SURFACE MODIFIED MAGNESIUM OXIDES FOR PRODUCTION OF ...eprints.utm.my/id/eprint/33420/1/NurSyazeilaBintiSamadiMFS2012.pdf · iii Dedicated with much love and affection to my beloved

SURFACE MODIFIED MAGNESIUM OXIDES FOR PRODUCTION OF

BIODIESEL VIA HETEROGENEOUS BASE CATALYST

TRANSESTERIFICATION OF PALM OIL

NUR SYAZEILA BINTI SAMADI

UNIVERSITI TEKNOLOGI MALAYSIA

SURFACE MODIFIED MAGNESIUM OXIDES FOR PRODUCTION OF

BIODIESEL VIA HETEROGENEOUS BASE CATALYST

TRANSESTERIFICATION OF PALM OIL

NUR SYAZEILA BINTI SAMADI

A thesis submitted in fulfilment of the

requirements for the award of the degree of

Master of Science (Chemistry)

Faculty of Science

Universiti Teknologi Malaysia

JANUARY 2012

iii

Dedicated with much love and affection

to my beloved father Samadi Kasmuri and my amazing mother Zainab Ibrahim

and to my helpful brothers, Mohd Syazmil, Mohd Syazli, Mohd Syazaruddin

and someone that never been forgotten Muhammad Syazmi Amir

and a special dedication to my fiancé Megat Husin Yunus

with deep gratitude for all their love in me

Your love would be so much worth to me…

To my supervisor

Prof. Dr. Abdul Rahim Yacob

Thanks for the kindness in giving me an opportunity and encouragement

By trusting me in everything I do…

To my beloved friends

who always support me and always there for me

when I need them

thanks for understand me well…

To all lab assistants, lecturers and my research team,

Special thanks for all your kindness in helping me…

iv

ACKNOWLEDGEMENT

First of all, in a humble way I wish to give all the Praise to Allah, the

Almighty God for giving me the strength and the time to complete this work.

I would like to take this opportunity to express my sincere thanks to my

supervisor Prof. Dr. Abdul Rahim bin Yacob for believing in me. I am also grateful

with his patience, endless efforts in guiding and imparting his vast knowledge to me.

Writing this thesis is a remarkable accomplishment, thanks to the ever constant

advice from my supervisor.

At the same time, I would also to thank all lecturers and lab assistants from

the Department of Chemistry for their help and advice with the handling of the

equipment in the laboratory. And also thanks to my research team mates, Mohd

Khairul Asyraf, Siti Zubaidah, Mohd Raizul, Nurul Aqmar, Norasyikin and Noor

Idayu for helping me to complete this project.

To all my colleagues, thank you for your help and support. I am also grateful

to the Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

for all the facilities and financial support.

Lastly, I would like to acknowledge my family, whose patience love enabled

me to complete this research.

v

PREFACE

This thesis is the result of my work carried out in Department of Chemistry,

Universiti Teknologi Malaysia between December 2008 until December 2010 under

the supervision of Prof. Dr. Abd. Rahim Yacob. Part of my work described in this

thesis has been sent for exhibition participations and reported in the following

publications:

1. Abd. Rahim Yacob, Mohd Khairul Asyraf Amat Mustajab and Nur Syazeila

Samadi. (2008). Surface Modified MgO for Base Catalytic Conversion of

Palm Oil to Biodiesel. Exhibition participation for the Industrial Art and

Technology Exhibition (INATEX) 2008. Bronze medal award. Universiti

Teknologi Malaysia, Skudai, Johor


Samadi. (2008). Surface Modified MgO for Base Catalytic Conversion of

Palm Oil to Biodiesel. Exhibition participation for the Malaysia Technology

Expo (MTE) 2008. Bronze medal award. Putra World Trade Centre. Kuala

Lumpur. 19 – 21 February 2009


Samadi. (2009). Palm Oil Biodiesel: Transesterification of Nano CaO.

Exhibition participation for the Industrial Art and Technology Exhibition

(INATEX) 2009. Silver medal award. Universiti Teknologi Malaysia, Skudai,

Johor

vi


Samadi. (2010). Palm Oil Biodiesel: Transesterification of Nano CaO.

Exhibition participation for the Malaysia Technology Expo (MTE) 2010.

Silver medal award. Putra World Trade Centre. Kuala Lumpur. 4 – 6

February 2009


Samadi. (2009). Calcination Temperature of Nano MgO on Base

Transesterification of Palm Oil. Submitted full paper for International

Conference on Energy and Environment 2009. Singapore. 26 – 28 August

2009

6. Abd. Rahim Yacob, Nur Syazeila Samadi and Mohd Khairul Asyraf Amat

Mustajab. (2010). Activation Temperature Effect on the Basic Strength of

Prepared Aerogel MgO (AP-MgO). Submitted full paperwork for

International Journal of Basic and Applied Sciences IJBAS-IJENS Vol. 10

Issues 02. Pages 118-121.


Samadi. (2010). Physical and Basic Strength of Prepared Nano Structured

MgO. Submitted full paper for 2010 International Conference on Mechanical

and Electrical Technology. Singapore. 10 – 11 September 2010.

8. Abdul Rahim Yacob and Nur Syazeila Samadi. Photosensitization Study of

Triethylamine and Acetophenone in NaY Zeolite Supercages Using ESR.

Poster presentation of Regional Annual Fundamental Science Symposium

2010. Kuala Lumpur. 8-9 June 2010.

9. Abd. Rahim Yacob, Nur Syazeila Samadi and Mohd Khairul Asyraf Amat

Mustajab. (2009). Synthesized Surface Modified Metal Oxide in Base-

Catalytic Transesterification for Biodiesel Production. Poster presentation of

2nd Junior Chemist Colloqioum. Sarawak. 1-2 July 2009.

vii

ABSTRACT

Surface morphology of prepared alkaline earth metal oxide MgO contributes

to the effect of basicity and reactivity in heterogeneous catalysis reactions. In this

study, two methods to prepare surface modified MgO were employed for

comparison. The first method is by conventional (CP-MgO) and the second method

by aerogel (AP-MgO). The methods of preparation will differentiate the effect of

size and morphology towards basicity and reactivity. For conventional method,

commercial magnesium oxide (CM-MgO) was first transformed into its hydroxide,

CP-Mg(OH)2 followed by heat under vacuum at 10-3

mbar. For aerogel method,

magnesium ribbon was transformed into its magnesium hydroxide AP-Mg(OH)2

followed by heat and vacuum as in conventional method. In both methods,

magnesium hydroxides were heated under vacuum at temperatures 100, 200, 300,

400, 500, 600 and 700°C respectively. The surface modified magnesium oxides were

then characterized. Detailed characterization involving Fourier Transform Infra-Red

(FTIR), Thermogravimetry Analysis (TGA), X-Ray Powder Diffraction (XRD),

Nitrogen Gas Adsorption, Field Emission Scanning Electron Microscope (FESEM),

Energy Dispersive X-Ray (EDX) and basicity titration has allowed a rationale

explanation for the high chemical reactivities. In this study, the prepared aerogel AP-

MgO, had a high surface area compared to the conventional CP-MgO. This is

however due to the smaller nano particle size of AP-MgO as compared to CP-MgO.

The main factors of AP-MgO which contributes to the high reactivity are due to the

pore volume and size distribution, unusual surface morphologies, and trace residual

surface of –OH and –OCH3. This will then effect the percentage conversion of

transesterification reaction when compared to CP-MgO. To study the reactivity both

of the best prepared CP-MgO and AP-MgO were used in base heterogeneous catalyst

for transesterification of palm oil to fatty acid methyl ester or also known as

biodiesel. The resulting transesterification reaction of palm oil to biodiesel was then

studied using Gas Chromatography equipped with Flame Ionization Detector (GC-

FID) and the highest percentage conversion of biodiesel of the best catalyst used was

AP-MgO at 700 oC is 94.3%. Further analysis of the biodiesel products was then

characterised using FTIR and Gas Chromatography equipped with Mass

Spectrometry (GC-MS) to determine the components of complex organic mixtures.

viii

ABSTRAK

Morfologi permukaan daripada penyediaan logam oksida alkali bumi MgO

memberi kesan terhadap kebesan dan kereaktifan dalam tindak balas sebagai

pemangkin heterogen. Dalam kajian ini, dua kaedah telah digunakan dalam

penyediaan modifikasi permukaan MgO sebagai perbezaan. Kaedah pertama adalah

menggunakan kaedah konvensional (CP-MgO) dan kaedah kedua menggunakan

aerogel (AP-MgO). Kaedah penyediaan pemangkin ini akan memberi kesan

perbezaan saiz dan morfologi terhadap kebesan dan kereaktifan. Melalui kaedah

konvensional, magnesium oksida komersial (CM-MgO) telah ditindak balaskan

untuk ditukarkan kepada bentuk hidroksida, CP-Mg(OH)2 dan diikuti dengan

pemanasan menggunakan vakum pada 10-3

mbar. Melalui kaedah aerogel pula, pita

magnesium telah diubah kepada magnesium hidroksida, AP-Mg(OH)2 dan kemudian

dipanaskan dan divakumkan seperti kaedah konvensional. Kedua-dua magnesium

hidroksida telah dipanaskan menggunakan vakum pada suhu 100, 200, 300, 400,

500, 600 dan 700°C. Magnesium oksida yang telah diubahsuai ini dilabel dan

dicirikan menggunakan kaedah kimia setiap satunya. Pencirian terperinci melibatkan

Transformasi Fourier Infra Merah (FTIR), Analisis Thermogravimetrik (TGA),

Analisis Pembelauan Sinar-X (XRD), Penjerapan gas Nitrogen, Mikroskop Imbasan

Elektron Emisi Medan (FESEM), Sinar-X Penyebaran Tenaga (EDX) dan kaedah

penitratan bes untuk memberikan penjelasan rasional terhadap kereaktifan kimia

pemangkin. Dalam kajian ini, penyediaan melalui kaedah aerogel AP-MgO

mempunyai luas permukaan yang tinggi berbanding kaedah konvensional CP-MgO.

Ini adalah kerana saiz nano partikel AP-MgO yang kecil berbanding CP-MgO.

Faktor utama AP-MgO yang menyumbang kepada tindak balas yang tinggi adalah

disebabkan isipadu liang, pengagihan saiz, morfologi permukaan yang berubah dan

peninggalan sisa –OH dan –OCH3 ini lantas permukaan yang mempunyai kesan dan

menyebabkan peratusan perolehan pertukaran dalam tindakbalas transesterifikasi

berbanding CP-MgO. Untuk mempelajari kedua-dua reaktiviti sebagai pemangkin

terbaik, CP-MgO dan AP-MgO telah digunakan sebagai pemangkin bes heterogen

untuk tindak balas transesterifikasi minyak kelapa sawit kepada biodiesel. Keputusan

dalam tindak balas transesterifikasi minyak kelapa sawit kepada biodiesel dengan

memilih pemangkin terbaik, kemudian dikaji dengan menggunakan kromatografi gas

yang dilengkapkan dengan Flame Ionization Detector (GC-FID) dan peratusan

pertukaran biodiesel paling tinggi adalah dengan menggunakan AP-MgO yang

dikalsinkan pada suhu 700oC iaitu sebanyak 94.3 %. Analisis mendalam terhadap

produk biodiesel telah dicirikan lagi dengan menggunakan FTIR dan kromatografi

gas yang dilengkapkan dengan Spektrometri Jisim (GC-MS) untuk menentukan

komponen dalam campuran kompleks organik.

ix

TABLE OF CONTENTS

CHAPTER TITLE

PAGE

DECLARATION ii

DEDICATION iii

ACKNOWLEDGEMENTS iv

PREFACE v

ABSTRACT vii

ABSTRAK viii

TABLE OF CONTENTS ix

LIST OF TABLES xiii

LIST OF FIGURES xiv

LIST OF SYMBOLS / ABBREVIATIONS xvi

LIST OF APPENDICES xix

1 INTRODUCTION

1.1 Background of Research 1

1.2 Problem of Statement 2

1.3 Objectives of Research 3

1.4 Significance of Research 3

1.5 Scope of Research 4

2 LITERATURE REVIEW

2.1 Metal Oxide 6

2.2 Magnesium Oxide 7

2.3 Commercial Prepared Magnesium Oxide 8

(CP-MgO)

x

2.4 Aerogel Prepared Magnesium Oxide (AP-MgO) 10

2.5 Palm Oil 11

2.6 Biodiesel 13

2.7 Characterization Technique 19

2.7.1 Fourier Transform Infrared (FTIR) 20

2.7.2 Thermogravimetry Analysis (TGA) 22

2.7.3 Nitrogen Gas Adsorption (NA) 24

2.7.2.1 Adsorption Isotherms 25

2.4.2.3 Surface Area Determination 27

Employing The Brunauer,

Emmett and Teller (BET) Method

2.7.4 X-ray Powder Diffraction (XRD) 29

2.7.5 Field Emission Scanning Electron 33

Microscopy (FESEM)

2.7.6 Energy Dispersive X-Ray (EDX) 34

2.7.7 Gas Chromatography – Flame Ionization 36

Detector (GC-FID)

2.7.8 Gas Chromatography – Mass 38

Spectrometry (GC-MS)

3 EXPERIMENTAL

3.1 Chemical Reagents 39

3.2 Instrumentation 40

3.3 Sample Preparation 40

3.3.1 Preparation of Commercial 41

Prepared Magnesium

Hydroxide, CP-Mg(OH)2.

3.3.2 Preparation of Aerogel Prepared 41

Magnesium Hydroxide,

AP-Mg(OH)2.

3.3.2.1 Preparation of 10% 41

magnesium methoxide

in methanol solution

xi

3.3.2.2 Hydrolysis of magnesium 42

methoxide

3.3.2.3 Autoclave treatment 42

procedure

3.4 Activation 43

3.4.1 Activation using vaccum line 43

system

3.5 Characterization 44



3.5.3 Nitrogen Gas Adsorption 46

3.5.4 X-Ray Diffraction (XRD) 46


Microscope (FESEM)


3.5.7 Basicity Test 48

3.6 Transesterification Reaction 48

3.7 Chromatographic Analysis 49

3.7.1 Gas Chromatography – Flame 49

Ionization Detector (GC-FID)

3.7.2 Gas Chromatography – Mass 50

Spectrometry

4 RESULTS AND DISCUSSIONS

4.1 Introduction 51

4.2 Physical properties of Magnesium Oxide 53

4.3 Characterization Techniques 53



4.3.3 Nitrogen Gas Adsorption 63

4.3.3.1 BET Surface Area 63

4.3.4 X-Ray Diffraction (XRD) 67


Microscope (FESEM)

xii


3.5.7 Basicity Test 81

4.4 Transesterification reaction 84

4.4.1 Fourier Transform Infrared 84

4.4.2 Gas Chromatography 86

4.4.2.1 Gas Chromatography –

Flame Ionization Detector

(FID) 86

4.4.2.2 Gas Chromatography –

Mass Spectrometry 88

5 CONCLUSION AND RECOMMENDATIONS

5.1 Conclusion 90

5.2 Recommendation 93

REFERENCES 94

Appendices A-J 101-135

xiii

LIST OF TABLES

TABLE NO. TITLE PAGE

2.1 Classification of pores according to their width 29

3.1 Chemical reagents used in this study 39

4.1 FTIR peaks assignment 56

4.2 SBET for CM-MgO and prepared surface modified CP-MgO

samples 64

4.3 SBET for prepared surface modified AP-MgO samples 66

4.4 XRD peaks assignment for CM-MgO 68

4.5 XRD peaks assignment for CP-Mg(OH)2 69

4.6 XRD peaks assignment for AP-Mg(OH)2 69

4.7 XRD peaks assignment for CP-MgO at different temperature 71

4.8 XRD peaks assignment for AP-MgO at different temperature 74

4.9 Elemental composition of EDX for CM-MgO, CP-Mg(OH)2,

CP-MgO 500°C and CP-MgO 600°C 79

4.10 Elemental composition of EDX for AP-Mg(OH)2, AP-MgO

500°C and AP-MgO 600°C 81

4.11 The wavelength of absorption peaks for Methyl Ester 86

4.12 Name of fatty acid methyl ester obtained in mass spectrum

by the qualitative value and percentage composition (%) 88

xiv

LIST OF FIGURES

FIGURE NO. TITLE PAGE

1.1 Schematic layout of research scope 5

2.1 Surface model of MgO proposed by Murphy et al. 9

2.2 World production of palm oil by major producing countries 1998

(‘000 tonnes) 13

2.3 Mechanism of transesterification reaction of vegetable oil 16

2.4 Conservative and reversible equations of transestericication

reaction 16

2.5 A schematic diagram of Michelson Interferometer 21

2.6 Shematic diagram of Thermogravimetry Analysis (TGA) 23

2.7 Types of BDDT physisorption isotherm 26

2.8 Simplified X-Ray Diffractometer diagram 30

2.9 Schematic diagram for determining Bragg’s Law 31

2.10 Reflection geometry 32

2.11 Transmission geometry 32

2.12 Elements in an EDX spectrum are identified based on the energy

content of the X-rays emitted by their electrons as these electrons

transfer from a higher-energy shell to a lower energy one 36

2.13 Schematic diagram of gas chromatography 37

3.1 Schematic diagram of rotary pump system 44

4.1 FTIR Spectra of (a) CM-MgO, (b) CP-Mg(OH)2 and

(b) AP-Mg(OH)2 55

4.2 A series of bands due to surface carbonates 56

4.3 FTIR Spectra of CP-MgO after activation under vacuum at

various temperatures (a)100°C, (b)200°C, (c)300°C, (d)400°C,

xv

(e)500°C, (f)600°C and (g)700°C 58

4.4 FTIR Spectra of AP-MgO after activation under vacuum at

various temperatures (a)100°C, (b)200°C, (c)300°C, (d)400°C,

(e)500°C, (f)600°C and (g)700°C 60

4.5 Percentage of weight lost (%) for CM-MgO 61

4.6 Percentage of weight lost (%) for CP-Mg(OH)2 62

4.7 Percentage of weight lost (%) for AP-Mg(OH)2 63

4.8 Specific surface area of CM-MgO and surface modified CP-MgO 65

4.9 Specific surface area of surface modified AP-MgO 67

4.10 XRD diffractogram of (a) CM-MgO, (b) CP-Mg(OH)2 and

(c) AP-Mg(OH)2 70

4.11 XRD diffractogram of (a) CP-MgO 100°C, (b) CP-MgO 200°C,

(c) CP-MgO300°C, (d) CP-MgO 400°C, (e) CP -MgO 500°C,

(f) CP-MgO 600°C, and (g) CP-MgO 700°C 73

4.12 XRD diffractogram of (a)AP-MgO 100°C, (b)AP-MgO 200°C,

(c)AP-MgO 300°C, (d)AP-MgO 400°C, (e)AP-MgO 500°C,

(f)AP-MgO 600°C, and (g)AP-MgO 700°C 76

4.13 FESEM images of CM-MgO 77

4.14 FESEM images of (a) CP-Mg(OH)2 and (b) CP-MgO 700°C 78

4.15 FESEM images of (a) AP-Mg(OH)2 and (b) AP-MgO 700°C 78

4.16 Proposed mechanism in the determination of amount basic site

for nano MgO 81

4.17 Graph amount of basic sites on the surface of CM-MgO,

CP-Mg(OH)2 and CP-MgO at different temperature 82

4.17 Graph amount of basic sites on the surface of AP-Mg(OH)2

and AP-MgO at different temperature 83

4.19 FTIR Spectra of (a) BD CP-MgO and (b) BD AP-MgO 85

4.20 Percentage conversion of biodiesel using CP-MgO 600oC,

CP-MgO 700oC, AP-MgO 600

oC and AP-MgO 700

oC 87

xvi

LIST OF SYMBOLS / ABBREVIATIONS

°C - degree Celsius

�m - micrometer

BET - Brunauer-Emmett-Teller

cm - centimetre

DTA - Differential thermal analysis

EDX - Energy Dispersive X-ray analysis

Eq. - equation

FTIR - Fourier Transformation Infra red

g - gram

K - Kelvin

NA - nitrogen adsorption

mL - millilitre

nm - nanometer

rpm - rotation per minute

TG - Thermogravimetry

XRD - X-ray Diffraction

� - Half angle of diffraction beam

xvii

� - wavelength

MgO - Magnesium Oxide

CM-MgO - Commercial Magnesium Oxide

CP-MgO - Commercial Prepared Magnesium Oxide

AP-MgO - Aerogel Prepared Magnesium Oxide

Mg(OH)2 - Magnesium Hydroxide

CP- Mg(OH)2 - Commercial Prepared Magnesium Hydroxide

AP- Mg(OH)2 - Aerogel Prepared Magnesium Hydroxide

BaO - Barium Oxide

SrO - Strontium Oxide

CaO - Calcium Oxide

% - percentage

FESEM - Field Emission Scanning Electron Microscope

NA - Nitrogen gas Adsorption

GC-FID - Gas Chromatography equipped with Flame

Ionization Detector

GC-MS - Gas Chromatography equipped with Mass

Spectrometry

KBr - Potassium Bromide

FAME - Fatty acid methyl ester

Ni - Nickel

CO2 - Carbon Dioxide

ASTM - American Standard Testing Material

SO2 - Sulfur dioxide

m2/g - milli square per gram

xviii

OH - Hydroxide

IV - Iodine Value

CPO - Crude Palm Oil

CO - Carbon Monoxide

NOx - Nitrogen Oxides

KOH - Potassium Hydroxide

NaOH - Sodium Hydroxide

FFA - Free fatty acid

BDDT - Brunauer, Demming, Demming and Teller

UV - Ultraviolet Radiation

FWHM - full width half maximum

SEM - Scanning Electron Microscope

xix

LIST OF APPENDICES

APPENDIX TITLE PAGE

A Calculation of alcohol needed for the

transesterification reaction 101

B The TGA thermogram of CM-MgO, CP-Mg(OH)2 and

AP-Mg(OH)2 103

C Calculation of amount of basic sites presence in the

samples by using the back titration technique 105

D Calculation of percentage conversion of fatty acid methyl

ester by using the data obtained from GC-FID 106

E The mass spectrum of each fatty acid methyl ester

observed in GC-MS 107

F Submitted proceeding for 2nd Junior Chemist

Colloqioum, 1-2 July 2009, Sarawak. 110

G Submitted paper for International Journal of Basic

and Applied Sciences IJBAS-IJENS Vol:10 No.:02 118

xx

H Submitted paper for International Conference on

Mechanical and Electrical Technology, 10 – 11

September 2010, Singapore. 122

I Submitted proceeding for Regional Annual Fundamental

Science Seminar 2010, 8-9 June 2010, Kuala Lumpur. 126

J Submitted paper for International Conference of

Energy and Environment, 26 - 28 August 2009,

Singapore. 131

CHAPTER 1

INTRODUCTION

1.1 Background of Research

The reactivity of catalyst in some cases are based on the porosity and cavity.

This is true for zeolite. This idea is used to produce catalyst by using other

compound than zeolite. Surface modified metal oxide such as magnesium oxide on

the other hand can be a good catalyst since it has high porosity, simple structure and

high cavity. It can also be used as an adsorbent.

The preparation process of surface modified with higher surface area metal

oxide is easy and economical in cost compared with zeolite and noble catalyst. In this

research, the surface modified magnesium oxide was produced via dehydration

process of commercial magnesium oxide (CP-MgO) and aerogel magnesium oxide

(AP-MgO) method. The aim of this research is to study on the preparation and

characterization of high surface area metal oxide and the reaction as a catalyst.

In this study, the commercial magnesium oxide and magnesium ribbon were

used as the precursor to produce surface modified commercial prepared magnesium

2

oxide (CP-MgO) and aerogel prepared magnesium oxide (AP-MgO) respectively.

Both were activated at different temperature from 100oC till 700

oC respectively. The

research was emphasized on the preparation and characterization of surface modified

MgO and the reaction as a heterogeneous base catalyst for the transesterification

reaction of palm oil to biodiesel.

1.2 Problem of Statement

The reserves of nonrenewable resource such as oil can be considered

economically depleted when 80% of the supply resources have been used and the

remaining 20% is too expensive to extract. According to Puppan (2001), the oil

extinction that its reserves may be 80% depleted within 35-84 years, depending on

how rapidly the oil used. At the current rate of consumption, the oil reserves

predicted will be last for another 44 years. The oil that have not been covered yet is

thought to exist might last around another 20-40 years ahead. Instead of remaining

the amount of oil at the same current level, the global oil consumption is projected to

increase by about 25% by year 2010. This somehow will hasten the gradual depletion

of oil reserve.

The gradual depletion of petroleum reserves gives big influence interest in

finding alternative source of energy. Furthermore, world oil demand driven by

economic development, posted the highest growth rate in recent years and the high

price of oil also created desire to find renewable and sustainable alternative energy to

decrease dependences in petroleum.

The last few decades, a substantial amount of research have been conducted

in order to find a new renewable and sustainable energy source to substitute the

usage of petrol fuel. A researchers Marchetti et al. (2007) concluded that there is one

3

promosing renewable source of energy that can substitute the nonrenewable energy

that is biodiesel.

Currently, biodiesel which also known as fatty acid methyl ester (FAME) is

commonly produced by performing a transesterification reaction of renewable lipid

feedstock such as animal fat or vegetable oil with homogeneous base catalysts such

as KOH or NaOH dissolved in methanol. However, the produced FAME needs to

undergo purification process to remove impurities such as base catalyst and glycerine

by using a water washing process and this somehow will requires the disposal of a

large amount of basic water.

1.3 Objectives of Research

The objectives of this research are to prepare Surface Modified Commercial

Prepared MgO (CP-MgO) and Surface Modified Aerogel Prepared MgO (AP-MgO)

which varies in temperature from 100°C-700°C respectively and characterize all the

prepared magnesium oxide. Secondly, to investigate the prepared magnesium oxide

catalytic capabilities as a solid base catalyst in the transesterification of palm oil for

biodiesel production.

1.4 Significance of Research

This research has several importances to the as the substitution of the

petroleum based oil such as:

4

1) To substitute petrol fuel which is nonrenewable source of energy with

renewable resources such as vegetable oil

2) To enhances the usage of magnesium oxide base catalyst for other

applications.

3) To reduced the green house gases effect of production of waste water

and reduce global warming phenomenon.

4) To develop a new alternative energy sources other than petroleum

resources from fuel.

1.5 Scope of Research

The scope of the research is to prepare and characterize seven types of

surface modified MgO (CP-MgO and AP-MgO) which differs in temperature of

activation. The prepared surface modified MgO was prepared at various

temperatures; 100°C, 200°C, 300°C, 400°C, 500°C, 600°C and 700°C respectively.

Resulting CP-MgO and AP-MgO samples were characterized using spectroscopy

instrument which include Fourier Transform Infra-Red (FTIR). To have better

understanding on the surface and morphological properties, Nitrogen Gas Adsorption

(NA) and Field Emission Scanning Electron Microscopes (FESEM), Energy

Dispersive X-Ray (EDX) X-Ray Diffractometer (XRD) and Thermogravimetry

Analysis were used. For determination of bacisity of magnesium oxide, basicity

titration was used. In reaction as a catalyst for transesterification of palm oil to

biodiesel, samples were analyzed using Fourier Transform Infrared (FTIR), Gas

Chromatography equipped with Flame Ionization Detector (GC-FID) and Gas

Chromatography – Mass Spectrometry (GC-MS). Figure 1.1 shows the schematic

layout of the research scope.

5

Figure 1.1 Schematic Layout of Research Scope

FTIR

GC-FID

GC-MS

Sample Preparation

CP-Mg(OH)2

Surface Modified MgO

Surface and

Morphology

Study

Reaction as a

catalyst for

transesterification

Spectroscopy

Study

TGA

NA

XRD

FESEM

EDX

FTIR

AP-Mg(OH)2

Basicity

Study

Basic Titration

94

REFERENCES

Abdullah, A.Z., Salamatinia, B., Mootabadi, H., Razali, N. and Bhatia, S. (2008).

Proposed Biodiesel Production and Development Policy in Malaysia.

International Conference on Environmental Research and Technology

(ICERT 2008).

Alan, G.S. (1981). Inorganic Chemistry. Longman Group Limited.

Ali, R., Garif, M.N., Shamsuddin, M., Ali, R., Ramli, Z. (2002). Kimia Unsur

Kumpulan Utama. Universiti Teknologi Malaysia. Johor.

Alvarado, E., Torres-Martinez, L.M., Fuentes, A.F, and Quintana, P. (2000).

Preparation and characterization of MgO powders obtained from

different magnesium salts and the mineral dolomite. Polyhedron. 19.

22-23.

Aramendia, M.A., Borau, V., Jimenez, C., Marinas, J. M., Ruiz, J.R. and Urbano,

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