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LOW TEMPERATURE PRECURSORS for METAL OXIDE CATALYSTS by ABDULAZIZ AHMED BAGABAS Bachelor of Science King Saud University Riyadh

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LOW TEMPERATURE PRECURSORS for METAL OXIDE CATALYSTS by ABDULAZIZ AHMED BAGABAS Bachelor of Science King Saud University Riyadh LOW TEMPERATURE PRECURSORS FOR METAL OXIDE CATALYSTS By ABDULAZIZ AHMED BAGABAS Bachelor of Science King Saud University Riyadh, Saudi Arabia 1997 Submitted to the Faculty of the Graduate College of the Oklahoma State University in partial fulfillment of the requirements for the Degree of DOCTOR OF PHILOSOPHY July, 2005 COPYRIGHT By Abdulaziz Ahmed Bagabas July, 2005 ii LOW TEMPERATURE PRECURSORS FOR METAL OXIDE CATALYSTS Dissertation Approved: Dr. Allen Apblett __________________________________________ Dissertation Adviser Dr. K. D. Berlin __________________________________________ Dr. LeGrande M. Slaughter __________________________________________ Dr. Gary Foutch __________________________________________ Dr. A. Gordon Emslie __________________________________________ Dean of the Graduate College iii ACKNOWLEDGMENTS In the Name of Allah, Most Gracious, Most Merciful First of all and formost, I direct all my thanks and praises to Almighty Allah, The Cherisher and Sustainer of the Worlds, for His guidance and assistance that facilitate every stage in my postgraduate studies and in my whole life. Really, my success in everything can only come from Allah. In Him I trust, and unto Him I turn. I would like to express my sincere appreciation and gratitude to my mentor and academic advisor, Dr. Allen W. Apblett, for his invaluable guidance and great support over the years of my graduate studies and during my dissertation research work at Oklahoma State University. I am very grateful and indebted to my advisory committee member and friend Dr. Kenneth Darrell Berlin, Regents Professor of Organic Chemistry, for his precious advice, comments, suggestions, and eternal encouragement throughout my academic program and this investigation. Dr. Berlin was a great reference, a teaching model, a man of honesty and principle, and a brilliant chemist. I will always carry with me his wisdom and exuberance. I also extend my cordial thanks to the rest of my advisory committee members, Dr. LeGrande M. Slaughter, Dr. Gary Foutch, and the late Professor Dr. Elizabeth M. Holt, for their kind cooperation and friendship. I would like also to express my sincere gratitudes to Dr. Margaret Eastman, the manager of Oklahoma statewide NMR facility and solid-state NMR, for recording the 13C iv solid-state NMR spectra for my solid specimens. She was very cooperative and helpful in the work. My appreciation and thanks also go to the late Professor Dr. Elizabeth M. Holt and Dr. Masood A. Khan, the staff crystallographer in the Department of Chemistry at the University of Oklahoma, for single-crystal X-ray diffraction structural determinations. They were ready to lend a hand. Dr. Nicholas F. Materer also deserves my gratefulness for the X-ray photoelectron spectroscopy analysis and his nice friendship. I also express my gratitude to Phoebe Doss, EM Lab manager, for her assistance with the transmission electron microscope (TEM) and scanning electron microscope (SEM) images. I would also like to take this opportunity to thank all the faculty members of the Department of Chemistry at Oklahoma State University from whom I learned a lot during the time of my graduate studies. In addition, I thank the staff and secretaries of the Department of Chemistry for their kindness and cooperation. I kindly thank my beloved parents for their supplications, patience, and support. I ask Allah to bestow on you thy mercy even as you cherished me in childhood. I wish also to express my gratitude to my darling grandmother, Mariam Bukhari, for her prayers, love, and concern. My deepest thanks also go to my brothers and sister and all uncles and aunts for their encouragement and support. I thank my wife, Serene AL-Momen, for her assistance and encouragement. My deepest thanks also go to my beloved kids, who are my great love and the jewels of my life, Zeid Bagabas, Norah AL-Othman, and Abdullah AL-Othman for their cheerfulness. I ask Allah to bless and take care of them. v I am extremely grateful to my chummy, loyal brother Zeid AL-Othman for his constant encouragement, support, assistance, friendship, and advice. He was always available in person to help me at almost all the times. I also express my sincere thanks to his parents, brothers, and relatives for their continual concern and inquiry about me and my studies. I would like also to acknowledge the help of my brothers, Mohammad Al-Ahmadi and Marzook Ashamary, in teaching me how to use the needed computer programs more efficiently. I would like also to thank my lab-mate Dr. B. P. Kiran for his help in GC/MS analysis and for his nice companionship. I also appreciate the friendship and support of all other lab-mates in Dr. Apblett’s group. I extend my thanks and gratitude to my close friends Dr. Othman AL-Nashwan, Dr. Mohammed AL-Saleh, Mohomodou Boncan, Mohammad Elyyan, Muhammad Shahrim AbKarim, Dr. Mumtaz Hussain, Saleh Ashaghathra, Sayeed Mohammad and Majed Nassar for their encouragement, support, and friendship. I appreciate also the great supervision and help of my academic advisors, Dr. Eman Ahmad, Ali Badi, and Dr. Musaed AL-Assaf, at the Royal Embassy of Saudi Arabia Cultrual Mission Attache in Washington, D.C., USA. Last but not the least, I would like to express my thanks to my boss, Dr. Solaiman AL-Khowaiter, my colleagues, and staff at the Petroleum and Petrochemicals Research Institute (PAPRI) for their aid and encouragement. I would also like to acknowledge the financial support of my sponsor King Abdulaziz City for Science and Technology (KACST), Riyadh, Kingdom of Saudi Arabia. vi I conclude these acknowledgements with the supplication of Prophet Solomon (Peace and Blessing upon him) as narrated by the Almighty Allah in The Holy Qur-ān in Sūrat An-Naml (Ants), verse 19, “O my Lord! So order me that I may be grateful for thy favors, which thou has bestowed on me and on my parents, and that I may work the righteousness that will please thee and admit me, by thy grace, to the ranks of thy righteous servants”. vii TABLE OF CONTENTS Chapter Page COPYRIGHT......................................................................................................................ii ACKNOWLEDGMENTS.................................................................................................iv TABLE OF CONTENTS.................................................................................................viii LIST OF TABLES...........................................................................................................xiii LIST OF FIGURES..........................................................................................................xv 1. INTRODUCTION.........................................................................................................1 1.1. SYNTHESIS OF SOLIDS............................................................................1 1.2. CERAMIC METHOD...................................................................................1 1.3 CERAMICS: DEFINITION AND CLASSIFICATION...............................3 1.4. CERAMICS: PROPERTIES AND IMPORTANCE...................................3 1.5. SCOPE OF THIS STUDY............................................................................4 REFERENCES.....................................................................................................7 2. SYNTHESIS OF PYRUVIC ACID OXIME (PAO) METAL COMPLEXES.............9 2.1. BACKGROUND...........................................................................................9 HPAO and its Complexes..............................................................................14 2.2. EXPERIMENTAL......................................................................................20 Materials.............................................................................................................20 Physical and Analytical Measurements.........................................................21 Synthesis........................................................................................................22 Precursors for Metal Oxides.....................................................................22 Pyruvic Acid Oxime (HPAO)...................................................................22 PAO- Salts of Main Group Elements........................................................23 Mg(PAO)2(H2O)3.2H2O.......................................................................23 HOAl(PAO)2.2H2O..............................................................................24 Pb(PAO)2.2H2O...................................................................................25 PAO- Salts of Group 12 Metals................................................................25 Zn(PAO)2.2H2O...................................................................................25 Hg(PAO)2.............................................................................................27 PAO- Salts of Divalent 3d Transition Metals...........................................27 viii Chapter Page Mn4(PAO)8.2H2O.................................................................................27 Fe(PAO)2.2H2O....................................................................................28 Co(PAO)2.2H2O...................................................................................28 Ni(PAO)2.2H2O....................................................................................29 Cu(PAO)2.2H2O...................................................................................29 PAO- Salts of Some Lanthanides..............................................................30
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