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Jessy Ju Lian, Lee PROCESS INTENSIFICATION OF NITROUS GAS ABSORPTION A thesis submitted in fulfilment of the requirements for the degree of Doctor of Philosophy By Jessy Ju Lian, Lee School of Chemical and Biomolecular Engineering The University of Sydney AUSTRALIA April 2012 Declaration I hereby declare that the work presented in this thesis is solely my own work. To the best of my knowledge, the work presented is original except where otherwise indicated by reference to other authors. No part of this work has been submitted for any other degree or diploma. __________________________ Jessy Ju Lian, Lee April 2012 i Acknowledgements My foremost gratitude goes to my supervisor Professor Brian S. Haynes. I would like to thank him for his guidance, patience and encouragement, and for his insights and suggestions that helped shape my research skills. I would not have learnt as much as I had if not for him. I am also truly grateful to Dr. David O. Johnson, whose constant professional and moral support has helped me immensely throughout my Phd journey. Special thanks also go out to Dr. Dean Chambers for assisting with the experimental setup during the initial stages of this project. I am also appreciative towards Adjunct Professor David F. Fletcher for all the help that he has given me, especially his assistance with the mathematical model. I would like to thank Orica Mining Services for taking me on this project, and Dr. Richard Goodridge, Dr. John Lear and Dr. Johann Zank for their continuous support and encouragement. I am also grateful to the Australian Federal Government for the funding of the Australian Postgraduate Award scholarship. I wish to thank the staff of the School of Chemical and Biomolecular Engineering: Dr. Jeffrey Shi, Linda Wang, Garry Towell and Alex Farago for aiding with the experimental setup; Dr. Ali Abbas, Dr. Alejandro Montoya and Carlos Moreno for their technical support; and Clara Spencer and Marta Kremky for their administrative support. I would also like to thank the fellow postgraduate students, especially Dr. Xavier Traversac, Dr. Yang Liu, Dr. Ryan Zhou, Dr. Raghvendra Gupta and Azadeh Najafi Asadolahi for their kind assistance and wise guidance throughout my Phd. I have been extremely fortunate to have the support, companionship and constant encouragement of very special friends to whom I am truly grateful: Maximilian Warner, Jason Mann and Sergio Londono. Their presences and fun-loving spirits have made this whole experience a truly memorable one. Last but not least, words cannot express the full gratitude I have towards my beloved parents and husband Greig Kurniawan for always being there when I needed them most, and for their continuous support, love, patience and guidance throughout all these years. ii Table of Contents DECLARATION...................................................................................................................... I ACKNOWLEDGEMENTS ................................................................................................... II TABLE OF CONTENTS ..................................................................................................... III LIST OF FIGURES ........................................................................................................... VIII LIST OF TABLES ............................................................................................................. XVI ABSTRACT ....................................................................................................................... XVII NOMENCLATURE ............................................................................................................. XX 1 INTRODUCTION............................................................................................................ 1 2 LITERATURE REVIEW ............................................................................................... 3 2.1 Introduction ...................................................................................................................... 3 2.2 Nitric Acid......................................................................................................................... 3 2.2.1 Properties ................................................................................................................... 3 2.2.2 Uses ............................................................................................................................ 3 2.2.3 Industrial Production .................................................................................................. 4 2.3 Oxidation and Absorption of Nitrogen Oxides ............................................................. 9 2.3.1 Mechanism ................................................................................................................. 9 2.3.2 Chemical Kinetics and Equilibria ............................................................................ 11 2.3.3 Mass Transfer ........................................................................................................... 15 2.4 Process Intensification for the Absorption of Nitrogen Oxides ................................. 16 2.4.1 Process Intensification ............................................................................................. 16 2.4.2 High Pressure Absorption ........................................................................................ 18 2.4.3 Absorption under High Oxygen Partial Pressures ................................................... 19 2.4.4 Process Intensification via Miniaturisation .............................................................. 20 2.5 Conclusion ...................................................................................................................... 23 3 EXPERIMENTAL SETUP AND PROCEDURE ....................................................... 24 3.1 Experimental Setup ....................................................................................................... 24 3.2 Acid sampling ................................................................................................................. 29 3.3 Analytical Measurements .............................................................................................. 30 iii 3.3.1 Infrared Spectroscopy .............................................................................................. 30 3.3.2 Ion Chromatography ................................................................................................ 34 3.4 Analytical Methods ........................................................................................................ 37 3.4.1 Titrimetric Analysis ................................................................................................. 37 3.5 Data evaluation............................................................................................................... 38 3.6 Comparison between Methods of Analysis .................................................................. 40 4 EXPERIMENTAL RESULTS AND PRELIMINARY DISCUSSION .................... 42 4.1 Introduction .................................................................................................................... 42 4.1.1 Experimental Conditions ......................................................................................... 42 4.1.2 Disproportionation of Nitrous Acid ......................................................................... 43 4.1.3 Collection into Empty Container ............................................................................. 46 4.1.4 Collection into Water ............................................................................................... 48 4.2 Effects of Nominal Residence Time .............................................................................. 51 4.3 Effects of Steam / Diluent Partial Pressure ................................................................. 53 4.4 Effects of System Pressure ............................................................................................ 58 4.5 Effects of Nitric Oxide Partial Pressure ....................................................................... 61 4.6 Effects of Gas Velocity ................................................................................................... 62 4.7 Effects of Reactor Diameter .......................................................................................... 63 4.8 Effects of Reactor Configuration .................................................................................. 64 4.9 Effects of Oxygen Partial Pressure ............................................................................... 65 4.10 Cooling water ............................................................................................................. 67 4.10.1 Water flow rate .................................................................................................... 67 4.10.2 Water temperature ................................................................................................ 68 4.11 First-Order Kinetics .................................................................................................. 69 4.12 Conclusion .................................................................................................................. 71 5 KINETIC MODELLING AND METHODOLOGY .................................................. 72 5.1 Kinetic Modelling and Model Implementation ........................................................... 72 5.1.1 Kinetic Modelling
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