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The Investigation of Platinum-Tellurium/Aluminum

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The Investigation of Platinum-Tellurium/Aluminum Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1988 The nI vestigation of Platinum-Tellurium/ Aluminum-Oxide and Platinum-Antimony/ Aluminum-Oxide Bimetallic Reforming Catalysts. Chi Hung Cheng Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Cheng, Chi Hung, "The nI vestigation of Platinum-Tellurium/Aluminum-Oxide and Platinum-Antimony/Aluminum-Oxide Bimetallic Reforming Catalysts." (1988). LSU Historical Dissertations and Theses. 4626. https://digitalcommons.lsu.edu/gradschool_disstheses/4626 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Historical Dissertations and Theses by an authorized administrator of LSU Digital Commons. For more information, please contact [email protected]. INFORMATION TO USERS The most advanced technology has been used to photo­ graph and reproduce this manuscript from the microfilm master. UMI films the text directly from the original or copy submitted. Thus, some thesis and dissertation copies are in typewriter face, while others may be from any type of computer printer. The quality of this reproduction is dependent upon the quality of the copy submitted. Broken or indistinct print, colored or poor quality illustrations and photographs, print bleedthrough, substandard margins, and improper alignment can adversely affect reproduction. In the unlikely event that the author did not send UMI a complete manuscript and there are missing pages, these will be noted. Also, if unauthorized copyright material had to be removed, a note will indicate the deletion. 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Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Order Number 8917805 The investigation of PtTe/Al20 3 and PtSb/Al20 3 bimetallic reforming catalysts Cheng, Chi Hung, Ph.D. The Louisiana State University and Agricultural and Mechanical Col., 1988 UMI 300 N. Zeeb Rd. Ann Arbor, MI 48106 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. The Investigation of PtTe/Al2 03 and PtSb/Al.203 Bimetallic Reforming Catalysts A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Chemical Engineering by Chi Hung Cheng B.S., Louisiana State University, 1983 December 1988 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Acknowledgments The author is pleased to acknowledge his indebted­ ness to Dr. Geoffrey. L. Price for his professional guidance and help throughout this work. The time Dr. Price devoted to reviewing this manuscript is especially appreciated. The author is deeply indebted to Dr. Kerry. M. Dooley for his many valuable suggestions during the progress of this work. The author would like to express his gratitude to the dissertation committee, Dr. K. M. Dooley, Dr. D. P. Harrison, Dr. A. B. Corripio in Chemical Engineering Department, and Dr. S. F. Watkins in Chemistry Department for their time spent developing constructive comments on this work. The author wishes to thank Mr. Marcus Nauman in the Chemistry Department for 13C-NMR experiments. The author also expresses his appreciation to the Exxon Foundation for financial support. The assistance of Drs. Kenneth Riley and A1 Schweizer at Exxon Research and Development in Baton Rouge, Louisiana is especially appreciated. Last, but not least, the author wishes to thank his parents and his three sisters for their encouragement ii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. and understanding during his college education. Without them, the author's life would be empty and the work fruitless. 1 1 1 Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. Table of Contents page Acknowledgements -------------------------------- ii Table of Conte n t s ------------------------------- iv List of F i g u r e s ---------------------------------- viii List of T a b l e s ----------------------------------- xiii A b s t r a c t ----------------------------------------- xvi I. Introduction ------------------------------ 1 A. Literature Review -------------------- 5 1. Previous Studies on Te- a n d ------ 5 Sb-containing Reforming Catalysts 2. Other Catalysts ------------------- 7 a. Kinetic Studies of Alloy ----- 9 Catalysts b. Surface Characterization ----- 12 c. Reaction Mechanisms ---------- 20 B. Research Goal and Plan -------- 42 II. Experimental------------------------------ 46 A. Materials and Reagents ---------- 46 B. Equipment---------------------------- 46 1. Recirculation Batch Reactor ---- 46 System 2. Volumetric Adsorption Apparatus - 53 3. Gas Chromatograph and Integrator 54 4. Gas Chromatograph - Mass -------- 62 Spectrometer (GC-MS) iv Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. page 5. Fourier Transform Infrared ----- 63 Spectrometer (FTIR) 6. Gas Adsorption System and IR Cell 65 7. Atomic Absorption ---------------- 68 Spectrophotometer 8. Preparative - Scale G a s ------- 69 Chromatograph 9. Fourier Transform 13 C-NMR ---- 69 10. Thermogravimetric Analyzer ----- 74 C. Experimental Procedures -------------- 74 1. Catalyst Preparation ------------ 74 a. Pt/Alz03 --------------------- 74 b. PtTe/AlzOs ------------------- 77 c. PtSb/Alz Os ------------------- 79 2. Gross Chemical Analysis ---------- 80 a. Determination of Pt Content - 80 b. Determination of Te Content - 81 3. Reducibilities of Telluric ------ 81 Acid 4. Chemisorption of H2 and C O --- 82 5. Reaction Studies ----------------- 83 6. 13 C Labeled Hydrocarbon------ 86 Reactions 7. Syntheses of Labeled ---------- 89 2-Methylpentane v Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. page a. 2-Methylpentane (2-13C) ----- 89 b. 2-Methylpentane (5-13C) ----- 94 8. Isotopic Dilution Method and FTIR 95 III. R e s u l t s ----------------------------------- 97 A. Catalysts-------------------------- 97 B. Chemisorption of H2 and C O -------- 99 C. Kinetic Measurements ----------------- 105 1. Blank Runs -------------------- 105 2. Internal Mass Diffusion------ 107 Limitations 3. n-Hexane Reaction ---------------- 110 a. Pt/AlzOs --------------------- 112 b. Vapor-Deposited PtTe/Al2 03 — 112 c. Coimpregnated PtTe/Al2 03 ---- 119 d. Coimpregnated PtSb/Al2 03 ---- 122 4. Cyclohexane Reaction ------------ 124 D. F T I R ------------------------------- 124 E. Isotopic Tracer Experiments ---------- 131 1. 2-Methylpentane (2-13C) and ----- 131 2-Methylpentane (5-l3C) Reactions 2. Reaction of Benzene and Deuterium 145 a. Deuterium Addition Reaction - 147 b. Benzene Exchange Reaction --- 147 IV. Discussion-------------------------------- 155 A. Surface Characterization ------------- 155 vi Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. page 1. Chemisorption of Hydrogen and --- 155 Carbon Monoxide 2. Fourier Transform Infrared------ 156 Spectroscopy B. Kinetic Studies ----------------------- 158 1. Vapor Deposited PtTe/Al2(>3------ 158 2. Coimpregnated PtTe/Al2<>3 a n d 160 PtSb/Al2 03 C. Mechanistic Studies ------------------ 164 1. Carbon-13 Tracer Experiments ---- 164 2. Reaction of Benzene and Deuterium 171 V. Conclusions and Recommendations --------- 172 A. Conclusions--------------------------- 172 B. Recommendations----------------------- 174 Literature Cited -------------------------------- 177 Appendix A. Dead Volume Determination in the - 186 Volumetric Adsorption Apparatus Appendix B. Calculation of Effectiveness ----- 188 Factor Appendix C. Product Distribution Data at 30% - 193 Conversion of n-Hexane Appendix D. Raw Data for 13C-NMR Experiments - 200 Appendix E. Chi Square Test on the Levels of - 206 Deuterium in Cyclohexane V i t a --------------------------------------------- 207 vii Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. List of Figures page Figure 1-1 Major Reactions in Reforming of 2 C6 Hydrocarbons. Figure 1-2 A Schematic
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