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DOCTORAL THESIS Chalcopyrite (Bio)Leaching in Sulphate Solutions

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DOCTORAL THESIS Chalcopyrite (Bio)Leaching in Sulphate Solutions DOCTORAL T H E SIS Department of Civil, Environmental and Natural Resources Engineering Division of Minerals and Metallurgical Engineering Mohammad Khoshkhoo Chalcopyrite (Bio)leaching in Sulphate Solutions ISSN 1402-1544 Chalcopyrite (Bio)leaching in Sulphate Solutions ISBN 978-91-7583-507-5 (print) ISBN 978-91-7583-508-2 (pdf) An Investigation into Hindered Dissolution with Luleå University of Technology 2016 a Focus on Solution Redox Potential Mohammad Khoshkhoo Process Metallurgy Chalcopyrite (Bio)leaching in Sulphate Solutions An Investigation into Hindered Dissolution with a Focus on Solution Redox Potential Mohammad Khoshkhoo Division of Minerals and Metallurgical Engineering Department of Civil, Environmental and Natural Resources Engineering Luleå University of Technology SE– 971 87 Luleå Sweden February 2016 Printed by Luleå University of Technology, Graphic Production 2015 ISSN 1402-1544 ISBN 978-91-7583-507-5 (print) ISBN 978-91-7583-508-2 (pdf) Luleå 2016 www.ltu.se Abstract Chalcopyrite (CuFeS2) is the most abundant and the most economically important copper mineral. Increasing worldwide demand for copper accompanied by exhaustion of copper resources necessitate the development of new processes for treating lower–grade copper ores. Heap (bio)leaching of copper oxides and secondary sulphides (covellite (CuS) and chalcocite (Cu2S)) is a proven and convenient technology. However, chalcopyrite is recalcitrant to leaching and bioleaching in conventional leaching systems in sulphate media. Slow dissolution of chalcopyrite is attributed to the formation of compounds on the surface of the mineral during its dissolution and is often termed “passivation” or “hindered dissolution”. There is still no consensus about the nature of the passivation layer. There are, however, four proposed candidates suggested in the literature: metal deficient sulphides, polysulphides, jarosite and elemental sulphur. This project aimed to further investigate the chalcopyrite dissolution and its passivation under strictly controlled redox potential conditions. Leaching experiments of aged and fresh chalcopyrite concentrates under identical conditions gave a significant lower copper dissolution form the aged concentrate. The common understanding of reductive leaching mechanism (i.e. higher recoveries at lower redox potentials) was not valid for aged concentrates as they gave steadily increasing recoveries with increased redox potential. The hindering effect exerted from atmospheric oxidation products on the surface of the aged concentrates was responsible for this behaviour. Reductive leaching mechanism would be beneficial in the presence of an active galvanic interaction. In addition, the effect of initial copper concentration had no significant effect on the leaching rates. Redox potential development during moderately thermophilic bioleaching experiments of a pyritic chalcopyrite concentrate and a relatively pure chalcopyrite concentrate were chemically/electrochemically mimicked in the absence of microorganisms. Copper recoveries in the absence and presence of microorganisms were similar. In some abiotic experiments, jarosite precipitated due to a control loss of the redox potential. However, presence of bulk jarosite did not hamper the copper recovery compared to the bioleaching experiments where there was no bulk jarosite formation. Biooxidation of elemental sulphur did not have a positive effect on the leaching behaviour compared to the abiotic experiments where bulk elemental sulphur accumulated. Isotopic fractionations of copper and iron during the bioleaching and abiotic experiments showed that regardless of presence or absence of I microorganisms, the isotope fractionations followed a similar trend and that such analyses could be used in natural systems as an indicator of the oxidation extent. Surface analyses using X–ray photoelectron spectroscopy (XPS) measurements on massive chalcopyrite samples leached for different durations, revealed persistent presence of iron– oxyhydroxides and elemental sulphur on the surface. The elemental sulphur on the sample surfaces was rigidly bound such that it did not sublimate in the ultra–high vacuum environment of the XPS spectrometer at room temperature. Surface jarosite was observed in only one sample but no correlation between its presence and the hindered leaching could be made. It is proposed that iron–oxyhydroxides are the main precursor of chalcopyrite hindered dissolution in sulphate media where their inevitable formation entraps surface elemental sulphur resulting in a consolidated phase on the surface. It was shown that when suitable conditions are met, high copper recoveries can be obtained before the surface is finally hindered. II Acknowledgments I wish to acknowledge the financial support from the Swedish Research Council Formas (contract number 229–2009–657). Boliden Mineral AB is highly appreciated for providing financial support, the mineral samples and the automatic redox potential control system. I would like to express my deep gratitude to Prof. Åke Sandström, my research supervisor, for his patient guidance, enthusiastic encouragement and useful critiques in educating me. He is not only an excellent supervisor, but also a very good friend whose office door is always open for a chat. I will never be able to thank him properly. His generous support and willingness to give his time made it much easier than it could have been. My co–supervisor Prof. Mark Dopson is greatly appreciated for his professionalism and perspective. He always had novel ideas and wise tips which became extremely constructive in development of this thesis. His invaluable assistance in language correction of the papers is highly appreciated. Andrei Shchukarev hosted me very kindly when I was at Umeå University. He was also extremely efficient in running the XPS and much credit for the XPS results should go to him. I like to extend my gratitude to Prof. Bo Björkman and Prof. Caisa Samuelsson, the ex–head and the current head of our group, whose friendly and broad– minded attitude made an environment in which it was so easy to stay focused and enjoy working. Dr. Andreas Lennartsson and Dr. Fredrik Engström had helped me a lot to run the SEM. They are great colleagues and friends whose presence in the division makes a real difference. I am also sincerely grateful to Boliden employees, Dr. Nils–Johan Bolin and Jan– Eric Sundkvist, for the fruitful discussions I had with them time to time. Rolf Danielsson and his team in pilotverket (Boliden) are acknowledged for the construction of the electrochemical cell. I have to also appreciate their hospitality for the period I was working there. Dr. Nathalie Pérez Rodríguez is acknowledged for her inspiring input in our joint paper. On the personal front, I have a long list of people to thank: My present and former colleagues in the division for their support, feedback and friendship. Ehsan, Sara, Roland, Saeid, Matthias, Saman and Sepehr as well as many other friends who I cannot list here, simply due to lack of space, will always be a part of my memories for the great moments we had spent with each other during the last few years. You all mean a lot to me. Pouyeh and Aneseh, my wonderful sisters, and Vahid, my brother in law, have been always a huge support and a source of inspiration in my life. And finally my mom and dad, my foundation, whom without unconditional support and love I could not stand where I am standing today. This thesis is dedicated to them. III IV List of papers I. Mohammad Khoshkhoo, Mark Dopson, Andrey Shchukarev and Åke Sandström, “Electrochemical simulation of redox potential development in bioleaching of a pyritic chalcopyrite concentrate”, Hydrometallurgy 144–145 (2014), p 7–14. II. Mohammad Khoshkhoo, Mark Dopson, Andrey Shchukarev and Åke Sandström, “Chalcopyrite leaching and bioleaching: An X–ray photoelectron spectroscopic (XPS) investigation on the nature of hindered dissolution”, Hydrometallurgy 149 (2014), p 220–227. III. Nathalie Pérez Rodríguez, Mohammad Khoshkhoo, Åke Sandström, Ilia Rodushkin, Lena Alakangas and Björn Öhlander, “Isotopic signature of Cu and Fe during bioleaching and electrochemical leaching of a chalcopyrite concentrate”, International Journal of Mineral Processing 134 (2015), p 58–65. IV. Mohammad Khoshkhoo, Mark Dopson, Fredrik Engström and Åke Sandström, “New insights into the influence of redox potential on chalcopyrite leaching behaviour”, submitted to Hydrometallurgy. Contributions to the papers: Running leaching experiments, analyses, interpretation of data and writing of papers I and II. XPS data interpretation was done with assistance of A. Shchukarev. Running leaching experiments, leaching analyses, interpretation of data and partial writing of paper III. Running leaching experiments, analyses, interpretation of data and writing of paper IV. V Conference papers (not included in the thesis): Mohammad Khoshkhoo and Åke Sandström, “An investigation on the role of microorganisms on chalcopyrite leaching efficiency”, Presented at Mineralteknikkonferens 2014, Luleå, Sweden. Other peer–reviewed journal papers (not included in the thesis): Samuel Awe, Mohammad Khoshkhoo, Paul Kruger and Åke Sandström, “Modelling and process optimisation of antimony removal from a complex copper concentrate”, Nonferrous Metals Society of China Transactions 22 (2012), p 675–685. Mohammad Khoshkhoo, Mark Dopson, Åke Sandström, “Bioleaching and electrochemical leaching of a pyritic chalcopyrite concentrate”, Advanced Materials Research
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