Louisiana State University LSU Digital Commons LSU Master's Theses Graduate School 2010 Parameterization of microwave assisted oil extraction and its transesterification to biodiesel Akanksha V. Kanitkar Louisiana State University and Agricultural and Mechanical College, [email protected] Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_theses Part of the Engineering Commons Recommended Citation Kanitkar, Akanksha V., "Parameterization of microwave assisted oil extraction and its transesterification to biodiesel" (2010). LSU Master's Theses. 4126. https://digitalcommons.lsu.edu/gradschool_theses/4126 This Thesis is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Master's Theses by an authorized graduate school editor of LSU Digital Commons. For more information, please contact [email protected]. PARAMETERIZATION OF MICROWAVE ASSISTED OIL EXTRACTION AND ITS TRANSESTERIFICATION TO BIODIESEL A Thesis Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Master of Science in Biological and Agricultural Engineering in The Department of Biological & Agricultural Engineering by Akanksha V. Kanitkar B.Tech., University Department of Chemical Technology, 2007 May 2010 DEDICATION ♥ To my beloved parents without whom I would not have come so far... ii ACKNOWLEDGMENTS I would like to thank the Almighty for his blessings towards achieving this goal in my life and my family for their encouragement and unconditional support. Mom and Dad, I owe all my success to you. I would like to express my gratitude towards my parents, Mrs. Prerna Kanitkar and Mr. Vishwas Kanitkar for their parental love and making me the person I am today. Most of all, I would like to thank Dr. Dorin Boldor for accepting me as a research assistant and for his guidance and advice throughout. He has been my mentor and my support at all the times. I am very thankful to him for having given me an opportunity to work on interesting projects and for his constant encouragement and faith in me. His constant enthusiasm and zeal during my research has made the work really interesting. I would also like to thank Dr. Marybeth Lima and Dr. Gary Breitenbeck for serving on my committee. Their timely and valuable inputs to my project are highly appreciated. I would also like to thank Dr. Sundar Balasubramanian for all his help and valuable piece of advice at all times when needed. I am also grateful to Dr. Cristina Sabliov for letting me work in her lab and encouraging me to give my best at all the times. I would like to thank all my colleagues and fellow graduate students at Biological & Agricultural Engineering Department. A special thanks to Beatrice Terigar, Laura Picou and Casey McMan for their help and assistance during the project. I thank Carlos Astete for all his inputs and help at all the times while working in the lab. He has been a great individual from whom I have got to learn a lot. I want to thank Cindy Henk and Ying Xiao for her assistance in using the scanning electron microscopy and Dr. Claudia Leonardi for help with the statistical analysis of the data. Thank you, Becky Schramm, for all your help. I am very thankful to Dr. Dooley from whom I got to learn a lot of things directly or indirectly related to my project. Javed Iqbal from W.A. Callegari Center deserves a iii special mention for all his help and coordination during analysis of biodiesel. His clarity on the subject helped me understand things in a better way. I am very grateful to Akshay Patel for making me aware of the wonderful research opportunity at LSU. Thanks to all my friends in Baton Rouge for making me feel at home away from home. I thank Sreekanth Pothanis and Monika Gadre who have been great friends, and patient listeners at all times! Thanks Dhruva for all the help and encouragement! Dnyanada, thanks for being with me and giving me the assurance that everything is possible if you think you can. You have been my stress buster at all the times. Last, but definitely not the least, I cannot express in words the mental support, motivation and love Kartik has given me without whom the journey so far seems impossible. He has stood by me during all the times and has been my confidence and motivation. Thank you dear, this is dedicated to you. Thank you all for being a part of it! iv TABLE OF CONTENTS ACKNOWLEDGEMENTS………………………………………………………………………iii LIST OF TABLES……………………………………………………………………………….vii LIST OF FIGURES………………………………………………………………………………ix ABSTRACT……………………………………………………………………………………….x CHAPTER 1. INTRODUCTION…………………………………………………………………1 1.1 References……………………………………………………………………………..6 CHAPTER 2. MICROWAVE- ASSISTED EXTRACTION OF SOYBEAN AND RICE BRAN OIL: YIELD AND QUALITY CHARACTERIZATION…………………………………..…….8 2.1 Introduction……………………………………………………………………………8 2.2 Materials and Methods……………………………………………………………….12 2.3 Results and Discussion……………………………………………………………… 17 2.4 Conclusions…………………………………………………………………………..35 2.5 References……………………………………………………………………………36 CHAPTER 3. MICROWAVE- ASSISTED EXTRACTION OF LIPIDS FROM CHINESE TALLOW TREE SEEDS: AN ALTERNATE FEEDSTOCK FOR BIODIESEL PRODUCTION…………………………………………………………………………………..40 3.1 Introduction……………………………………………………………………….…..40 3.2 Materials and Methods…………………………………………………………….….44 3.3 Results and Discussion….…………………………………………………………… 46 3.4 Conclusions…………………………………………………………………….……..56 3.5 References….…………………………………………………………………………57 CHAPTER 4. COMPARISON OF METHYL AND ETHYL ESTERS PRODUCTION FROM SOYBEAN AND RICE BRAN OIL IN THE PRESENCE OF MICROWAVES……………... 60 4.1 Introduction…………………………………………………………………………..60 4.2 Materials and Methods……………………………………………………………….64 4.3 Results and Discussion……………………………………………………………….66 4.4 Conclusions..……………………………………………………………………….…80 4.5 References……………………………………………………………………………80 CHAPTER 5. SUMMARY AND FUTURE WORK……………………………………………83 APPENDIX A. SOYBEAN AND RICE BRAN OIL EXTRACTION DATA………………….87 APPENDIX B. OIL EXTRACTION DATA FOR CTT SEEDS………………………………..92 v APPENDIX C. TRANSESTERIFICATION DATA OF SOYBEAN AND RICE BRAN OIL TO METHYL AND ETHYL ESTERS……………………………………………………………..105 VITA……………………………………………………………………………………………118 vi LIST OF TABLES Table 2.1. Oil yields using MAE and control extraction (CE) (mean± std dev)………………...18 Table 2.2. Oil yields from soybeans and rice bran (mass basis)…………………………………20 Table 2.3. Coefficients for the multiple linear regression……………………………………….30 Table 2.4. Acid and iodine values for microwave extracted soybean oil and rice bran oil……...31 Table2.5. Fatty acid composition of microwave extracted soybean oil (Tr. = trace amounts)…..32 Table 2.6. Fatty acid composition of microwave extracted rice bran oil (Tr. = trace amounts)…33 Table 2.7. Phospholipid (hydratable) content of microwave extracted soybean oil and wax content of microwave extracted rice bran oil………………………………………...35 Table 3.1. Fatty acid composition of CTT lipid yields…………………………………………..46 Table 3.2. CTT lipid yields obtained using batch MAE and control extraction ………………...48 Table 3.3. Mass balance showing differences between batch and CMAE process…..………….53 Table 3.4. Coefficients for the multiple linear regression……………………………………….55 Table 4.1. Free and total glycerin content and conversion for fatty acid esters of soybean oil….66 Table 4.2. Free and total glycerin content and conversion for fatty acid esters of rice bran oil...67 Table 4.3. Specific heat values for oils and alcohol………………………………………………71 Table 4.4. Energy consumed per kg of biodiesel produced……………………………………...71 Table 4.5. Methanol and ethanol consumption values …………………………………………..73 Table 4.6. Energy consumed for evaporation of residual alcohol…………………………….....73 Table 4.7. Oxidative stability of fatty acid alkyl esters………………………………………….76 Table 4.8. Viscosity of fatty acid alkyl esters………………………………………………..…..77 Table 4.9. Cloud point of fatty acid alkyl esters………….……………………………………...78 Table 4.10. Flash point of fatty acid alkyl esters……………………………...…………………78 vii Table 4.11. Acid value of fatty acid esters……………………………………………………….79 viii LIST OF FIGURES Figure 2.1. Cross section of soybean seed (Pietrzak and Miller, 2005)…………………………...9 Figure 2.2. SEM images of soybeans subjected to control (top) and microwave extraction (bottom) at 120°C for 15 min……………………...………………...…………………………..21 Figure 2.3. SEM images of rice bran subjected to control (top) and microwave extraction (bottom) at 120°C for 15 min……………………...………………...……………………………………...22 Figure 2.4. Soybean oil yields as a function of extraction time and temperature……….……….24 Figure 2.5. Rice bran oil yields as a function of extraction time and temperature……..………..25 Figure 2.6. Soybean oil yields as a function of temperature, f(T)= y0+b*T……………..…..…..27 Figure 2.7. Rice bran oil yields as a function of temperature, f(T)= y0+b*T……………………....……..27 -bt Figure 2.8. Soybean oil yields as a function of extraction time, f(t)= y0+ a(1- e )……………..28 -bt Figure 2.9. Rice bran as a function of extraction time, f(t)= y0+ a(1- e )………………...…….29 Figure 3.1. a) Chinese TT seeds with coating and kernels and b) cross section of seed (USDA, 2000)………………………………………………………………………………………….….41 Figure 3.2. a) Outer vegetable tallow coating, b) Kernel rich in Stillingia oil and c) SEM image of Chinese TT seed at 200X magnification………………………………………..……………42 Figure 3.3. Snapshots of microwave power input into the batch (left) and continuous (right) systems ………………………………………………………………………………………….49