COMPARATIVE STUDIES ON REFINING OF PALM OIL USING NIGERIAN CLAYS

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COMPARATIVE STUDIES ON REFINING OF PALM OIL USING NIGERIAN CLAYS SALA WUDEEN TAOFEEK OLALEKAN M.ENG/SEET/20011725 DEPARTMENT OF CHEMICAL ENGINEERING, FEDERAL UNIVERSITY OF TECHNOLOGY, MINNA NIGERIA AUGUST, 2005

COMPARATIVE STUDIES ON REFINING OF PALM OIL USING NIGERIAN CLAYS - SALA WUDEEN TAOFEEK OLALEKAN M.ENG/SEET /20011725 A PROJECT SUBMITTED TO THE POSTGRADUATE SCHOOL, FEDERAL UNIVERSITY OF TECHNOLOGY, MINNA IN PARTIAL FULFILLMENT OF THE AWARD OF MASTER OF ENGINEERING (M.ENG.) IN CHEMICAL ENGINEERING AUGUST, 2005 II

DECLARATION I, Salawudeen Taofeek Olalekan (M.ENG/SEET/2001l725) declare that this thesis: Comparative Studies on Refining of Palm Oil Using Nigerian Clays presented for the award of Masters of Engineering has not been presented for any other degree elsewhere. fu. -At-...... ~?. /~ Signature Date iii

CERTIFICATION This thesis titled "Comparative Studies on Refining of Palm Oil Using Nigerian Clays" Salawudeen Taofeeq Olalekan meet the regulations governing the degree of (M.Eng) of Federal University of Technology, Minna and is approved for its contribution to scientific knowledge and literal presentation.. ~.~.. Dr. F. Aberuagba Date (Project Supervisor) Dr. F. Aberuagba Date (Head of Department) External Examiner Date... ~ Prof. F.O Akinbode (Dean S.E.E.T) Date Prof. J.A. Abalaka (Dean Post -Graduate School) Date IV

DEDICATION This project is dedicated to the memory of my late mother Alhaja Alimotu Salawudeen (Ajiboye). May her gentle soul rest in perfect peace. v

ACKNOWLEDGEMENT My sincere appreciation goes to Almighty God for the successful completion of this programme. I wish to express my profound gratitude to my supervisor, HOD, Dr. F. Aberaugba, for his invaluable suggestions and corrections that facilitated a lot of improvement on this project. I wish to express my appreciation to my lecturers: Dr. K.R. Onifade, Dr. lo. Odigure, Dr. D. Aloko, Dr. M.O. Edoga, Engr. A.S. Abdulkareem, Engr. O.D. Adeniyi, Engr. M.A. Olutoye, Engr. U.G. Akpan, Engr. (Mrs) EJ. Eterigho and all other members of the department. I would like to thank my beloved brother Engr. F.B. Akande and Mal. K.A. Akande for their substantial care during the course of the programme. My appreciations go to my friends and neighbors most especially Engr. E.O. Dada and Afolabi Eyitayo (SIR TEE) for going through the manuscript. My sincere gratitude goes to Mrs. Oyeronke Ola Ajiboye for her understanding during the programme. Finally my appreciation goes to the members of the family for their moral and financial support. They are Dr & Mrs F.O. Ajiboye, Mr. & Mrs 0.0. Ajiboye. Miss Abiola Idowu, Mr. & Mrs Idowu and my beloved father Pa Salawudeen Oyemomilara Ajihoye and the rest of the family. vi

ABSTRACT This project work evaluated the bleaching power of some selected clays found in I Nigeria with the aim of developing substitute bleaching agents for the palm oil refining industries. Five clay samples were collected from different localities in Oyo and Osun States. The physiochemical properties of the clays were determined by both physical and chemical analysis, and their performances in bleaching palm oil were assessed before and after activation with varying concentration of I-hS04 and HC!. A percentage colour reduction of 74% was achieved with HCI activated clay and 67% with H2S04 activated clay at 100 C with 5% dose of the adsorbent in 10 minutes. The result compared favorably with imported bleaching earth (Bentonite). When the bleached oil was deodorized, the percentage colour reduction of the best activated clay increased to 87% and this compared favorably with commercial refined palm oil with all the properties falling within the recommended standards. When these results were statistically analyzed, variation existed and the analysis of the variance showed that at 95 % confidence limit, clay sample 5 (CaO- O.02±O.OO%, MgO- O.30±O.OO%, Fe20)- 2.52±O.Ol %, AlzO)- 5.l8±O.03%, Si02-91.29±O.OI %) ranked the most effective followed by sample 1 (MgO O.03±O.Ol, Fe20)- 3.30±O.OO%, AIzO)- 5.22±O.OO%, Si02-90.36±O.Ol %) and sample 2 ( MgO- O.02±O.OO%, Fe20)- 3.13±O.Ol%, AIzO)-6.22±O.Ol%, Si02-90.09±O.Ol%) while clay samples 3 (MgO- O.06±O.Ol %, Fe203-3.12±O.Ol %, AlzO)- 8.04±O.03%, Si02-88.22±O.03%) and 4 (MgO-O.Ol±O.OO%, Fe203-10.80±O.Ol%, AlzO)-6.51±O.Ol%, Si02-81.89±O.O 1 %) were less effective. These results agreed with those obtained when the experimental results were subjected to Freudlich Adsorption Isotherm. Vll

TABLE OF CONTENTS Cover Page Title page Declaration Certification Dedication Acknowledgement Abstract Table of Contents List of figures List of Tables Notation, Symbols and Abbreviations CHAPTER ONE 1.1 Introduction 1 1.2 Aims and Objectives 2 1.3 Scope of Project Work 3 1.4 Significance of Project Work 3 CHAPTER TWO 2.0 Literature Review 4 2.1,History of Palm Oil 4 2.2 The Oil Palm Fruit and Crude Palm Oil 4 2.3 World Palm Oil Producers 5 2.4 Component of Palm Oil 6 2.5 Palm Refining and Downstream Processing 7 2.6 Uses of Palm Oil 10 2.7 Preservation of Palm Oil (Hydrogenation) 11 2.8 Factors Used in Determining the Quality of the Vegetable Oil 12 2.9 Environmental Impact Assessment on Vegetable Oil Base Industry 14 2.10 Clay and Clay Minerals 14 2.11 Definition of Clay 15 2.12 How and Where Clay Deposit Form 15 u III IV v VI vu Vlll Xl XU XIV Vlll

2.13 Uses and Types of Clay 17 2.14 Physical and Chemical Properties of Clay 18 2.15 Clay Mineralogy 20 2.16 Clay Mining and Processing 22 2.17 Theory and Principle of Adsorption in Clay 23 CHAPTER THREE 3.0 Experimental Method 24 3.1 Equipment/Instruments 24 3.2 Materials 24 3.3 Methodology 24 3.3.1 Clay Characterization 24 3.4 Clay Preparation 26 3.5 Crude Palm Oil Refining 27 3.5.1 Determination of Optimum Concentration of NaOH for Neutralization of the Crude Palm Oil 27 3.5.2. Degumming 28 3.5.3. Neutralization 28 3.5.4. Adsorption Bleaching 28 3.5.5 Adsorption Isotherms 29 3.5.6 Deodorization 29 3.6 Crude and Refined Palm Oil Analysis 30 3.6.1 Colour and Percentage Colour Reduction 30 3.6.2 Determination of Acid Value (Indicator Method) 30 3.6.3. Determination of Percentage Free Fatty Acid (FFA) 31 3.6.4 Determination of Saponification Value (S.V) 31 3.6.5 Determination of Ester Value (E.V) 32 3.6.6 Determination of Iodine Value (LV) 32 3.6.7 Determination Peroxide Value 33 CHAPTER FOUR 4.1 Results 34 4.2 Discussion of Results 62 IX

4.2.1 Mineralogy and Porosity Results 62 4.2.2 Effect of Adsorptive Bleaching on Physiochemical Properties of Palm Oil 62 4.2.3 Effectiveness of Activated Local Clays Using Freudlich Adsorption Isotherm 66 4.2.4 Comparison between Local Activated Clays and Imported Bleaching Earth 67 4.2.5 Statistical Analysis of the Results 67 CHAPTER FIVE 5.1 Conclusions 5.2 Recommendations References Determination of Clay Porosity A2.1 PV Standards in Relation to Mass A2.2 Values for Index of Quality of Palm Oil A3.1 Statistical Analysis Results 68 68 69 71 72 72 73 x

LIST OF FIGURES Figure 4.1: Adsorption isotherm plot of clay sample 1 Figure 4.2: Adsorption isotherm plot of clay sample 2 Figure 4.3: Adsorption isotherm plot of clay sample 3 Figure 4.4: Adsorption isotherm plot of clay sample 4 Figure 4.5: Adsorption isotherm plot of clay sample 5 57 58 59 60 61 Xl

LIST OF TABLES Table 2.1: World Palm Oil Producers 6 Table 2.2: Component of Vegetable Oils 7. Table 4.1: The Average Values for Mineralogy Test 34 Table 4.2: Average Values for the Physical Properties of the Clay Samples 35 Table 4.3: Average Values for the Physicochemical Properties of Crude Palm Oil used 36 Table 4.4: Estimated yield of Palm Oil after Neutralization with Various Concentrations ofnaoh 37 Table 4.5: Average Values for the Properties of Oil Obtained when unactivated clays were used for Refining 38 Table 4.6: The Average Values for the Properties of oil Obtained when HCI activated clay Sample 1 was used for Refining 40 Table 4.7: Average Values for the Properties of oil Obtained when HCI Activated Clay Sample 2 was used 41 Table 4.8: Properties of oil Obtained when HCI Activated Clay Sample 3 was used for Refining 42 Table 4.9: Average Values for the Properties of oil Obtained when HCI activated clay sample 4 was used for Refining Palm Oil 43 Table 4.10: The Average Values for the Properties of oil Obtained when HCI activated clay sample 5 was used for Refining Palm Oil 44 Table 4.11: The Average Values for the Properties of oil when Obtained when H2S04 Activated clay sample 1 was used for refining of Palm Oil 45 Table 4.12: The Average Values for the Properties of oil when H2S04 activated clay sample 2 was used for Refining 46 Table 4.13: The Average Values for the Properties of oil Obtained when H2S04 activated clay sample 3 was used for Oil Refining 47 Table 4.14: The Average Values for the Properties of oil obtained when H2S04 activated clay Sample 4 was used for Refining 48 Table 4.15: The Average Values for the Properties of oil obtained when H2S04 activated clay Sample 5 was used for Refining 49 xu

Table 4.16: The Average Values for the Properties for the Adsorption Isotherms Results for Clay Samples 1-5 50 Table 4.17: Adsorption Isotherm results for: 51 Table 4.18: Adsorption Isotherm results for clay samples 5 52 Table 4.19: nand k value from the isotherms 53 Table 4.20: The Average Values for the Properties changes during various refining processes 54 Table 4.21: Percentage Colour Reduction (%CR) Adsorption Isotherms Constant for Local and Imported Activated Clays 55 Table 4.22: Properties of Local and Imported Refined Palm Oil Table A2.1: PV Standards in Relation to Mass 72 Table A2.2: Values for Index of Quality of Palm Oil 73 Xlll