ABSTRACT
The production of biodiesel from waste vegetable oil using eggshell based catalyst was studied.
Eggshell was investigated to utilize the composition of calcium carbonate as a heterogeneous
catalyst for biodiesel production. The objective of the experiment is to utilize the calcium
carbonate obtained from the calcination-hydration-dehydration method of the eggshell waste as
solid catalyst for biodiesel production from waste vegetable oil by the variation of temperature,
catalyst weight and reaction time. Catalyst form the waste raw eggshell was prepared by firstly,
washing the eggshell to remove impurities, it was dried in hot air oven at 120 0C under static
condition for 6hrs. Calcination was carried out at 900 0C for 3hr, after which it was washed, dried
and recalcined at 600 0C for 3hr. Waste vegetable oil was filtered in order to remove impurities
and food bits, after which qualitative analysis was carried out to determine the physiochemical
properties such as viscosity, pH, free fatty acid and density. Transesterification reaction was
performed by methanol to oil ratio of 6:1 and varying reaction temperature (60 °C, 65 °C, and 70
°C), reaction time (1hr, 2hr, and 3hr), catalyst weight (1%wt, 3%wt, 5%wt, 7%wt, 9%wt). The
highest biodiesel yield was found to be 76.889% by using methanol oil ratio of 6:1, temperature
of 60 0C reaction time for 2 hr.
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CONTENTS
PAGE
TITLE PAGE……………………………………………………………………………….i
CERTIFICATION…………………………………………………………………………ii
ABSTRACT……………………………………………………………………………….iii
ACKNOWLEGDEMENT…………………………………………………………………iv
DEDICATION……………………………………………………………………………..v
CONTENT ………………………………………………………………………………..vi
LIST OF FIGURES………………………………………………………………………..ix
LIST OF TABLES …………………………………………………………………………x
CHAPTER ONE …………………………………………………………………………..1
1.0 INTRODUCTION………………………………………………………………………1
1.1 Background……………………………………………………………………………. 1
1.2 Project statement………………………………………………………………………..2
1.3 Objectives ……………………………………………………………………………….2
1.4 Justification of study…………………………………………………………………….3
1.5 Scope of study……………………………………………………………………………4
CHAPTER TWO……………………………………………………………………………5
2.0 THEORETICAL BACKGROUND ……………………………………………………5
2.1 Biodiesel…………………………………………………………………………………5
2.1.1 Economic Advantages of Biodiesel…………………………………………..6
2.2 Transesterification Process………………………………………………………………8
2.2.1 Catalysts in Transesterification Process……………………………………….8
2.2.2 Homogeneous Catalyst………………………………………………………..9
2.2.3 Heterogeneous Catalyst………………………………………………………..9
2.2.4 Eggshell as Heterogeneous Catalyst…………………………………………..10
2.3 Feedstock for Biodiesel Production……………………………………………………..12
vii
2.3.1 Vegetable Oils and Animal Fats………………………………………………13
2.3.2 Waste Cooking Oil……………………………………………………………13
2.3.1 Alcohol………………………………………………………………………..14
2.4 Variables Affecting the Transesterification Process…………………………………….15
2.4.1 Moisture and Free Fatty Acids Contents………………………………………15
2.4.2 Molar Ratio of Alcohol to Oil and Type of Alcohol ………………………….15
2.4.3 Type and Amount of Catalyst…………………………………………………16
2.5 Characterization of FAME………………………………………………………………16
2.5.1 Fourier Transform Infrared spectrophotometer ……………………………….16
2.5.2 Gas Chromatograph Mass Spectrometry………………………………………17
2.5.3 X-Ray fluorescence…………………………………………………………….17
2.5.4 Scanning Electron Microscope…………………………………………………17
CHAPTER THREE…………………………………………………………………………18
3.0 MATERIALS AND METHODOLOGY………………………………………………..18
3.1 Materials and Reagents………………………………………………………………….18
3.2 Equipment used………………………………………………………………………….18
3.3 Waste Vegetable Oil Treatment………………………………………………………….18
3.4 Catalyst Preparation……………………………………………………………………..19
3.5 Catalyst Characterization…………………………………………………………………20
3.6 Transesterification of Waste Vegetable Oil………………………………………………21
3.7 Characterization of Waste Vegetable Oil and Methyl Ester…………………………….22
CHAPTER FOUR…………………………………………………………………………..23
4.0 RESULT and DISCUSSION……………………………………………………………23
4.1 Waste Vegetable Oil Characterization…………………………………………………..23
4.2 Catalyst Characterization………………………………………………………………..23
4.2.1 X-Ray Fluorescence Analysis………………………………………………….23
4.2.2 Scanning Electron Microscope Analysis………………………………………24
4.3 Fame Characterization…………………………………………………………………..26
viii
4.3.1 Fourier Transform Infra-Red Spectrophotometer Analysis……………………26
4.3.2 Gas Chromatograph Mass Spectrometer Analysis…………………………….28
4.4 Determination of Biodiesel Yield………………………………………………………30
4.4.1 Effect of Catalyst Concentration on Biodiesel Yield…………………………30
4.4.2 Effect of Temperature on Biodiesel Yield…………………………………….31
4.4.3 Effect of Reaction Time on Biodiesel Yield………………………………….32
CHAPTER FIVE……………………………………………………………………………33
5.0 CONCLUSION…………………………………………………………………………33
REFERENCES……………………………………………………………………………..34
ix
LIST OF FIGURES
FIGURE PAGE
2.1 Transesterifications reaction of triglyceride…………………………………8
3.1 Waste vegetable oil sample………………………………………………..19
3.2 Raw eggshell preparation to catalyst………………………………………..20
3.3 Produced biodiesel………………………………………………………….21
4.1 SEM image of raw egg……………………………………………………..24
4.2 Calcined eggshell at 900 0C for 3hr………………………………………..25
4.3 Eggshell washed and re-calcined at 600 0C for 3hr…………………………25
4.4 FTIR Analysis of Waste Vegetable Oil…………………………………….27
4.5 FTIR Analysis of FAME at 5 wt. % catalyst……………………………….27
4.6 GC – MS with data band matching number……………………………….29
4.7 GC – MS image without data band matching number…………………….29
4.8 A Graph of Yield vs Catalyst weight………………………………………31
4.9 A Graph of yield vs Reaction Temperature………………………………..31
4.10 A Graph of Yield vs Time of Reaction…………………………………….32
x
LIST OF TABLES
TABLE PAGE
2.1 Comparison of the Standards for Diesel and Biodiesel Based On (ASTM)……………6
2.2 Different Heterogeneous Catalysts Used For Transesterification of Vegetable Oils…….11
2.3 Comparison of Homogeneous and Heterogeneously Catalyzed Transesterification…….12
2.4 Main Production Facilities of Methanol and Ethanol…………………………………….15
4.1 Physiochemical Properties of Waste Vegetable Oil………………………………………23
4.2 XFR Analysis of Raw eggshell in weight percentage…………………………………….24
4.3 GC – MS breakdown of methyl esters into their various components…………………..28
4.4 Biodiesel yield at varied parameters………………………………………………………30
1
CHAPTER ONE
1.0 INTRODUCTION
1.1 Background
Biodiesel has tremendously gained popularity because it is a renewable and environmentally
friendly fuel. It is a major key component in the motor diesel engines today because of their
attractive features. It represents a largely closed carbon dioxide cycle (approximately 78%), as it
is derived from renewable biomass sources. Compared to petroleum diesel, biodiesel has lower
emission of pollutants, it is biodegradable and enhances the engine lubricity (Kurki et al., 2006).
Biodiesel has a higher cetane number than diesel fuel, no aromatics, no sulfur, and contains 10–
11% oxygen by weight (Canakci, 2007). It can be easily synthesized through transesterification of
oil or esterification of fats using basic or acidic catalysts with heating functions (Khemthong et al.,
2012).
Chemically, biodiesel is a mixture of methyl esters with long-chain fatty acids and is typically
made from transesterification reaction of biological triglyceride sources such as vegetable oil with
alcohol in the presence of catalyst such as sodium hydroxide, sodium methoxide, potassium
hydroxide, and potassium methoxide (Meher et al., 2006). The major reason that vegetable oils is
transesterified to methyl esters (biodiesel) is that the kinematic viscosity of the biodiesel is much
closer to that of petro-diesel. The high viscosity of untransesterified oils and fats leads to
operational problems in the diesel engine such as deposits on various engine parts.
Numerous feedstock have been experimented for biodiesel production. Though oil straight from
the agricultural industry represents the greatest potential source, it is not being produced
2
commercially simply because the oil is too expensive. After the cost of converting it to biodiesel
has been added it, it will be too expensive to compete with fossil diesel.
Subsequently, this work intends to investigate the transesterification of triglycerides, using waste
vegetable oil and raw eggshell as cost effective and eco-friendly catalyst.
1.2 Problem Statement
Commercial production technology of biodiesel via homogenous transesterification has a lot
limitation, making the cost of biodiesel production economically unfeasible.
Waste eggshell-environmental nuisance, medium for growth of microorganism, aside odor.
Waste vegetable oil constitutes an environmental concern
1.3 Research Aim and Objectives
1.3.1 Aim
The aim of this project is to produce a solid catalyst from waste eggshell that can be used as
catalyst in the transesterification of waste frying oil to biodiesel.
1.3.2 Objectives
• To synthesize and characterize catalyst from waste eggshell
• To study the feasibility of waste vegetable oil as alternative feedstock in the
transesterification process.
• To characterize the product from the transesterification process (FAME)
3
• To study and optimize the transesterification of waste vegetable oil using eggshell based
catalyst under a range of operating parameters (reaction temperature, reaction time, ratio
of oil/methanol and amount of catalyst)
1.4 Justification of Study
The increase in pollutants emissions from the use of petroleum fuel affects human health as well
as the environments. Both the energy needs and increased environmental consciousness have
stimulated the researching of an alternative fuel. Also, the recent research developments in the
exploitation of biodiesel especially in Nigeria and the rest of Africa provides a reliable platform
for adoption of biodiesel as an alternative energy source. The following could be key reasons to
adopt and promote biodiesel production and research;
(i) It reduces the country’s dependence on imported petroleum.
(ii) It is renewable and contributes less to global warming than petroleum fuel due to its
closed carbon cycle. The primary feedstock is cheap and readily available such as used
cooking oil and non-edible oil.
(iii) It provides good engine performance and can be used without engine modification.
(iv) It provides a market for excess production of vegetable oils and animal fats, thus
enhancing the rural economies.
(v) it is biodegradable and non-toxic
(vi) It exhibits lower combustion profile, especially Sulphur
(vii) Ready Market for Biodiesel especially in Nigeria
4
1.5 Scope of Study
To achieve the objective of this research, the listed scopes have been identified
1. Preparation of activated egg shell as a solid catalyst.
2. Production of biodiesel from waste vegetable oil using activated egg shell as a catalyst in batch
system.
3. Optimizing the selected parameter for biodiesel production (temperature, catalyst weight and
reaction time).
4. Identifying the effect of the temperature, reaction time, and catalyst weight on biodiesel yield.
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