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Understanding Fluid–Rock Interactions and Lixiviant/Oxidant Behaviour for the In-Situ Recovery of Metals from Deep Ore Bodies

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Understanding Fluid–Rock Interactions and Lixiviant/Oxidant Behaviour for the In-Situ Recovery of Metals from Deep Ore Bodies School of Earth and Planetary Science Department of Applied Geology Understanding Fluid–Rock Interactions and Lixiviant/Oxidant Behaviour for the In-situ Recovery of Metals from Deep Ore Bodies Tania Marcela Hidalgo Rosero This thesis is presented for the degree of Doctor of Philosophy of Curtin University February 2020 1 Declaration __________________________________________________________________________ Declaration To the best of my knowledge and belief, I declare that this work of thesis contains no material published by any other person, except where due acknowledgements have been made. This thesis contains no material which has been accepted for the award of any other degree or diploma in any university. Tania Marcela Hidalgo Rosero Date: 28/01/2020 2 Abstract __________________________________________________________________________ Abstract In-situ recovery (ISR) processing has been recognised as a possible alternative to open- pit mining, especially for low-grade resources. In ISR, the fluid–rock interaction between the target ore and the lixiviant results in valuable- (and gangue-) metal dissolution. This interaction is achieved by the injection and recovery of fluid by means of strategically positioned wells. Although the application of ISR has become more common (ISR remains the preferential processing technique for uranium and has been applied in pilot programs for treating oxide zones in copper deposits), its application to hard-rock refractory and low-grade copper-sulfide deposits is still under development. This research is focused on the possible application of ISR to primary copper sulfides usually found as deep ores. Lixiviant/oxidant selection is an important aspect to consider during planning and operation in the ISR of copper-sulfide ores. Oxidant addition is required to break down the refractory copper-sulfide structure. During the course of the reaction, the fluid stability, mineral selectivity and accessibility (from precipitation or side reactions) may be affected, which in turn limits the application of ISR. Extensive research has been conducted on lixiviant kinetics under heap-leaching conditions, especially for 3+ common oxidants (Fe and O2) in acid solutions for fine-grained powder, pure- mineral and concentrate samples and from ambient temperature to 90°C. However, few studies have investigated different reagents for ISR application and with a focus on coarse materials. This study focuses on the changes in the chemical composition of both the solutions and the mineral samples after their reaction with different lixiviant/oxidant solutions under conditions that may simulate an ISR application. Copper-sulfide samples used included natural chalcopyrite, bornite, chalcocite and covellite with different percent contents of gangue (e.g., pyrite, carbonates and silicates) and sample types that varied from powder (–38 μm to –160 μm) to cuboids (~4 mm on each side). To identify potential alternative lixiviant/oxidant solutions for ISR environments, a comparative analysis of chalcopyrite dissolution was performed. The tests were performed on cuboids with eleven leach solutions (FeCl3, CuCl2 and K2Cr2O7 in HCl; 3 Abstract __________________________________________________________________________ Fe2(SO4)3, CuSO4, NaNO3 and H2O2 in H2SO4; O2 and H2O2 in glycine; (NH4)2SO4 in ammonium hydroxide and ferric methanesulfonate) at 110°C (below the sulfur melting point) and 170°C (above the sulfur melting point), and under anoxic conditions. Copper dissolution tended to increase with an increase in temperature, but some solutions, such as potassium dichromate and hydrogen peroxide, were affected negatively by elevated temperature. Mineralogical characterisation of the reacted solids showed the formation of different surface layers, which depended on the fluid chemistry. Some of the product phases that replaced chalcopyrite had a porous texture and the initial fracture size increased as the reaction proceeded. Ferric chloride in hydrochloric acid was found to be the most efficient leach solution. Once the preferred leach solution had been selected, kinetic analyses were performed to identify energy requirements for pure (chalcopyrite) and composite (chalcopyrite/bornite) samples when leached with ferric-chloride solution. Activation energies were determined by using the shrinking-core model and the ‘time-to-a-given- fraction’ method. The latter method proved more appropriate when mineral dissolution occurred as a result of a combination of mechanisms. The kinetics of the composite samples were driven by the major phase present, and the activation energy increased because of the presence of chalcopyrite. The experimental data could not be fitted accurately to the equations in the shrinking-core model and led to incorrect estimates of the activation energies. This result suggests that, for ISR targets (composite with gangue), the best approach for kinetic analysis is to use model-independent equations that allow for the calculation of activation energies throughout the reaction. The calculation of partial activation energies helps to understand the propensity for subsurface solid transformation and the dissolution rates. Experiments were conducted under replicate ISR conditions to identify copper-sulfide transformations and mineralogical changes in acidic solutions with depleted oxidant. Even at low temperatures, bornite and chalcocite/digenite transformed to covellite. The replacements showed characteristic features of an interface-coupled dissolution– reprecipitation (ICDR) mechanism, such as sharp chemical interfaces and porosity development in newly formed phases. Bornite transformations indicated the coexistence of an ICDR mechanism with solid-state diffusion processes by the formation of fluid-mediated exsolution of copper-deficient lamellas. 4 Abstract __________________________________________________________________________ Finally, multistage fluid–rock interactions were studied using natural low-grade samples with a high concentration of gangue to replicate fluid movement through subsurface ore. Acid consumption and changes in pH resulted in the precipitation of jarosite, akaganeite and gypsum because of cation and anion build up in solution. Sulfate solutions showed higher precipitation rates compared with chlorides, but NaCl addition increased gypsum precipitation. The precipitates act as passivation layers and could produce blockages that present a risk for subsurface ISR operations. This research presents a geometallurgical approach to ISR processing by understanding the fluid–rock interactions through solid–fluid analysis after reaction. The results provide valuable information for fluid selection in an ISR process, which, when coupled with other research efforts currently underway to progress understanding towards ISR, may unlock the reality of hard-rock copper ISR processing. 5 Acknowledgement __________________________________________________________________________ Acknowledgement I would like to thank all my supervisors for their support given during this PhD. Thank you for believing in me and for providing me with this opportunity. All my gratitude to Dr Laura Kuhar for all the time spent working with me, I could not have completed this work without having an outstanding mentor such as you. Special thanks to Prof. Andrew Putnis; it has been an honour to work with someone as experienced as you, and I have learned a lot from you during this research. I would like to thank Dr Andreas Beinlich for all the help with the research and for taking the time to help me familiarize myself with new techniques in the laboratory. To Dr Robbie McDonald, I consider you as one my supervisors, thank you for all the draft revisions, training and helping me to understand my results. I want to thank to my sponsors, the Minerals Research Institute of Western Australia (MRIWA), BASF and the former Parker Centre from which grants were obtained for MRIWA project M488, which allowed me to conduct all experiments and analysis required to finalize this research. I am very grateful to Drs Dave Robinson, Denis Shiers, Jian Li and Richard Macoun for all the good ideas and useful comments on the experiments and manuscripts. I am incredibly grateful for having had the opportunity to work at CSIRO Mineral Resources; as an engineer and scientist I think that CSIRO serves as a great bridge between scientific research and industry requirements. Thank you to all the people that helped me with analysis, experiments, planning and training. Special acknowledgements to Michael Verrall, Peter Austin, Karl Bunney, Tuyen Pham, Nicky Chapman, Rebecca Meakin, Dr Belinda Godel, Dr Martijn Woltering and Milan Chovancek. Many thanks to all the people I met in Australia. Thanks for the encouragement and good times to Cameron, Michelle, Tobi, Sophia, Aja, Evelien, Franzi and Lars. To my family, you are the reason of all my efforts, thank you for always believing in me and for being there even though we are on different sides of the globe. This work would not exist without your support and love. 6 Table of Contents __________________________________________________________________________ Table of Contents Declaration .................................................................................................................. 2 Abstract ....................................................................................................................... 3 Acknowledgement .....................................................................................................
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