
1.4 Objectives………………………………………………………………………………………………………….. 3
1.5 Scope of Study……………………………………………………………………………………………………. 4
1.6 Motivation/Significance of Study………………………………………………………………………….. 4
1.7 Justification………………………………………………………………………………………………………… 4
CHAPTER TWO ……………………………………………………………………………………………………………. 5
2.0 THEORECTICAL BACKGROUND ……………………………………………………………………….. 5
2.1 Biodiesel ……………………………………………………………………………………………………….. 5
2.2 Catalyst ……………………………………………………………………………………………………………. 10
2.4. Vegetable Oil for Transesterification ………………………………………………………………….. 13
2.6. Characterization Methods for Catalyst and Biodiesel ……………………………………………. 15
2.7. Past Work On Biodiesel Production with Catalyst Gotten From Natural Sources …….. 19
CHAPTER 3 ………………………………………………………………………………………………………………… 23
3.0 METHODOLOGY……………………………………………………………………………………………….. 23
3.1 MATERIALS AND EQUIPMENT……………………………………………………………………… 23
3.2 Catalyst Preparation…………………………………………………………………………………………… 24
3.3 Waste Cooking Oil ……………………………………………………………………………………………. 25
3.4 Biodiesel Production………………………………………………………………………………………….. 28
CHAPTER 4 ………………………………………………………………………………………………………………… 30
4.0 RESULTS AND DISCUSSION …………………………………………………………………………….. 30
vii
4.1 Oil Analysis…………………………………………………………………………………………………. 30
4.2 Oil Characterization………………………………………………………………………………………. 30
CHAPTER 5 ………………………………………………………………………………………………………………… 38
5.0 CONCLUSION AND RECOMMENDATION………………………………………………………… 38
5.1 Conclusion…………………………………………………………………………………………………………… 38
5.2 Recommendation………………………………………………………………………………………………….. 38
REFERENCE……………………………………………………………………………………………………………….. 39
APPENDIX………………………………………………………………………………………………………………….. 42
viii
LIST OF FIGURES
Figure 1.1. Transesterification reaction……………………………………………………………2
Figure 2.1. Overall mechanism of Transesterification……………………………………………..6
Figure 2.2. Structure of Vegetable Oil……………………………………………………………14
Figure 2.3. Block diagram of an FTIR spectrometer………………………………………………….19
Figure 3.1. Process for catalyst preparation………………………………………………………26
Figure 3.2. The sieved oil…………………………………………………………………………26
Figure 3.3. pH meter………………………………………………………………………………27
Figure 3.4. Atmospheric mud balance…………………………………………………………….27
Figure 3.5. Marsh funnel………………………………………………………………………….28
Figure 3.6. Process of biodiesel production………………………………………………………29
Figure 3.7. Synthesized biodiesel before separation…………………..…………………………30
Figure 4.1. SEM of raw anthill……………………………………………………….…………..32
Figure 4.2. SEM AT 800 °C…….………………………………………………………………..33
Figure 4.3. SEM AT 1000 °C….…………………………………………………………………33
Figure 4.4. Biodiesel yield against catalyst activation temperature……..………………………..34
Figure 4.5. Biodiesel yield with time……………………………………………………………..35
Figure 4.6. Biodiesel yield with temperature……………………………………………………..35
ix
Figure 4.7. Waste cooking oil FTIR spectrum……………………………………………………36
Figure 4.8. Waste cooking oil derived biodiesel at 800°C……………………………………………36
Figure 4.9. GCMS data…………………………………………………………………………..37
Figure 4.10. GCMS with data band matching number…………………………………………..37
x
LIST OF TABLES
Table 2.1. Properties of biodiesel compared to diesel……………………………………………10
Table 2.2. Comparison of homogenous and heterogeneously catalyzed transesterification..……12
Table 2.3. Compositional analysis of ant-hill clay…………………………………………………13
Table 4.1. Oil analysis result………..…………………………………….…………………………31
Table 4.2. Composition of anthill…………………………………………………………………31
Table 4.3. Fatty acid contents of each oil represent the composition of methyl esters in
biodiesel………………………………………………………………………………………….38
xi
NOMENCLATURE
FAME Fatty Acid Methyl Ester
SEM Scanning Electron Microscope
FTIR Fourier Transform Infrared
FFA Free Fatty Acid
XRF X-Ray Fluorescence
GC-MS Gas Chromatograhy-Mass Spectrometry
A/D Analog to Digital
XRD X-Ray Diffraction
1
CHAPTER ONE
1.0 INTRODUCTION
1.1 Research Background
Currently there is an urgent need to develop alternative energy resources, such as biodiesel fuel
due to the gradual reduction of world petroleum reserves, its economic and social concerns and
the environmental pollution of increasing exhaust emissions of harmful gases like SOx, NOx, and
Cox, coupled with the steady increase in energy consumption have spurred research interest in
alternative and renewable energy sources. A successful substitute for diesel fuel, used mainly in
the transportation sector, was found to be the mixture of the ester derivatives from the vegetable
oils and animal fats. This new feedstock is environmental friendly, renewable, and totally independent from petroleum
Biodiesel is a renewable, biodegradable fuel that can be manufactured domestically from vegetable
oils, animal fats, or recycled restaurant grease. It is a cleaner-burning replacement for petroleum
diesel fuel. Biodiesel is defined as the mono-alkyl esters of vegetable oils or animal fats, obtained
by transesterification of oils or fats with an alcohol, usually methanol or ethanol. The major
component of vegetable oil is triglycerides. When the triglycerides react with alcohol in the
presence of base catalyst, this is called “transesterification.” In this reaction, triglycerides are
converted to diglyceride, monoglyceride, and finally converted to glycerol. The reaction occurs in
three steps. In the first step, a triglyceride reacts with an alcohol molecule producing a diglyceride
–ester and then the diglyceride reacts with another alcohol molecule producing a mono-glyceride
and another mono-ester, and finally, the mono- glyceride reacts with another alcohol molecule
giving glycerin and another mono-ester. (Vonortas and Pappayanakos, 2014)
2
Figure 1.1. Transesterification reaction
The parameters affecting the transesterification reaction are temperature, molar ratio of alcohol to
oil, type and quantity of catalyst, the type of the process, and the composition of the reactants
mixture.
Catalyst is any substance that increases the rate of a chemical reaction. Catalyst are not consumed
during a reaction therefore it is possible to recycle them. The process for producing biodiesel use
different catalyst
i. Homogenous (NaOH, KOH, H2SO4)
ii. Biocatalyst (lipases)
iii. Heterogeneous (metal hydroxides, metal complexes and metal oxides like calcium oxide,
magnesium oxide, zeolites etc.)
Homogenous catalyst is a catalyst that is in the same phase with the reactant while heterogeneous
catalyst means that the catalyst are in different phase with the reactant. Biocatalyst are known as
the enzyme catalyst.
It has been estimated that the cost of biodiesel produced from virgin vegetable oil through
transesterification is higher than that of fossil fuel, because of high raw material cost. This has
3
hindered wider utilization and commercialization of future biodiesel plant. To minimize the biofuel
cost, in recent days, cheaper feedstock such as low-grade oil, typically waste cooking oil is being
used as feedstock. The high viscosity and poor volatility are the major limitation of using vegetable
oil in diesel engines. (Paugazhabadivu et al., 2005). Large amount of waste cooking oil is
generated from eatery establishment, restaurant and food industry etc. every year, discarding of
this oil can be of a challenge since it has the probability of contaminating the environment. (Hubera
et al., 2007). Accordingly, this research work will focus on biodiesel production from waste
cooking oil using thermally activated anthill.
1.2 Problem Statement
Homogenous catalyst result in complex separation and purification process steps due to its high
saponification. Catalyst gotten from anthill has never been recorded to be used in biodiesel
production based on the previous research. The competition of using edible vegetable oil in the
production of biodiesel in place of food stock has made it a wrong choice for biodiesel production.
Waste vegetable oil poses an environmental concern in the disposal. Depletion of petroleum
reserves makes dependence on it as the only source of energy a problem.
1.3 Aim
This research project is aimed at the investigation of anthill as a suitable catalyst for the production
of biodiesel by transesterification.
1.4 Objectives
Preparing the anthill catalyst at varied activation temperature.
Varying the time during biodiesel production
Varying the temperature and time of the reaction
4
1.5 Scope of Study
The scope of my study covers the production of biodiesel using anthill as catalyst. Various samples
of the anthill catalyst at various activation temperature will be tested during the biodiesel
production while varying the methanol to oil ratio, temperature and time of reaction to find out the
optimum conditions for the best conversion of the biodiesel.
1.6 Motivation/Significance of Study
In most of hotels, restaurants, and in other food industries, the waste cooking oil is either simply
discharged into the river or dumped into the land, In spite of this, the waste cooking oil can be
used effectively for the biodiesel synthesis. Biodiesel production from waste cooking oil is found
to be economically feasible method. This research is proposed to improve the capability of waste
cooking oil as a biodiesel feedstock in the present worldwide due to the increasing demand of
biodiesel, the environmental concern and limited resources of petroleum oil. Many researches
before use waste cooking oil to produce but none has used anthill as a catalyst for the biodiesel
production. Hence, this research is to investigate if using anthill as a catalyst will give a good yield
and the parameter suitable for the yield.
Biodiesel have so many advantages such as, is a renewable energy sources, safe for use in all
conventional diesel engines, offers the same performance and engine durability as petroleum diesel
fuel, non-flammable and nontoxic, reduces tailpipe emissions, visible smoke and noxious fumes
and odors. So, waste cooking oil is used as a raw material to substitutes the petroleum because
it provides a safer means of disposing of the oil.
1.7 Justification
Availability of anthill across the nation and abundant quantity of waste cooking oil
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