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Study of Catalyst Deactivation in Three Different Industrial Processes Study of Catalyst Deactivation in Three Different Industrial Processes Acta Wexionensia No 106/2007 Chemical Engineering/Bioenergy Technology Study of Catalyst Deactivation in Three Different Industrial Processes Ann-Charlotte Larsson Växjö University Press Study of Catalyst Deactivation in Three Different Industrial Processes. The- sis for the degree of Doctor of Technology, Växjö University, Sweden 2007. Series editors: Tommy Book and Kerstin Brodén ISSN: 1404-4307 ISBN: 978-91-7636-533-5 Printed by: Intellecta Docusys, Göteborg 2007 Abstract Larsson, Ann-Charlotte (2007). Study of Catalyst Deactivation in Three Different Industrial Processes, Acta Wexionensia No 106/2007. ISSN: 1404-4307, ISBN: 978-91-7636-533-5. Written in English. Deactivation of catalysts were investigated focusing on three industrial proc- esses: 1) Selective Catalytic Reduction (SCR) for abatement of NOx from bio- mass combustion using V2O5-WO3/TiO2 catalysts; 2) Catalytic oxidation of vola- tile organic compounds (VOC) from printing industries using a Pt/γ-Al2O3 cata- lyst; and 3) Ni and Pt/Rh catalysts used in steam reforming reaction of bio- syngas obtained from biomass gasification. The aim has been to simulate industrial conditions in laboratory experiments in order to comprehend influence of compounds affecting catalysts performance. Typical catalyst lifetimes in industrial processes are several years, which are a challenge when accelerating deactivation in laboratory scale experiments where possible exposure times are few hours or days. Catalysts can be introduced to deactivating compounds through different routes. The first method examined was gaseous exposure, which was applied to deactivate VOC oxidation catalyst through exposure of gaseous hexamethyldisiloxane. The second method involved wet impregnation and was used for impregnation of SCR catalyst with salt solu- tions. The third method was based on exposure and deposition of size selected particles of deactivating substances on the catalyst. The latter device was devel- oped during this work. It was applied to monolithic SCR catalysts as well as to pellet catalysts intended for steam reforming of biomass gasification syngas. De- activated SCR catalyst samples by size selected exposure method were verified and compared with SCR catalysts used in a commercial biomass boiler for 6 500 h. Evaluations of fresh and deactivated samples were investigated using BET surface area; chemisorption and temperature programmed desorption (TPD); sur- face morphology using Scanning Electron Microscopy (SEM) and poison pene- tration profile through SEM with an Electron Micro Probe Analyser (EMPA) also equipped with a energy dispersive spectrometer (EDS); chemical analysis of accumulation of exposed compounds by Inductively Coupled Plasma - Atomic Emission Spectroscopy (ICP-AES); and influence on catalyst performance. The size selected generated particles of deactivating substances were characterized with respect to mean diameter and number size distribution through Scanning Mobility Particle Sizer (SMPS) and mass size distribution applying an Electric Low Pressure Impactor (ELPI). Results from catalyst characterization methods were useful tools in evaluation of catalyst deactivation routes. Understanding deactivation processes and impact on catalyst performance is vital for further optimization of catalysts with respect to performance and life- time. Further research in this field can provide more resistant catalysts for appli- cation in industry leading to higher commercial benefits and further application of environmental catalysts in thermo-chemical conversion of biomass. Key words: deactivation; catalyst; SCR; VOC; steam reforming; aerosol particle; potassium; zinc; ash salts; biomass; organosilicon; qç=lä~I=gç~âáã=~åÇ=^äÉñ~åÇÉê= = List of Papers This thesis is based on the following papers appended in the thesis. They are re- ferred to in the text by their Roman numerals: I Deactivation of SCR Catalysts by Exposure to Aerosol Parti- cles of Potassium and Zinc Salts Ann-Charlotte Larsson, Jessica Einvall and Mehri Sanati Accepted for publication in Aerosol Science and Technology (Dec 2006) II Targeting by Comparison with Laboratory Experiments the SCR Catalyst Deactivation Process by Potassium and Zinc Salts in a Large Scale Biomass Combustion Boiler Ann-Charlotte Larsson, Jessica Einvall, Arne Andersson and Mehri Sanati Energy & Fuels (2006) 20, 1398-1405 III Physical and Chemical Characterisation of Potassium Deac- tivation of a SCR Catalyst for Biomass Combustion Ann-Charlotte Larsson, Jessica Einvall, Arne Andersson and Mehri Sanati in Proceedings 12th Nordic Symposium on Catalysis Confer- ence, Trondheim, Norway, May 28-30, 2006, (P51, p 198) Accepted for publication in a special issue of Topics of Catalysis (Dec 2006) IV Pilot-Scale Investigation of Pt/Alumina Catalysts Deactiva- tion by Organosilicon in the Total Oxidation of Hydrocar- bons Ann-Charlotte Larsson, Mohammad Rahmani, Karl Arnby, Morteza Sohrabi, Magnus Skoglundh, Neil Cruise, and Mehri Sanati in Proceedings 12th Nordic Symposium on Catalysis Confer- ence, Trondheim, Norway, May 28-30, 2006, (O24, p 82) Accepted for publication a special issue of in Topics of Catalysis (Dec 2006) 1 V Investigation of Reforming Catalyst Deactivation by Expo- sure to Fly Ash from Biomass Gasification in Laboratory Scale Jessica Einvall, Simone Albertazzi, Christian Hulteberg, Fran- cesco Basile, Ann-Charlotte Larsson, Jan Brandin and Mehri Sanati Submitted for publication in Energy & Fuels VI Comparison of Deactivated Catalysts in Laboratory and Large Scale Biomass Combustion Focussing on Potassium and Zinc Salts Ann-Charlotte Larsson, Mikael Strand, Simone Albertazzi, Francesco Basile and Mehri Sanati Submitted for publication in Applied Catalysis A: General Results related to this thesis are also presented in: Developing a Method to Deactivate a V2O5-WO3/TiO2 Mono- lithic Catalyst by Aerosol Salts Ann-Charlotte Larsson, Jessica Einvall, Mehri Sanati, Poster presentation at European Aerosol Conference, Ghent, Belgium, August 30-September 1, 2005, p 665, ISBN 90-8091- 5939 Environmental Catalyst for Abatement of NOx from Bio- mass Boilers Ann-Charlotte Larsson, Jessica Einvall, Mehri Sanati, Oral presentation at Swedish Finnish Flame Days, October 18- 19, 2005, 176-184, ISBN 91-7178-185-4 Deactivation of Catalysts for Reforming of Gas from Biomass Gasification by Exposure to Aerosol Particles Jessica Einvall, Simone Albertazzi, Christian Hulteberg, Fran- cesco Basile, Ann-Charlotte Larsson, Eva Gustafsson, Jan Brandin, Ferruccio Trifirò and Mehri Sanati Poster presentation at 12th Nordic Symposium on Catalysis Con- ference, Trondheim, Norway, May 28-30, 2006, (P18, p 132) ISBN 82-9955-69-1-0 2 List of Contents Introduction........................................................................................................... 5 Catalyst Deactivation................................................................................ 5 Deactivation in Industrial Processes......................................................... 6 Selective Catalytic Reduction (SCR) in Biomass Combustion................. 6 Deactivation of VOC Oxidation Catalyst ................................................. 7 Steam Reforming Catalyst Applied to Product Gas of Biomass Gasification............................................................................................... 8 Simulation of Catalyst Deactivation in Laboratory Scale....................... 10 Scope of Work........................................................................................ 10 Experimental....................................................................................................... 13 Exposure to Generated Poisons .............................................................. 13 Catalyst Reactor Configuration .............................................................. 13 Particle Generation and Deposition Process........................................... 14 Gaseous Exposure Process ..................................................................... 17 Wet Impregnation of Catalyst Samples by Poisons................................ 18 Commercial Deactivation of Catalyst Samples ...................................... 19 Characterisation .................................................................................................. 21 Catalyst Characterisation........................................................................ 21 Physical Characterisation of Catalyst Samples (BET)............................ 21 Chemisorption ........................................................................................ 21 Surface Analysis of Catalyst Samples .................................................... 22 Poison Penetration Profile ...................................................................... 23 Chemical Analysis.................................................................................. 23 Physical Characterisation of Generated Particles ................................... 24 Scanning Mobility Particle Sizer (SMPS) .............................................. 24 Tandem Differential Mobility Analyser (TDMA).................................. 25 Electric Low Pressure Impactor (ELPI).................................................. 26 Catalyst Performance.............................................................................. 28 SCR Catalyst Activity Measurement...................................................... 28 VOC Catalyst Activity Measurement....................................................
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