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Bioleaching of Chalcopyrite

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Bioleaching of Chalcopyrite Bioleaching of chalcopyrite By Woranart Jonglertjunya A thesis submitted to The University of Birmingham For the degree of DOCTOR OF PHILOSOPHY Department of Chemical Engineering School of Engineering The University of Birmingham United Kingdom April 2003 University of Birmingham Research Archive e-theses repository This unpublished thesis/dissertation is copyright of the author and/or third parties. The intellectual property rights of the author or third parties in respect of this work are as defined by The Copyright Designs and Patents Act 1988 or as modified by any successor legislation. Any use made of information contained in this thesis/dissertation must be in accordance with that legislation and must be properly acknowledged. Further distribution or reproduction in any format is prohibited without the permission of the copyright holder. Abstract This research is concerned with the bioleaching of chalcopyrite (CuFeS2) by Thiobacillus ferrooxidans (ATCC 19859), which has been carried out in shake flasks (250 ml) and a 4-litre stirred tank bioreactor. The effects of experimental factors such as initial pH, particle size, pulp density and shake flask speed have been studied in shake flasks by employing cell suspensions in the chalcopyrite concentrate with the ATCC 64 medium in the absence of added ferrous ions. The characterisation of T. ferrooxidans on chalcopyrite concentrate was examined by investigating the adsorption isotherm and electrophoretic mobility. Subsequently, a mechanism for copper dissolution was proposed by employing relevant experiments, including the chemical leaching of chalcopyrite by sulphuric acid and ferric sulphate solutions, bioleaching of chalcopyrite in the presence of added ferric ions, and cell attachment analysis by scanning electron microscopy. Following the above, the work then focused on the bioleaching of the chalcopyrite concentrate in a stirred tank bioreactor for the purpose of scaling up, and investigated the effects of agitation speeds. Finally, the bioleaching of low-grade copper ores has been briefly studied. The results show that the rate of copper dissolution has a positive relationship with bacterial growth, particularly with respect to bacterial attachment, which has an important role based on adsorption isotherm and scanning electron microscopy studies. However, it is not only bacteria that play an important role in copper dissolution; also the strength of sulphuric acid can influence copper solubility. For example, copper dissolution can be achieved using a sulphuric acid solution of pH 1.5, giving a concentration of about 1 g/l copper after 25 days. The results obtained from the adsorption isotherm of T. ferrooxidans and the electrophoretic mobility of chalcopyrite particles before and after interaction with each other has proved the fact that the changes in surface chemistry occurred when bacterial interactions on the mineral surface took place. Furthermore, agitation speed have a significant influence on cell growth, metal dissolution and cell adsorption ratio when carried out in shake flasks and a stirred tank bioreactor. The bioleaching results for different shake flask speeds (i.e. 100, 200 and 300 rpm) in shake flasks displayed that shake flask speed above 100 rpm was detrimental to bacterial growth and thus copper dissolution. For the bioreactor experiments, agitation was performed within a rotor speed range of 50, 100, 150 and 200 rpm. A rotor speed of 150 rpm represents the most suitable conditions for bacterial growth and the percent extraction of copper dissolution amongst those considered. In conclusion, the concentration of copper dissolution for all pulp densities reached its maximum at a concentration of 4.8 ± 0.2 g/l after 30 days leaching time. This indicted that copper dissolution has a limited solubility; this may be because the chalcopyrite particle surface was covered by mineral and bacterial deposits over the period of bioleaching time as described in the SEM analysis of the bioleaching surface. Finally, this work attempted to extract copper from a low-grade ore using bioleaching techniques. However, initial bioleaching tests proved that T. ferrooxidans could not leach copper and iron from the low-grade copper ores due to the chemical composition of the gangue minerals (mainly carbonates). This is due to the neutralising action of carbonates, which create an environment in which the pH is too high for the acidophilic bacteria to grow. Acknowledgements I would like to express my thanks to my supervisors, Dr. Neil Rowson and Dr. Caroline McFarlane for their guidance, encouragement, support and invaluable help throughout this project. I would also like to thank H. Jennings, E. Mitchell, D. French and P. Plant for their technical assistance, as well as L. Draper for her clerical assistance. I would also like to thank my colleagues for their comments, cheerfulness and friendship. I would also like to express my thanks to Dimitra, Fosco, Anya, Frank, Eng Seng for their unstinting and enjoyable friendship. Special thanks also go to my parents, T. Jonglertjanya and S. Sapayatosok, for their unconditional love and support. Finally, I would like to thank my sister, Fon, for her understanding, patience and love. Table of Contents LIST OF FIGURES i LIST OF TABLES vi CHAPTER 1 INTRODUCTION 1 1.1 Copper extraction 1 1.2 Bioleaching 3 1.3 Motivation for the research 9 1.3.1 Selecting T. ferrooxidans 9 1.3.2 Bioleaching of chalcopyrite 11 1.3.3 Research on the bioleaching of chalcopyrite 12 1.3.4 Industrial relevance 13 1.4 Aims and objectives 15 1.5 Layout of thesis 15 CHAPTER 2 LITERATURE REVIEW 17 2.1 Microorganisms in bioleaching processes 17 2.1.1 Thiobacillus 19 2.1.2 Leptospirillum 21 2.1.3 Thermophilic bacteria 22 2.1.4 Heterotrophic microorganisms 23 2.2 Thiobacillus ferrooxidans 24 2.2.1 Characteristics and physiology 24 2.2.2 Energy consideration 26 2.3 The general mechanisms of bioleaching 28 2.4 Factors affecting bacterial leaching 37 2.4.1 Type of microorganisms 38 2.4.2 The type of mineral ores 40 2.4.3 Medium 42 2.4.4 Temperature 44 2.4.5 pH 45 2.4.6 Particle size 46 2.4.7 Pulp density 46 2.4.8 Oxygen and carbon dioxide 47 2.4.9 Conclusion 48 CHAPTER 3 FACTORS AFFECTING BACTERIAL LEACHING ON SHAKE FLASK CULTURES OF T. ferrooxidans 49 3.1 Introduction 49 3.2 Materials and methods 50 3.2.1 Chalcopyrite concentrate 50 3.2.2 Microorganism and media 53 3.2.3 Bacterial preparation 53 3.2.4 Analysis of the solution pH, the redox potential and the free cell concentration 54 3.2.5 Analysis of the copper and iron concentration 55 3.2.6 Experimental procedure 55 3.3 Effect of shake flask speed on bioleaching of chalcopyrite 57 3.3.1 Introduction 57 3.3.2 Effect of shake flask speed on bacterial growth 58 3.3.3 Effect of shake flask speed on the solution pH and the redox potential 67 3.3.4 Effect of shake flask speed on metal dissolution 69 3.3.5 Control experiments 70 3.3.6 Conclusion 72 3.4 Effect of particle size on the bioleaching of chalcopyrite 75 3.4.1 Introduction 75 3.4.2 Effect of particle size fractions on bacterial growth 77 3.4.3 Effect of particle size range of chalcopyrite on solution pH 82 3.4.4 Effect of particle size on metal dissolution 83 3.4.5 Conclusion 83 3.5 Effect of initial pH on bioleaching of chalcopyrite 86 3.5.1 Introduction 86 3.5.2 Effect of initial pH on bacterial growth 88 3.5.3 Effect of initial pH on the solution pH and redox potential 93 3.5.4 Effect of initial pH on metal dissolution 94 3.5.5 Conclusion 100 3.6 Effect of pulp density on bioleaching of chalcopyrite 101 3.6.1 Introduction 101 3.6.2 Effect of pulp density on bacterial growth 103 3.6.3 Effect of pulp density on the solution pH 105 3.6.4 Effect of pulp density on metal dissolution 105 3.6.5 Conclusion 109 CHAPTER 4 THE CHARACTERISATION OF T. ferrooxidans ON CHALCOPYRITE CONCENTRATE 110 4.1 Introduction 110 4.2 Adsorption isotherm 111 4.2.1 Introduction 111 4.2.2 Experimental procedure 112 4.2.3 Results and discussion 113 4.3 Electrophoretic mobility 117 4.3.1 Introduction 117 4.3.2 Experimental procedure 117 4.3.2.1 Particle preparation 117 4.3.2.2 Buffer preparation 119 4.3.3 Results and discussion 120 4.4 Conclusion 126 CHAPTER 5 MECHANISM OF COPPER DISSOLUTION IN FLASK CULTURES OF Thiobacillus ferrooxidans 127 5.1 Introduction 127 5.2 Chemical leaching: sulphuric acid and ferric sulphate solutions 128 5.2.1 Introduction 128 5.2.2 Experimental procedure 131 5.2.2.1 Sulphuric acid leaching 131 5.2.2.2 Ferric sulphate leaching 131 5.2.3 Results and discussion 132 5.2.3.1 Sulphuric acid leaching 132 5.2.3.2 Ferric sulphate leaching 137 5.3 Effect of ferric sulphate on bioleaching 141 5.3.1 Introduction 141 5.3.2 Materials and methods 141 5.3.2.1 Inoculum preparation procedure 141 5.3.2.2 Experimental procedure 142 5.3.2 Effect of initial ferric sulphate on bacterial growth, the solution pH and the redox potential 143 5.3.4 Effect of initial ferric ions on metal dissolution 150 5.3.5 Control experiments 151 5.4 Scanning electron microscope (SEM) 153 5.5 Conclusion 157 CHAPTER 6 BIOLEACHING OF THE CHALCOPYRITE CONCENTRATE IN A 4L STIRRED TANK BIOREACTOR 159 6.1 Introduction 159 6.2 Materials and methods 162 6.2.1 Bioreactor 162 6.2.2 Experimental procedure 163 6.2.2.1 Preparation of inoculum 163 6.2.2.2 Calibration of pH probe, dissolved oxygen probe and temperature probe 164 6.2.2.3 Preparation of bioleaching of the chalcopyrite concentrate 165 6.2.2.4 Preparation of T.
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