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Gibbs Energy Between Carbide and Graphite Reactions Correlates with the Decrease of Water Concentrations at Low Operating Temperatures

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Gibbs Energy Between Carbide and Graphite Reactions Correlates with the Decrease of Water Concentrations at Low Operating Temperatures CARBON DEPOSITION IN A BOSCH PROCESS USING A COBALT AND NICKEL CATALYST by James Edwin Garmirian B.A., Hope College (1976) SUBMITTED IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY at the MASSACHUSETTS INSTITUTE OF TECHNOLOGY March 1980 Massachusetts Institute of Technology 1980 Signature of Author: Department of CheyXlca-l Engineering Certified by: Thesis Supervisor Certified by: Thesis Supervisor 7) Accepted by: Chairman, Departmental Committee on Graduate Theses ARCHIVES MASSACHJ3T i• JUN i 3 1980 LIBRARIES 2 Abstract NASA has been active in developing processes to recover oxygen from meta- bolic carbon dioxide. Their ultimate objective has been to construct a life support system capable of supplying oxygen in a cyclic process. The cycle of interest here begins by reducing the carbon dioxide with hydrogen to form solid carbon and is known as the Bosch process. An iron catalyst is normally used. CO2 + 2H2 Catalyst. C + 2H20 2H20 Electroylsis, 2H2 + 02 CO2 - C + 02 The water is then electrolyzed to oxygen and hydrogen. The overall process results in the conversion of carbon dioxide to carbon and oxygen. Previous studies have shown that water concentrations over an iron catalyst are limited to a maximum of 16% (915K) due to the formation o'f non-catalytic iron oxides. It has been found in this thesis that through the use of cobalt and nickel catalysts, water concentrations of 32% (800K) and 25% (825K), re- spectively, may be obtained. The assumption that the gas phase is in equilib- rium with graphite leads to predictions that even higher water concentrations could be obtained at lower temperatures. However, it is shown that the equilib- rium state cannot be achieved. A mechanism has been proposed which suggests that carbon formation occurs via a carbide intermediate. The difference in Gibbs energy between carbide and graphite reactions correlates with the decrease of water concentrations at low operating temperatures. DEDICATION This thesis is dedicated to my parents, Edwin and Rachael Garmirian, for all their love, guidance, and support which they have given me throughout my life. Acknowledgements This project was supported by a research grant from the National Aeronautics and Space Administration. The assistance of Dr. Philip D. Quattrone is gratefully acknowledged. To Hope College, I give great thanks for providing me with more than just a college education, most of all, to Professors Sheldon Wettack, and William Mungall, and the rest of the Chemistry department for their encourage- ment and leadership. I thank Professors Richard Brockmeirer, James Van Puttan, and James Toevs of the Physics department for their guidance and education. To Lise Hager, thanks for everything,Stratford, school, and just fooling around. Bill Doerr and James Christowski made life in the basement interesting and were always very supportive, thanks. The friendship of Ted Bush, John Ninniger, Ken Hellyar, Tom Irwin, Patty Rich, Gina Shuck, Mike Klein and of course David Stern made graduate life both in and out of the lab enjoyable and entertaining. The friendship, discussions, and technical advice of Charles Foshey are greatly appreciated. Harold Duffett was a good friend, thanks. I must thank (Father) Frank Bates, Peter Levy (Goodwrench), and Sue Harrison for their friendship and my Armenian wife. Without the help and friendship of both Sally Kreuz and Stan Mitchell this thesis would have never been bound. Jeffrey Wingard's participation in collecting the experimental data is also appreciated. I would like to thank Professor Williams for sincerely and patiently answering the somewhat obscure questions of a wondering graduate student. I appreciate the time Professors Meissner and Satterfield spent discussing this thesis with me. 5 Albert Sacco was the one who inspired my initial interest in the Bosch process, to him I give many thanks. I would like to thank Professor Robert Reid for the guidance and inspir- ation he has given me throughout my years here at M.I.T. Without Professor Michael Manning's daily discussions and technical advice, I still might have finished this thesis, but without his inspiration, dedication, and genuine concern for my development both as an engineer and a human being, I would have drifted by the wayside. I would like to thank my brothers and sisters Bobby, Calvin, Paul, Bob, Dawn, Pat, Mary, Peter, Cutts, Billy, Mag, Jim, Joanne, and of course Patty for all their love and support. For a beautiful family, Sunday dinners, all the love in the world, and their daughter, I thank Marty and Helen (Granny) Mehron. And ofcourse, who can forget Barbara. The two years I have known her have been the happiest years of my life. Without her unfailing love and support I might have ended up an automechanic. Department of Chemical Engineering Massachusetts Institute of Technology Cambridge, Massachusetts 02139 Professor Jack P. Ruina Secretary of the Faculty Massachusetts Institute of Technology Cambridge, Massachusetts 02139 Dear Professor Ruina: In accordance with the regulations of the Faculty, I herewith submit a thesis entitled, "Carbon Deposition in a Bosch Process Using a Cobalt and Nickel Catalyst", in partial fulfillment of the requirements for the degree of Doctor of Philosophy In Chemical Engineering at the Massachusetts Institute of Technology. Respectively submitted, James E. Garmirian Table of Contents 1. Summary ........................................................ 14 1.1 Experimental Apparatus ................................ 15 1.2 Approach ........................................ 16 1.3 Experimental Results .................................. 18 1.4 Discussion of the Equilibrium Results ................. 20 1.5 Application of Results ................................ 25 2. Literature Survey ............................................ 27 2.1 Previous Bosch Studies ................................ 28 2.1.1 CO-C0 2-Fe-Fe30 4 Equilibrium .................... 29 2.1.2 The Equilibrium of H2 ,CO, CO2 , CH4, and H2 0 with Iron and Iron Oxide .......................... 34 2.2 Nickel and Cobalt as Catalysts in the Bosch Process ... 39 2.2.1 Thermodynamics of the Ni-0 2 and Co-0 2 Systems .. 39 2.2.2 Thermodynamics of the H2 -CO-CH 4 -CO2 -H2 0-Carbon System ....................................... 44 2.2.2.1 Dent's Study of the Carbon-Gas Equilibrium ................................... 47 2.2.2.2 Rostrup-Nielsen's Study of the CO- C02-C and the CH4 -H2 -C Equilibrium ............. 53 2.2.2.3 Methane-Hydrogen Equilibrium Over Various Solid Phases ........................... 59 2.2.3 Carbon and Carbides ............................ 66 2.2.3.1 The Formation and Decomposition of Cobalt and Nickel Carbide ...................... 66 2.2.3.2 The Occurence of Carbides During Car- bon Formation ................................. 74 2.2.3.3 The Hydrogen Content of Carbon Formed Over Iron ........................... ......... 80 2.2.4 Carbon Fiber Formation Mechanism .............. .. 80 2.2.4.1 Dissolution-Diffusion Mechanisms for Filamentary Growth ............................ 80 2.2.4.2 Filamentary Growth through a Carbide Intermediate .................................. 96 2.2.4.3 The Importance of Surface Diffusion in Filamentary Growth ........................... 99 3. Apparatus and Procedure ...................................... 102 3.1 Experimental Apparatus .............................. 102 3.1.1 Feed-Gas Delivery System ....................... 102 3.1.2 Thermogravimetric Reactor ..................... 107 3.1.2.1 Preheater and Lower Reactor Support Tube ........................................... 107 3.1.2.2 Top Section Reactor Support Tube 107 109 3.1.2.3 Catalyst Assembly . ..... e.... 3.1.2.4 Furnace ........... 109 3.1.3 Gas Sampling System ........ ...... e... 111 3.2 Experimental Procedure ............ 114 3.2.1 Determination of Run Conditi ons ...... 114 114 3.2.2 Equipment Start-Up ......... .......... 3.2.3 Run Procedure .............. 115 115 3.2.4 Shut-Down Procedure ........ ............... .. .. ... , 117 Results and Discussion ..................... .oo... 4.1 Preliminary Experiments .... 117 ..io 117 4.2 Equilibrium Studies ........ ... 4.2.1 Bosch Equilibrium Studies 123 4.2.2 Equilibrium Studies at Var ious Compo- sitions and Temperatures ... 137 4.2.3 A Discussion of the Equili brium Re- sults ............................. ......... i.o. 151 4.4 Hydrogen Content of Carbons Formed Under Various Conditions ............................................ 171 Application of Results ......................................... 175 Conclusions ................................................... 184 Recommendations ................................................ 185 186 Appendix .............................. ......................... 8.1 Calculation of Equilibrium Gas Compositions ........... 186 8.2 Nomenclature ................. ................... ...... 188 8.3 Literature References ........ .......... ............... 190 Table of Figures 2-1 Phase Diagram for the Iron-Iron Oxide-Gas and Graphite-Gas Equilibria .. 31 2-2 Carbon Deposition from CO-CO 2 Mixtures (Manning,1976) .................. 32 2-3 Inhibition of Carbon Deposition by Fe30 4 at Various O/H Ratios (Sacco, 1977 ) ................................................................. 35 2-4 Determination of the Iron/Wustite Phase Boundary in a Five Component Gas Mixture at Various O/H Ratios (Sacco, 1977) ........................ 37 2-5 Percentage of Theoretical PH /PH Versus Experimental PH H .... 38 for Various O/H values
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