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Fe2o3-Based Oxygen Carriers for Gaseous and Solid-Fueled Chemical Looping Processes

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Fe2O3-based Oxygen Carriers for Gaseous and Solid-Fueled Chemical Looping Processes DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Ankita Majumder Graduate Program in Chemical Engineering The Ohio State University 2016 Dissertation Committee: Professor Liang-Shih Fan, Advisor Professor David L. Tomasko Professor Andre F. Palmer Copyrighted by Ankita Majumder 2016 Abstract Chemical looping is an efficient, economic and sustainable means for electricity and/or chemicals production with inherent CO2 sequestration ability. Oxygen carriers play a crucial role in the successful operation of a chemical looping system as their physical and chemical properties dictate the fuel conversion efficiency of the system. They are expected to undergo multiple redox cycles while maintaining their reactivity and mechanical strength in order to improve the overall process economics for commercial viability. This research investigates the behavior of oxygen carriers under different reactive conditions and evaluates their feasibility for biomass chemical looping systems. The reduction kinetics of OSU’s iron titanium complex metal oxide (ITCMO) oxygen carrier particles are investigated at elevated pressures with H2 and CH4 for application in OSU’s Shale gas-to-Syngas process. Under CH4, there is almost a 5-fold increase in the reduction rate with an increase in pressure from 1 to 10 atm. Solid characterization revealed increased porosity and surface area at elevated pressures. Faster reaction kinetics at higher pressures can translate into increased processing capacity, reduced reactor sizing, and decreased capital costs. The steam to H2 conversion efficiency of Fe2O3 based oxygen carriers using Al2O3, MgAl2O4 and TiO2 as support materials is investigated in a fixed bed for chemical looping H2 generation. All supported-Fe2O3 based oxygen carriers exhibited >70% steam conversion, close to thermodynamic predictions. Due to its ability to not form complexes with the active material, MgAl2O4-supported Fe2O3 was selected ii for further investigation. Thermogravimetric studies with steam oxidation exhibited excellent recyclability and no significant drop in reactivity. MgAl2O4-supported Fe2O3 also exhibited enhanced steam oxidation kinetics at elevated pressures. Tar derived from biomass pyrolysis is a major concern for biomass thermochemical conversion processes. For biomass fueled chemical looping processes, it is important to evaluate effects of tars on the oxygen carriers. Fixed bed experiments demonstrated that OSU’s ITCMO oxygen carriers have reasonable reactivity for cracking most biomass-derived tar components. To further enhance the tar cracking ability of Fe2O3-based oxygen carriers, they are combined with traditional tar cracking catalysts. Based on thermogravimetric reactivity and fixed bed tar cracking experiments, NiO is selected as an additive for Fe2O3-based oxygen carriers for biomass chemical looping systems. The outcomes from this research will help in the development of economic and efficient oxygen carriers for the commercialization of the various chemical looping applications. iii Dedicated to my parents for their immeasurable love, support and encouragement iv Acknowledgements I would like to begin by thanking The Ohio State University and the William G. Lowrie Department of Chemical and Biomolecular Engineering for giving me the opportunity to work in such state-of-the-art facilities. Having easy access to all the excellent university resources and infrastructure has played a huge role in making my academic experience enjoyable and seamless. I would like to express my deepest gratitude and appreciation for my advisor, Dr. Liang-Shih Fan, for constantly encouraging me to strive for excellence in my work. His boundless enthusiasm and thirst for learning has been a constant source of inspiration for me and his constructive feedback has always helped me grow as a researcher as well as a person. I would like to thank Prof. David Tomasko, Prof. Andre Palmer, Prof. Jacques Zakin, and Prof. Lisa Hall for serving on my qualifier, candidacy and dissertation committees. Their discussions and feedback provided me with new ideas and directions for my research. I am grateful to the National Science Foundation (NSF) and the United States Department of Energy (US DOE) for their financial support for the projects I have been a part of during this academic career. The Fan group is full of extremely talented, hardworking and intelligent individuals and I consider myself fortunate to be a part of this group. I would like to thank my seniors, Dr. Liang Zeng, Dr. Siwei Luo, Dr. Andrew Tong, Dr. Zhenchao Sun and Dr. Dawei Wang for their guidance and support and for always being available for discussions. Their v invaluable insights have helped shape up my research in many ways. Dr. Niranjani Deshpande, Dr. Samuel Bayham, Elena Chung, William Wang and Cheng Chung have not only been incredible co-workers, but also great friends, who have provided constant support and made work very enjoyable. It has been a great experience working with all the other Fan group members as well, which include Dr. Lang Qin, Dr. Zhuo Cheng, Dr. Pengfei He, Dr. Qiang Zhou, Dr. Aining Wang, Omar McGiveron, Alan Wang, Mandar Kathe, Dikai Xu, Tien-Lin Hsieh, Sourabh Nadgouda, Amoolya Lalsare, Yaswanth Pottimurthy, Yitao Zhang, and Mengqing Guo. Every member of the group has in many ways helped me grow as researcher and made my experience invaluable. I would also like to mention Camille Ayala and Nicholas Justus, undergraduate researchers who I had the opportunity to mentor. Their keen interest in the work and their insightful questions and suggestions helped me in my research as well. I want to take this opportunity to thank the technical staff at OSU including Paul Green, Michael Wilson, Hendrik Colijn, and Cameron Begg for their willingness to help and provide ideas to help solve any technical problems. A special thanks to Angela Bennett, Susan Tesfai, and Lynn Flanagan for their assistance in completing all my administrative tasks seamlessly in a timely manner. I would like to thank Prof. Bhavik Bakshi and Prof. Kurt Koelling, who guided me in the completion of my teaching assignments. I would like to thank all my friends, who have been like a family to me and filled these past few years with a lot of love and laughter. I would like to especially mention my friend Pooja, who has been there for me at all times, even from a distance. Lastly, I want to take this opportunity to thank my parents, Mrinmoy and Krishna Majumder, for their vi unconditional love and support to grow into the person I am today. They have and continue to remain my pillars of strength and keep me going. Finally, a special thank you my fiancé, Hrishikesh, for always being by my side and encouraging me to strive for more. vii Vita June 2005 ..............................................S.S.C., Fr. Agnel Multipurpose High School June 2007 ..............................................H.S.C., Fr. Agnel Junior College June 2011 ..............................................B.Chem., Institute of Chemical Technology, Mumbai University Sept 2011 to present ..............................Graduate Research Associate, Department of Chemical and Biomolecular Engineering, The Ohio State University Publications Luo, S., Majumder, A., Chung, E., Xu, D., Bayham, S., Sun, Z., Zeng L. and Fan, L.-S. (2013). Conversion of Woody Biomass Materials by Chemical Looping Process: Kinetics, Light Tar Cracking, and Moving Bed Reactor Behavior. Ind. Eng. Chem. Res. 52 (39), 14116-14124. Qin, L., Majumder, A., Fan, J. A., Kopechek, D., and Fan, L.-S. (2014). Evolution of nanoscale morphology in single and binary metal oxide microparticles during reduction and oxidation processes. J. Mat. Chem. A. 2 (41), 17511-17520. Deshpande, N., Majumder, A., Qin, L., and Fan, L.-S. (2015). High-Pressure Redox Behavior of Iron Oxide-Based Oxygen Carriers for Syngas Generation from Methane. Energy Fuels, 29 (3), 1469-1478. Majumder, A., Deshpande, N., Zhang, Y., and Fan, L.-S. Investigation of Al2O3, TiO2 and MgAl2O4 as support materials for Fe2O3-based oxygen carriers for chemical looping hydrogen generation. (In preparation). viii Majumder, A., Ayala, C., Chung, E., and Fan, L-S. Study of Fe2O3-based composite oxygen carriers for in situ tar cracking in biomass chemical looping. (In preparation). Luo, S., Zeng, L., Xu, D., Kathe, M., Chung, E., Deshpande, N., Qin, L., Majumder, A., Hsieh, T.-L., Tong, A., Sun, Z., and Fan, L.-S. (2014). Shale gas-to-syngas chemical looping process for stable shale gas conversion to high purity syngas with a H2: CO ratio of 2:1. Energy Environ. Sci. 7(12), 4104-4117. Luo, S., Bayham, S., Zeng, L., McGiveron, O., Chung, E., Majumder, A., and Fan, L. S. (2014). Conversion of metallurgical coke and coal using a coal direct chemical looping (CDCL) moving bed reactor. Applied Energy, 118, 300-308. Bayham, S. C., Kim, H. R., Wang, D., Tong, A., Zeng, L., McGiveron, O., Kathe, M. V., Chung, E., Wang, W., Wang, A., Majumder, A., and Fan, L.-S. (2013). Iron-based coal direct chemical looping combustion process: 200-h continuous operation of a 25- kWth subpilot unit. Energy Fuels, 27(3), 1347-1356. Fields of Study Major Field: Chemical Engineering ix Table of Contents Abstract ...........................................................................................................................................
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