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Advanced Microwave Technology for Biodiesel Feedstock Processing Beatrice G

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Advanced Microwave Technology for Biodiesel Feedstock Processing Beatrice G Louisiana State University LSU Digital Commons LSU Master's Theses Graduate School 2009 Advanced microwave technology for biodiesel feedstock processing Beatrice G. Terigar 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 Terigar, Beatrice G., "Advanced microwave technology for biodiesel feedstock processing" (2009). LSU Master's Theses. 590. https://digitalcommons.lsu.edu/gradschool_theses/590 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]. ADVANCED MICROWAVE TECHNOLOGY FOR BIODIESEL FEEDSTOCK PROCESSING 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 and Agricultural Engineering by Beatrice G. Terigar B.S., Aurel Vlaicu University of Arad, Romania, 2007 August 2009 ACKNOWLEDGMENTS I am thankful to God for the opportunity to pursue my studies at the Louisiana State University; I have been blessed to meet many bright and special individuals here. The encouragement and support of many people have contributed to the completion of this thesis. There are, however, several people that deserve special mention. Words cannot express my deepest appreciation and respect that I have for my major professor, Dr. Dorin Boldor, and his family. He has served as my mentor, teacher, role-model, colleague and friend. The guidance, constant enthusiasm, kindness, approachability, and inspiration that he provided were indispensable throughout my graduate studies, and completion of the thesis. Appreciation is extended to my committee members, Dr. Marybeth Lima and Dr. Vadim Kochergin. Thank you all for your time, support, and insights. To all the people from our research group, Sundar Balasubramanian, Jeff Ortego, Akanksha Kanitkar, all student workers, and Javed Iqbal from W.A. Callegari Center, for their help and assistance during this project, I express a very special thank you. A special acknowledgement is made to my parents, Iolanda and Gabriel Terigar, - without whom I would not be here -, and all my family. There is absolutely no way I could have done this without the love and support that they provided. I feel your love and support despite the distance of a half-globe. In addition, I need to thank my friends; the friendship that they have freely given me is one of the greatest sources of comfort in my life. Thank you all for helping me grow to become the person I am today! ii TABLE OF CONTENTS ACKNOWLEDGMENTS ………………………………………………………………….…… ii LIST OF TABLES………………………………………………………………………………...v LIST OF FIGURES…………...………………………………………………………………….vi LIST OF SYMBOLS AND ABBREVIATIONS……...………………………………………..viii ABSTRACT………………………………………….…………………………………………....x CHAPTER 1. INTRODUCTION ……………………………………...…………………………1 References ……………………………....……………………………………………….. 3 CHAPTER 2. AN ANALYSIS OF THE MICROWAVE DIELECTRIC PROPERTIES OF OIL- SOLVENT MIXTURES AT 300 TO 3000 MHZ ……...……………………………….. 5 Introduction …...……………….………………………………………………....……… 5 Materials and Methods ……...….………………………………………………….……..8 Results and Discussion ...……….…………………………………………………….....10 Conclusions ….….......…………………………………………………………….….… 22 References ….……..……………….………………………………….…………………24 CHAPTER 3. SOYBEAN AND RICE BRAN OIL EXTRACTION EFFICIENCY IN A CONTINUOUS MICROWAVE SYSTEM (LAB AND PILOT SCALE).…….………..26 Introduction ………………………………………………………………….……...….. 26 Materials and Methods …………………………………………………...…...….……...32 Results and Discussion ………………………………………………………………… 39 Conclusions ……………………………………………………….……………………. 57 References ……………………………...……………….…………………………….....58 CHAPTER 4. TRANSESTERIFICATION OF SOYBEAN AND RICE BRAN OIL WITH ETHANOL IN A CONTINUOUS-FLOW MICROWAVE-ASSISTED SYSTEM ………………………………………………………………..…………....… 62 Introduction …………………………………………………………….……………..…62 Materials and Methods …………………………………………………………..….…...67 Results and Discussion ……………………………………………………………….…69 Conclusions ………………………………………………………………….…………..77 References ……………………………..………………………………………………..77 CHAPTER 5. CONTINUOUS MICROWAVE EXTRACTION OF OIL FROM CHINESE TALLOW TREE, AN ALTERNATIVE BIODIEESEL FEEDSTOCK. EFFECT OF STORAGE CONDITIONS ON OIL QUALITY.……...………………..……………... 81 Introduction ……………………………………………………………………….……. 81 Materials and Methods …………………………………………………………………..84 iii Results and Discussion ………………………………………………………………….87 Conclusions …………………………………...…………………………………..……. 98 References ……..……………………...………………………………..……………… 98 CHAPTER 6. CONCLUSIONS AND FUTURE WORK ……………………….…………….102 APPENDIX A. OIL EXTRACTION DATA …………………………………………………….....105 B. OIL AND BIODIESEL COMPOSITION DATA ……………………………...….108 C. STATISTICAL ANALYSIS DATA ………………………...………………...…..116 VITA ………………………………………………………………………………………….. 167 iv LIST OF TABLES Table 2.1. Values for dielectric constant of soy flour mixed ethanol……………..…….….……13 Table 2.2. Values for dielectric constant of rice bran and ethanol…………………….…...........13 Table 2.3. Dielectric constant and loss of soy flour mixed with methanol, isopropanol, and hexane……………………………….…………......……..……………14 Table 2.4. Dielectric constant and loss of rice bran mixed with methanol, isopropanol, and hexane……………………………………………………………..…..14 Table 2.5. Values of '' for soy flour and ethanol………………….….……………..………….17 Table 2.6. Values of '' for rice bran and ethanol……………………………………………….17 Table 2.7. Coefficient values for dielectric constant fitted curve as frequency (Eq. 3)………….21 Table 2.8. Coefficients values and r2 for the multiple linear regressions for methanol and isopropanol with the two feedstocks (Eq. 4 and 5)……………………....22 Table 2.9. Coefficients values and r2 for the multiple linear regressions (frequency and solvent content) for ethanol with the twO feedstocks (Eq. 6 and 7)…………………………………….23 Table 3.1. Free fatty acid composition of soybean and rice bran oil (%)………………………..49 Table 3.2. Acid and iodine value of soybean and rice bran for different flow rates and extraction times (%)……………………………………………….……..56 Table 3.3. Free fatty acid composition of soybean oil (%)………………………………………56 Table 3.4. Free fatty acid composition of rice bran oil (%)………………………………...……57 Table 4.1. Free and total glycerin of SB and RB biodiesel at studied temperatures and reaction times…………………………………………………..……………………70 Table 4.2. FAEE of SB biodiesel at studied temperatures and reaction times…………..………71 Table 4.3. FAEE of RB biodiesel at studied temperatures and reaction times…………………..71 Table 5.1. Average titratable acidity (TA) (mg KOH/g sample) and peroxide values (PV) (meq/kg) of the stored TT seeds……………………………………………...………….89 Table 5.2. Fatty acid composition of stillingia oil (%)……….…………………………….……91 Table 5.3. Properties and composition of the oil from early and late harvested seeds……..……95 v LIST OF FIGURES Figure 2.1. Dielectric constant of soy flour:ethanol at 23°C…………………………………….10 Figure 2.2. Dielectric constant of rice bran:ethanol at 23°C………………………………….…11 Figure 2.3. Dielectric constant of soy flour:hexane at 23°C………………………………….…12 Figure 2.4. Dielectric constant of rice bran:hexane at 23°C…………………………………….13 Figure 2.5. Dielectric loss of soy flour:ethanol at 23°C………………………………………...15 Figure 2.6. Dielectric loss of rice bran:ethanol at 23°C…………………………………………15 Figure 2.7. Dielectric loss of soy flour:ethanol 1:2……………………………………………..18 Figure 2.8. Dielectric loss of rice bran:ethanol 1:2. ………………………………………….…18 Figure 2.9. Dielectric loss of soy flour with different solvents…………………………………19 Figure 2.10. Dielectric loss of rice bran with different solvents………………………………...20 Figure 3.1. Schematic representation of the laboratory-scale continuous microwave assisted extraction system……………………………………………..…….34 Figure 3.2. Laboratory-scale microwave assisted extraction system: left – batch; right – continuous…………………………………………………………..35 Figure 3.3. Schematic design of the pilot scale continuous microwave assisted extraction…….37 Figure 3.4. Design of the pilot scale continuous microwave assisted extraction………………..37 Figure 3.5. Oil extracted at different temperatures and extraction times from A. Soybean and B. Rice bran……………………………...……………...……...………41 Figure 3.6. Soybean oil phospholipids extracted at different temperatures and extraction times…………………………………………………...…..43 Figure 3.7. Rice bran oil waxes extracted at different temperatures and extraction times………44 Figure 3.8. Maximum yields in different extraction methods…………………………...………45 Figure 3.9. Soybean oil Acid and Iodine value at different temperatures and extraction times…47 Figure 3.10. Rice bran oil Acid and Iodine value at different temperatures and extraction times……………………………………………………….47 vi Figure 3.11. Oil extracted at different flow rates and extraction times from A. Soybean and B. Rice bran…………………………………………………………….51 Figure 3.12.Scanning Electron Micrograph of microwave treated soybean (left column) and rice bran (right column) for 6, 10 and 60 min…………………………………….…53 Figure 3.13. Soybean oil phospholipids extracted at different flow rates and extraction times………………………………………………………..…54 Figure 3.14. Rice bran oil waxes extracted at different flow rates and extraction
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