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Design and Applications of Charge-Separated Metal-Organic Frameworks

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Design and Applications of Charge-Separated Metal-Organic Frameworks University of New Mexico UNM Digital Repository Chemistry ETDs Electronic Theses and Dissertations Fall 11-13-2019 Design and Applications of Charge-Separated Metal-Organic Frameworks Sheela Thapa University of New Mexico - Main Campus Follow this and additional works at: https://digitalrepository.unm.edu/chem_etds Part of the Physical Chemistry Commons Recommended Citation Thapa, Sheela. "Design and Applications of Charge-Separated Metal-Organic Frameworks." (2019). https://digitalrepository.unm.edu/chem_etds/165 This Dissertation is brought to you for free and open access by the Electronic Theses and Dissertations at UNM Digital Repository. It has been accepted for inclusion in Chemistry ETDs by an authorized administrator of UNM Digital Repository. For more information, please contact [email protected], [email protected], [email protected]. Sheela Thapa Candidate Chemistry and Chemical Biology Department This dissertation is approved, and it is acceptable in quality and form for publication: Approved by the Dissertation Committee: Prof. Yang Qin, Chairperson Prof. Brian Gold Prof. Christine Mai Le Prof. Gayan Rubasinghege i Design and Applications of Charge-Separated Metal-Organic Frameworks by Sheela Thapa M.Sc. Chemistry, Tribhuvan University, 2009 DISSERTATION Submitted in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy Chemistry The University of New Mexico Albuquerque, New Mexico December 2019 ii DEDICATION To my beloved parents and my loving husband! iii ACKNOWLEDGEMENTS First of all, I would like to express my sincere gratitude to my advisor, Professor Yang Qin for providing me an opportunity to work under his supervision. I would like to thank him for his encouragement, guidance and research training during my PhD research. The research knowledge and skills I have learned from him are the most valuable achievements of my PhD degree. My cordial thanks to my dissertation committee members, Professor Brian Gold, Professor Christine Mai Le and Professor Gayan Rubasinghege for their time and suggestions about my work. I would also like to thank my research proposal committee members Professor Ramesh Giri and Professor Wei Wang for their feedback and advice on my research work. Special thanks to Professor Jeff Rack for all the insightful comments and advice on my research work. Thanks to Dr. Diane Dickie from University of Virginia for all single crystal XRD analysis. Thanks to Professor Gayan Rubasinghege and Eshani Hettiarachchi from New Mexico Tech for the research collaboration. Additionally, I would like to thank all the past and present group members of the Qin research group for their help and assistance in the lab and my research work. I will always remember and cherish every happy and funny moments I spent with my lab mate and a very good friend Lingyao. Many thanks to my friends Rajani, Surendra, Jillian, Griffin, Sangita, Umesh, Prakash, Tefera and Ranjana for their friendship and making my time at UNM memorable. I am also thankful to all the professors and staffs of the UNM Chemistry Department for their assistance throughout my PhD study. Finally, I would like to thank my family, my father Narayan B. Thapa, my late mother Krishna K. Thapa, my sisters and brothers-in-law for their unconditional love and iv support. I would like to thank my sweet and loving husband Dr. Shekhar KC for being my best friend. He has always inspired me to pursue my dream and supported me during my good and bad times. My PhD research would not have been possible without his love, help, guidance and encouragement. v Design and Applications of Charge-Separated Metal-Organic Frameworks By Sheela Thapa M.Sc. Chemistry, Tribhuvan University, Nepal, 2009 Ph.D. Chemistry, University of New Mexico, USA, 2019 Abstract Ionic tetrapodal ligands with colinear coordinating arms are very effective for designing hybrid porous materials with unusual structure and properties. The novelty of this research work lies in the utilization of a unique borate ligand that leads to charge- separated MOF structure with tailor designed properties. Borate ligands being tetrahedral afford 3D materials and the negative charge of borate anion can compensate the positive charge of metal ion in the framework. The borate ligands designed in this research consists of quaternary ammonium cation and anionic borate with four pyridine arms. These ligands upon coordination with Cu(I), Cu(II), Ag(I) and Co(II) metal cations formed six different charge-separated MOFs (UNM-1 to UNM-6). Chapter 1 covers a brief review on the design, synthesis, classification and applications of MOFs. Additionally, MOF interpenetration, control and applications of interpenetration are discussed with examples. Chapter 2 is about the synthesis, structural characterization and application of a charge-separated diamondoid UNM-1 MOF assembled from tetrakis(4- vi pyridyltetrafluorophenylethynyl)borate (T1) and Cu(I) metal cation. UNM-1 MOF structure displays 4-fold interpenetration, resulting in high environmental stability, and at 2 the same time possesses relatively large surface area (SABET = 621 m /g) due to the absence of free ions. Gas adsorption measurements revealed temperature-dependent CO2 adsorption/desorption hysteresis and large CO2/N2 ideal selectivities up to ca. 99 at 313 K and 1 bar, suggesting potential applications of this type of charge-separated MOFs in flue gas treatment and CO2 sequestration. In Chapter 3, synthesis and single-crystal structural characterization of four new charge- separated MOFs (UNM-2, UNM-3, UNM-4 and UNM-5) based on two tetrapodal borate ligands: (T1) and tetrakis(4-pyridyltetrafluorophenyl)borate (T2) having coordinating arms of different lengths and pyridine groups at the end of each arm are discussed. Coordination of these tetrapod with Cu(I)/Cu(II), and Ag(I) ions under specific conditions led to a series of new charge-separated MOFs in single crystalline forms. UNM-2/UNM-3 in monoclinic C 2/c space group, are derived from Cu(NO3)2 upon coordination with T1. On the other hand, coordination of T2 with Cu(CH3CN)4BF4 and AgBF4 respectively formed UNM-4 and UNM-5 in monoclinic I 2/a space group. These MOFs possesses several degrees of interpenetration that are correlated with the arm lengths of ligands. All these MOFs, except UNM-3 are 3D, 2-fold interpenetrated crystalline frameworks. UNM-3 is 1D framework containing coordinated solvent molecules in the crystal structure. In Chapter 4, synthesis of UNM-6, characterization, post-synthetic ionic exchange, applications in chemical fixation of CO2 and CO2/N2 adsorption are discussed. UNM-6 is synthesized via solvothermal synthesis from the assembly of T2 with Co(NO3)2. UNM-6 is crystallized in cubic crystal system with P -4 3 n space group and is 4-fold vii interpenetrated, 3D framework containing coordinated nitrate ion in the crystal structure. The nitrate ion in UNM-6 is replaced with different anions like halides, cyanide and azide by post-synthetic ionic exchange reaction. Furthermore, UNM-6 and bromide exchanged Br-UNM-6 MOFs are used as heterogenous catalysts in the cycloaddition reaction of CO2 to epichlorohydrin without co-catalyst. Both catalysts can be easily separated from the product, very efficient and stable, with ability to be reused multiple times. Additionally, UNM-6 showed very high CO2/N2 separation selectivity of 1022 at 313 K under 1 atm pressure. In summary, this dissertation highlights the versatility of tetrapodal borate ligands in engineering charge-separated MOFs with diverse structures and controlled functionality. viii Table of Contents DEDICATION ............................................................................................................. iii ACKNOWLEDGEMENTS ......................................................................................... iv Abstract ........................................................................................................................ vi List of Figures ............................................................................................................. xii List of Schemes ........................................................................................................ xviii List of Tables ..............................................................................................................xix List of Abbreviations ................................................................................................ xxii Chapter 1. A Review on Metal-Organic Frameworks .................................................1 1.1 Introduction ...........................................................................................................1 1.2 Metal Organic Frameworks (MOFs) ......................................................................2 1.2.1 Design and Synthesis of Metal-Organic Frameworks.......................................4 1.2.2 Classification of Metal-Organic Frameworks ..............................................8 1.2.3 Applications of MOFs .........................................................................................9 1.2.4 Interpenetration in MOFs .............................................................................. 12 Chapter 2. Synthesis, Characterization and Application of Charge-Separated Diamondoid UNM-1 MOF .......................................................................................... 18 2.1 Introduction ........................................................................................................
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