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Ion Exchange Behavior Among Metal Trisilicates: Probing Selectivity, Structure, and Mechanism

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Ion Exchange Behavior Among Metal Trisilicates: Probing Selectivity, Structure, and Mechanism ION EXCHANGE BEHAVIOR AMONG METAL TRISILICATES: PROBING SELECTIVITY, STRUCTURE, AND MECHANISM A Dissertation by CHRISTOPHER SEAN FEWOX Submitted to the Office of Graduate Studies of Texas A&M University in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY August 2008 Major Subject: Chemistry ii ION EXCHANGE BEHAVIOR AMONG METAL TRISILICATES: PROBING SELECTIVITY, STRUCTURE, AND MECHANISM A Dissertation by CHRISTOPHER SEAN FEWOX Submitted to the Office of Graduate Studies of Texas A&M University in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY Approved by: Chair of Committee, Abraham Clearfield Committee Members, Marcetta Darensbourg Kim Dunbar Charles Glover Head of Department, David H. Russell August 2008 Major Subject: Chemistry iii ABSTRACT Ion Exchange Behavior among Metal Trisilicates: Probing Selectivity, Structure, and Mechanism. (August 2008) Christopher Sean Fewox, B.S., North Carolina State University Chair of Advisory Committee: Dr. Abraham Clearfield One model system for the investigation of selectivity in inorganic ion exchangers is a group of synthetic analogues of the mineral umbite. Hydrothermally synthesized trisilicates with the general form A 2BSi 3O9•H 2O, where A is a monovalent cation, and B = Ti 4+ , Zr 4+ , and Sn 4+ have been shown to have ion exchange properties. The extended three dimensional framework structure offers the ability to tune the selectivity based on the size of the cavities and channels. The unit cell volume, and therefore the pore size, can be altered by changing the size of the octahedral metal. The substitution of Ge for Si can also increase the pore size. A variety of cations have been exchanged into the trisilicates including alkali and alkaline earths, lanthanides, and actinides. The reason for the selectivity rests in the pocket of framework oxygens which make up the exchange sites. Close examination of the cation environments shows that the ions with the greatest affinity are those that have the closest contacts to the framework oxygens. For example, among alkali cations, zirconium trisilicate demonstrates the greatest affinity for Rb + and has the most A-O contact distances approaching the sum of their ionic radii. The origins of selectivity also rely upon the valence of the incoming cation. When cations are of similar ionic radius, a cation of higher charge is always preferred over the lower valence. Ion exchange studies in binary solutions of cations of different valence, but similar size (1.0Å) have proven the selectivity series to be Th 4+ > Gd 3+ > Ca 2+ > Na +. iv Through structural characterization, kinetic studies, and use of in situ x-ray diffraction techniques the origins of selectivity in these inorganic ion exchangers has been further elucidated. The principles gleaned from these studies can be applied to other inorganic framework materials. The umbite system has the potential to be altered and tailored for specific separation needs. The trisilicate materials presented in this work are representative of the types of advances in inorganic materials research and prove their potential as applicable compounds useful for solving real world problems. v DEDICATION To my wife Miriam whose dedication and dream for me made this work complete and to whom I pledge an eternal life of love and freedom vi ACKNOWLEDGEMENTS As contributors to my education and professional growth and enlightenment these persons hold a special place in my heart. Each one is unique, but the sum of their efforts has made me the scientist and philosopher I am today. Ralton Harris has served as a boss, mentor, and scientific sounding board for over ten years now and has my eternal gratitude for his advice, investment in my growth, and unconditional friendship. Dr. Forrest C. Hentz was an indispensable source of guidance and inspiration in my chemical education. A man of wit, great character, and devotion to his students, he has been blessed with the gift of teaching young minds the world of chemistry. He is the one unique person who showed me how beautiful chemistry is from a simple balanced chemical equation to the complexities of a momentum operator or Eigen function. I would like to thank Dr. F. A. Cotton, who gave me my start here at Texas A&M. In his lab I learned the complexities of inorganic synthesis and gained the confidence to know that I can synthesize anything. I would like to acknowledge Dr. Sharath Kirumakki. He has been a valuable colleague and advisor throughout my endeavors at A&M. Above all the friendships and relationships I have forged here in Texas, his is the one I value the most. I gratefully thank Dr. Akhilesh Tripathi for his attention in training me as a crystallographer. There is no finer or more patient teacher that I have met. I promise him I will continue to break down communication barriers and shake the framework of an inorganic ion exchanger like a cage around a rabbit. Dr. Daniel S. Grum has been my friend for over 17 years. It is no small miracle that we chose the same university to pursue our Ph. D. I am thankful that God chose to make us neighbors and graced us with the ability to support each other. Without him here in College Station, my experience would not have been as rich. I would like to acknowledge my committee members, Dr. Charles Glover, Dr. Marcetta Darensbourg, and Dr. Kim Dunbar. I requested they sit on my committee vii because I have the utmost respect for them as scientists, chemists, and teachers. They have taught me much, and I have always valued my time in and outside the classroom with them. To my family, I am grateful for their support, emotionally, financially, and spiritually. I could not have done this without them. My father, Dalton Fewox, my mother, Alice Fewox, my grandparents, Julius and Irma Wiggins, and Dorothy Fewox all share in the success I have had at A&M. Lastly, and most gratefully I acknowledge Dr. Abraham Clearfield. God truly blessed me the day I joined his research group. I could not hope for a wiser individual to steer me through my course on the way to my doctorate. He has shown patience and kindness throughout my journey over the past 5 years. He has blessed me with gifts of knowledge that I can never repay. He has guided my path, let me stumble, but has always been there for me to lean on as a scientist and a human being. There are no more words to describe appreciation and adoration I hold for him. May his dedication and all his sacrifices in my education be a mitzvah unto him. viii TABLE OF CONTENTS Page ABSTRACT ............................................................................................................... iii DEDICATION ............................................................................................................... v ACKNOWLEDGEMENTS .......................................................................................... vi TABLE OF CONTENTS .......................................................................................... viii LIST OF FIGURES ....................................................................................................... x LIST OF TABLES ....................................................................................................... xii CHAPTER I INTRODUCTION .......................................................................................... 1 1.1. Impetus for this work ..................................................................... 1 1.2. Previously studied inorganic ion exchange materials .................... 2 1.3. Trisilicates ..................................................................................... 4 1.4. Purpose and overview .................................................................. 11 II STRUCTURAL AND MECHANISTIC INVESTIGATION OF RUBIDIUM ION EXCHANGE IN POTASSIUM ZIRCONIUM TRISILICATE .................................................................... 13 2.1. Introduction ................................................................................. 13 2.2. Experimental methods ................................................................. 14 2.3. Results ........................................................................................ 20 2.4. Discussion .................................................................................... 35 2.5. Conclusions ................................................................................. 39 III SYNTHESIS AND CHARACTERIZATION OF PROTONATED ZIRCONIUM TRISILICATE AND ITS EXCHANGE PHASES WITH STRONTIUM ................................... 40 3.1. Introduction ................................................................................. 40 3.2. Experimental methods ................................................................. 41 3.3. Results ......................................................................................... 46 3.4. Discussion .................................................................................... 59 3.5. Conclusions ................................................................................. 62 ix CHAPTER Page IV LANTHANIDE ION EXCHANGE IN METAL TRISILICATES .......................................................................... 63 4.1. Introduction .................................................................................. 63 4.2. Experimental methods .................................................................. 64 4.3. Results .......................................................................................... 70
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