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An Experimental Study on Solvent Liquefaction Martin Robert Haverly Iowa State University

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An Experimental Study on Solvent Liquefaction Martin Robert Haverly Iowa State University Iowa State University Capstones, Theses and Graduate Theses and Dissertations Dissertations 2016 An experimental study on solvent liquefaction Martin Robert Haverly Iowa State University Follow this and additional works at: https://lib.dr.iastate.edu/etd Part of the Mechanical Engineering Commons Recommended Citation Haverly, Martin Robert, "An experimental study on solvent liquefaction" (2016). Graduate Theses and Dissertations. 15928. https://lib.dr.iastate.edu/etd/15928 This Dissertation is brought to you for free and open access by the Iowa State University Capstones, Theses and Dissertations at Iowa State University Digital Repository. It has been accepted for inclusion in Graduate Theses and Dissertations by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. An experimental study on solvent liquefaction by Martin Robert Haverly A dissertation submitted to the graduate faculty in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY Co-Majors: Mechanical Engineering and Biorenewable Resources and Technology Program of Study Committee: Robert C. Brown, Major Professor Mark Mba Wright Theodore J. Heindel Steven J. Hoff Max D. Morris Iowa State University Ames, Iowa 2016 Copyright © Martin Robert Haverly, 2016. All rights reserved. ii TABLE OF CONTENTS NOMENCLATURE ................................................................................................................. v ACKNOWLEDGMENTS ...................................................................................................... vii ABSTRACT ............................................................................................................................. ix CHAPTER 1 INTRODUCTION .............................................................................................. 1 Biomass as a Renewable Source of Carbon ........................................................................ 1 Biomass Composition ......................................................................................................... 4 Overview of Direct Liquefaction ........................................................................................ 8 Continuous Processing ...................................................................................................... 13 Dissertation Organization ................................................................................................. 16 References ......................................................................................................................... 20 CHAPTER 2 CONTINUOUS SOLVENT LIQUEFACTION OF BIOMASS IN A HYDROCARBON SOLVENT ........................................................................................ 24 Abstract ............................................................................................................................. 24 Introduction ....................................................................................................................... 25 Materials and Methods ...................................................................................................... 29 Results & Discussion ........................................................................................................ 41 Conclusions ....................................................................................................................... 53 Acknowledgements ........................................................................................................... 54 Funding Sources................................................................................................................ 55 CHAPTER 3 THE EFFECT OF MOISTURE ON HYDROCARBON-BASED SOLVENT LIQUEFACTION OF BIOMASS .................................................................................... 58 Abstract ............................................................................................................................. 58 Introduction ....................................................................................................................... 59 Experimental ..................................................................................................................... 62 Analytical Methods ........................................................................................................... 68 Results and Discussion ..................................................................................................... 69 iii Conclusions ....................................................................................................................... 87 References ......................................................................................................................... 88 CHAPTER 4 OPTIMIZATION OF PHENOLIC MONOMER PRODUCTION FROM SOLVENT LIQUEFACTION OF LIGIN ........................................................................ 93 Abstract ............................................................................................................................. 93 Introduction ....................................................................................................................... 94 Materials and Methods ...................................................................................................... 99 Results and Discussion ................................................................................................... 107 Conclusions ..................................................................................................................... 120 Acknowledgements ......................................................................................................... 121 References ....................................................................................................................... 122 CHAPTER 5 THERMAL STABILITY OF FRACTIONATED BIO-OIL FROM FAST PYROLYSIS ................................................................................................................... 126 Abstract ........................................................................................................................... 126 Introduction ..................................................................................................................... 127 Materials and Methods .................................................................................................... 129 Results and Discussion ................................................................................................... 140 Conclusions ..................................................................................................................... 148 Acknowledgements ......................................................................................................... 149 References ....................................................................................................................... 149 CHAPTER 6 DEVELOPMENT AND APPLICATION OF ALTERNATIVE METHODS FOR DETERMINING THERMOPHYSICAL PROPERTIES OF PYROLYSIS LIQUIDS......................................................................................................................... 153 Abstract ........................................................................................................................... 153 Introduction ..................................................................................................................... 154 Experimental Section ...................................................................................................... 155 Results and Discussion ................................................................................................... 171 Conclusions ..................................................................................................................... 181 iv Acknowledgements ......................................................................................................... 182 References ....................................................................................................................... 182 CHAPTER 7 CONCLUSIONS AND FUTURE WORK ..................................................... 187 Conclusions ..................................................................................................................... 187 Future Work .................................................................................................................... 190 APPENDIX A PHYSICAL BEHAVIOR OF WATER DURING SOLVENT LIQUEFACTION OF BIOMASS IN A HYDROCARBON-BASED SOLVENT ........ 193 APPENDIX B EFFECT OF MOISTURE ON SOLVENT LIQUEFACTION OF LOBLOLLY PINE.......................................................................................................... 195 APPENDIX C THERMAL CONDUCTIVITY RESULTS ................................................. 198 APPENDIX D ENTHALPY OF VAPORIZATION RESULTS .......................................... 205 v NOMENCLATURE AF – ash-free ANOVA – analysis of variance DI – de-ionized EDS – Exxon Donor Solvent ESP – electrostatic precipitator FTIR – Fourier Transform Infrared spectroscopy GC-MS/FID – gas chromatography – mass spectroscopy/flame ionization detector GPC – gel permeation chromatography HDS – hydrogen donor solvent HPLC – high performance liquid chromatography HPTT – high pressure thermal treatment HSP – Hildebrand solubility parameter IC – ion chromatography LCO – light cycle oil mGC – micro gas chromatograph
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