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View to Its Use in An Florida State University Libraries Electronic Theses, Treatises and Dissertations The Graduate School 2017 Electro-Oxidation of Glycerol with Electroless CuNiMoP: Production of Fine Chemicals and Prospects for Co-Generation of Energy Oyidia Elendu Follow this and additional works at the DigiNole: FSU's Digital Repository. For more information, please contact [email protected] FLORIDA STATE UNIVERSITY COLLEGE OF ENGINEERING ELECTRO-OXIDATION OF GLYCEROL WITH ELECTROLESS CUNIMOP: PRODUCTION OF FINE CHEMICALS AND PROSPECTS FOR CO-GENERATION OF ENERGY By OYIDIA ELENDU A Dissertation submitted to the Department of Biomedical and Chemical Engineering in partial fulfillment of the requirements for the degree of Doctor of Philosophy 2017 Oyidia Elendu defended this dissertation on April 11, 2017. The members of the supervisory committee were: Yaw Yeboah Professor Co-Directing Dissertation Egwu Kalu Professor Co-Directing Dissertation Peter Kalu University Representative John Telotte Committee Member The Graduate School has verified and approved the above-named committee members, and certifies that the dissertation has been approved in accordance with university requirements. ii ACKNOWLEDGMENTS I would like to first thank my supervisors, Dr. Egwu E. Kalu and Dr. Yaw Yeboah, for the opportunity to do this work. They believed that I could do it and thus, guided, encouraged and often pushed me beyond what I thought was adequate. I see the individual strengths they each brought to bear on this project, and I am grateful. I would also like to thank my committee members: Dr. Telotte always provided a fresh perspective to the challenges I encountered, and often his suggestions helped to find my way out of a maze. Dr. Onyeozili provided invaluable help in the identification of organic species encountered in electro-synthesis aspect of the project. She often went far and beyond the call of duty, coming down to work with our equipment, if she thought it necessary. I also thank Dr. Peter Kalu for his help in understanding metal and composite behavior in the electro-catalysts. I thank my colleagues in the Electrochemical and Renewable Energy Research Group in the FAMU-FSU College of Engineering – past and present. Shannon Anderson, Ever Velasquez, James Akrasi, Ruben Nelson, Venroy Watson, Wasu Chaitree, Joel Sankar and Joyce Kosivi: thank you for being sounding boards for ideas, willing guinea pigs for presentations, and all the lunch dates. I could not have asked for a better group of colleagues. You guys are truly awesome. I am grateful to the Eziyis, Kosivis, Ufodikes and Oforis. It would be next to impossible to fail with these guys rooting for you. If any of you are ever in any city where I am, know that you have at least one friend there already. I think of my family and each person’s contribution to today: my husband, Chidi, it was providence that made our paths cross. Thank you for your unquestioning support, kindness and love; my son Dirim, who brought laughter to many days; my father, Chief Godwin Eze who instilled in me the thirst for knowledge; my mother, Mrs. Jane Eze and mother-in-law, Mrs. iii Comfort Elendu who looked after my family when I left Nigeria for the USA; my sisters, Dr. Onyinye Anyaso and Dr. Uzochi Anemene; my brothers – Eze, Ojukwu and Chidi; my aunts- Mrs. Ngozi Kalu and Mrs Victoria Chuku – voices of reason in a quest in which it was easy to lose focus. I celebrate every one of them today, and honor the memory of those who have passed on. I acknowledge that this work would not have been possible without funding from the National Science Foundation and the Department of Biomedical and Chemical Engineering, College of Engineering, FAMU-FSU College of Engineering. Above all, my most humble appreciation to God for His infinite grace and mercy throughout my academic pursuit. iv TABLE OF CONTENTS LIST OF TABLES ....................................................................................................................... viii LIST OF FIGURES ....................................................................................................................... ix ABSTRACT ................................................................................................................................. xiv 1. INTRODUCTION ...................................................................................................................... 1 1.1 Background ....................................................................................................................... 1 1.2 Sustainable Uses of Glycerol ............................................................................................ 2 1.3 Catalysts for Glycerol Oxidation .................................................................................... 10 1.4 The Technique of Electroless Deposition ....................................................................... 13 1.5 Economic Considerations for Glycerol Electro-Oxidation ............................................. 16 1.6 Research Goals and Organization of Text ...................................................................... 17 2. METHODS AND MATERIALS .............................................................................................. 20 2.1 Introduction ..................................................................................................................... 20 2.2 Electroless Bath Formulation .......................................................................................... 21 2.3 Substrate Preparation ...................................................................................................... 23 2.4 Electrode Preparation ...................................................................................................... 23 2.5 Deposit Characterizations ............................................................................................... 25 2.6 Fabrication of Electrochemical Reactor.......................................................................... 26 2.7 Cyclic Voltamograms ..................................................................................................... 27 2.8 Constant Potential Oxidation .......................................................................................... 28 2.9 Oxidation Product Analysis ............................................................................................ 28 3. CATALYST SYNTHESIS AND CHARACTERIZATION .................................................... 30 3.1 Introduction ..................................................................................................................... 30 3.2 Choice of Main Active Materials .................................................................................... 30 3.3 Electroless Deposition of Copper and Nickel: Reducing Agent Study .......................... 32 v 3.4 Effect of Time of Deposition on Deposit Characteristics ............................................... 36 3.5 Effect of Cu2+ and Dual Reducing Agents in the Electroless Bath ............................... 47 4. ELECTROCHEMICAL PERFORMANCE OF CUNIMOP.................................................... 50 4.1 Introduction ..................................................................................................................... 50 4.2 Combined Effect of Copper, Nickel, Molybdenum and Phosphorus ............................. 50 4.3 Reactions at CuNiMoP Anode ........................................................................................ 52 4.4 Performance of CuNiMoP/C under Unstirred Cell Conditions ...................................... 54 4.5 Performance of CuNiMoP/C under Stirred Conditions .................................................. 59 4.6 Determination of Kinetic Parameters for CuNiMoP/C ................................................... 61 4.7 Chronoamperometry of Glycerol Oxidation on CuNiMoP ............................................ 64 5. GLYCEROL CONVERSION AND OXIDATION PRODUCT YIELD DURING POTENTIOSTATIC OXIDATION OF GLYCEROL ON CUNIMOP ....................................... 67 5.1 Introduction ..................................................................................................................... 67 5.2 Thermodynamic Considerations for 3-Carbon Oxidation Products ............................... 67 5.3 Controlled Potential Electro-Oxidation of Glycerol ....................................................... 68 5.4 Reaction Mechanism and Pathways................................................................................ 79 6. STUDIES IN CATALYST STABILITY ................................................................................. 85 6.1 Introduction ..................................................................................................................... 85 6.2 Catalyst Loss in Use........................................................................................................ 85 6.3 Copper Behavior under Alkaline Conditions .................................................................. 87 7. CONCLUSIONS AND FURTHER WORK ............................................................................ 89 7.1 General Conclusions ....................................................................................................... 89 7.2 Directions for Future Work ............................................................................................. 90 APPENDICES .............................................................................................................................
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