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An Investigation of Zinc Oxide Promotion of Skeletal Copper Catalysts for Methanol Synthesis and Water Gas Shift Reaction

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An Investigation of Zinc Oxide Promotion of Skeletal Copper Catalysts for Methanol Synthesis and Water Gas Shift Reaction AN INVESTIGATION OF ZINC OXIDE PROMOTION OF SKELETAL COPPER CATALYSTS FOR METHANOL SYNTHESIS AND WATER GAS SHIFT REACTION by Danmei Wang (BEng and MEng) A Dissertation submitted to the School of Chemical Engineering and Industrial Chemistry, The University of New South Wales in partial fulfilment of the Degree of Doctor of Philosophy The University of New South Wales July 1998 CANDIATE'S CERTIICATE This is to certify that the work presented in this thesis was carried out in the School of Chemical Engineering and Industrial Chemistry, The University of New South Wales, and has not been submitted previously to any other university or technical institution fora degree or award. SRPOI Form I WAVER The University of New South Wales Declaration Relating to Disposition of Project Report/Thesis This is to certify that r, being a candidate of the degree of amcyof the University relating i't-.D , to retention and used of higher degree project reports and theses, namely that the University retains the copies submitted for examination and is free to allow them to be consulted or borrowed. Subject to the provisions of the Copyright Act, 1968, the University may issue a project report or thesis or in part in Photostat or microfilmor other copying medium. [n the light of these provisions I grant the University Liberation Permission to publish, or to authorise the publication of my project report/thesis, in whole or in part. I also authorise the publication by University Microfilms of a 350 work abstract in Dissertation Abstracts International. Date_l_b_/ O_f�{ _I �-9�1� To my husband, Darren and sons, Elliott and Dan RESEARCH PAPERS AND PUBLICATIONS 1. D.Wang, D.G.Sizgek, H.E. Curry-Hyde (1993), "Raney Methanol Synthesis Catalysts Development for large Scale Application", Chemeca'93, Canberra, Australia. 2. D.Wang, L.Ma, C.Jiang, D. Trimm, M. Wainwright and D.Kim (1996), "The Effect of ZnO in Raney Cu Catalyst on Methanol Synthesis, Water Gas Shift and Methanol Steam Reforming Reactions", J.W.Hightower, W.N.Delgass, E.lglesia and A.T.Bell (Eds.), 11th International Congress on Catalysis-40th Anniversary, Studies in Surface Science and Catalysis, VlOl, PI379, Elsevier Science B.V. 3. D.Wang, D. Trimm and M.Wainwright, "The behaviour of H2 in Skeletal Cu/ZnO Catalysts: H2-TPD Study", To be submitted. ABSTRACT The synthesis of methanol from syngas (CO-H2-C02) over Cu/ZnO-based catalysts is an important industrial process and one of the most investigated catalytic reactions. Despite a number of mechanistic studies conducted over past decades, there is still considerable debate regarding the nature of active sites on the catalyst surface and the role of ZnO in promoting catalytic activity. The skeletal Cu/ZnO/ Alz03 catalysts used in this study of methanol synthesis were produced by leaching CuAh alloy using various concentrations of sodium zincate in 6.09M NaOH solution. It was found that high surface area catalysts can be achieved with high loadings of ZnO on the skeletal Cu catalyst surface. The selectivity of methanol from C02 is greatly improved with increasing ZnO contents. Detailed study of this preparation technique suggests that an increase the concentration of sodium zincate or a decrease in leaching temperature tends to retard the leaching rate and results in a decrease of the Cu crystallite size in the skeletal copper catalysts. It was confirmed that reprecipitation of Zn(OH)2 and Ah03 takes place on the leached material. The hydrogenation of C02 over skeletal Cu/ZnO catalysts was carried out to clarify the role of ZnO in the skeletal Cu -based catalysts for methanol synthesis. The skeletal Cu/ZnO catalysts produced using caustic leaching were loaded with precipitated zinc oxide using a novel preparation technique. The resulting catalysts maintained approximately the same surface area as the unpromoted catalyst with varying coverage of copper surface by zinc oxide. The catalysts contained a very small Ah03 residue (approximately at 1.3 wt¾). The skeletal Cu/ZnO/Ah03 catalysts were used the study in the hydrogenation of C02. The experimental results clearly indicated that the activity of methanol synthesis over these catalysts increases with an increase of zinc oxide content, while activity of the reverse water gas shift reaction decreases thereby improving the selectivity for methanol synthesis from C02. These results can be explained in terms of a model in which synergy between copper and zinc oxides relates to formation of H atoms on copper followed by their migration to zinc oxide. Hydrogen TPD studies have been carried out on the skeletal Cu catalysts and skeletal Cu catalysts modified by the precipitation of zinc oxide. The experimental results show that there were three H2 desorption peaks for skeletal Cu/ZnO catalysts, at 343- 393 K, 473-493K and 573-593 K. There was evidence that increasing ZnO content in skeletal Cu catalysts enhanced H2 adsorption and created a new H2 desorption spectrum in the temperature range 473-493 K. The H2 desorption site in the temperature range 473-493 K, created by ZnO loading, may be correlated to the promotion of catalytic activity for methanol synthesis at 493-513 K. II ACKNOWLEDGMENTS The author wishes to express her gratitude to all of the people who made contribution to the completion of this thesis. In particular, she is greatly indebted to: Her supervisors, Professors Mark S. Wainwright and David L. Trimm for making it possible to do these studies, for their constant encouragement, guidance, great patience and understanding. Professor Dong Hyun Kim, Department of Chemical Engineering, Kyung Pook University, Taegu, Korea, for his inspiration help and advice particularly with sharing his knowledge on the technical aspects of reactor technology. The school's technical staff, especially Miss J.Steer for the XRD measurement, Mr.P.McCauley and Mr. J.Starling for their technical assistance. All fellow postgraduates, especially Judy Greenwood, Scott Buckingham, Ken Ng, Jason Scott, Donia Beydoun, for their valued friendship and assistance. The University of New South Wales and Australian Government, for financial support through a scholarships. Finally my parents, for their patience, understanding, encouragement and for sacrificing so much to allow me to complete my studies. III TABLE OF CONTENTS Page ABSTRACT iii ACKNOWLEDGEMENTS V TABLE OF CONTENTS Vi LIST OF TABLES Vi LIST OF FIGURES X Chapter 1 Introduction 1 Chapter2 Literature Review 7 2.1 Introduction 7 2.2 Recent Development In Cu-Based Methanol 8 Synthesis Catalyst 2.2.1 Introduction 8 2.2.2 Characterisation of catalyst 9 2.2.2.1 Bulk Properties 9 2.2.2.2 Surface Properties 14 (A) Chemical Analysis 15 (B) Adsorption Studies 18 2.2.3 Activity of CuZnO/Al203 Catalysts 22 2.2.3.1 Effect of Nominal Phase Composition of the Precursor 2.2.3.2 Interface in the Cu/ZnO System 2.2.4 Mechanism of Methanol Synthesis 27 2.3 Water Gas Shift Reaction 31 2.3.1 Catalyst Characterisation 31 2.3.2 Mechanism Studies 36 2.3.2.1 The Redox Mechanism 2.3.2.2 The Associative Mechanism 2.4 Skeletal Copper-Zinc Oxide Catalysts for Methanol 42 Synthesis and Water Gas Shift Reaction 2.4.1 Introduction 42 2.4.2 Catalyst Preparation 43 2.4.2.1 Development of Skeletal Metal Catalyst 43 2.4.2.2 Precursor Alloys 45 2.4.2.3 Studies of Leaching and Leaching Kinetic 49 (A) Leaching Cu-Al Alloy (B) Leaching Cu-AI-Zn Alloy (C) Leaching Kinetic IV 2.4.3 Characterisation of ZnO Promoted Skeletal Cu Catalysts 54 2.4.3.1 Physical and Chemical Properties 54 2.4.3.2 Mechanism of Methanol Synthesis and Water-Gas Shift Reaction over ZnO Promoted Skeletal Copper Catalysts 56 2.4.3.3 Water Gas Shift Reaction 63 Chapter3 Objectives 65 Chapter4 Experimental Techniques 67 4.1 Materials 67 4.1.1 Gases 67 4.1.2 Chemicals 67 4.2 Catalyst Preparation 69 4.2.1 Leachant 70 4.2.2 Leaching Process 70 4.2.3 Impregnation Method 72 4.3 Catalyst Activity Testing 73 4.3.1 Apparatus for Catalyst Testing 73 4.3.2 Catalyst Testing Procedures 76 4.3.3 Product Analysis 76 4.3.4 Processing of Data 78 4.4 Characterisation of Catalyst 81 4.4.1 Bulk Characterisation 81 4.4.1.1 Atomic Absorption Spectroscopy 4.4.1.2 X-ray Diffraction Analysis 4.4.1.3 Bulk Density 4.4.2 Surface Characterisation 84 4.4.2.1 Total BET Surface Area Measurement 85 4.4.2.2 Cu surface Area Measurement 89 4.4.2.3 Temperature Programmed Desorption 92 Chapter5 Initial Studies of Copper Surface Area and of Possible Mass Transf er Limitations 94 5.1 Copper Surface Area Measurement 94 5.1.1 Introduction 94 5.1.2 Experimental Technique 96 5.1.3 Results and Discussion 97 5.1.3.1 The Effect of ZnO on the Surface Area Measurement 97 5.1.3.2 Effect of Pretreatment on the Copper Surface Area Measurement 99 5.1.4 Conclusion 100 V 5.2 Possible Mass Transfer Limitation During Activity Measurement 101 5.2.1 Introduction 101 5.2.2 Results and Discussion 102 5.2.3 Conclusions 106 Chapter 6 Activities And Surface Structure Development Of Skeletal 107 Cu-ZnO catalyst Prepared By Sodium Zincate Leaching. 6.1 Introduction 107 6.2 Experimental 108 6.2.1 Preparation of Catalyst 108 6.2.2 Characterisation of Catalyst 108 6.2.3 Activity Measurement 109 6.2.4 Stability Test 110 6.2.5 Blank Test 111 6.3 Results and Discussion 111 6.3.1 Effect of Zincate concentration and Leaching Temperature 111 6.3.2 Structure Development During the Leaching Processes 117 6.3.3 Activity and Selectivity of Methanol Synthesis andRWGS 125 6.4 Conclusions 132 Chapter 7 The Role Of Zinc Oxide On Skeletal Cu Catalyst In Methanol Synthesis And Reverse Water Gas Shift 133 Reactions
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