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Mohahmad Shuva Thesis Analysis of Thermodynamic Behaviour of Valuable Elements and Slag Structure during E-Waste Processing through Copper Smelting By Mohammad Al Hossaini Shuva (B.Sc.Eng., M.Sc.Eng.) A Thesis Submitted to the Faculty of Science, Engineering and Technology for the Degree of Doctor of Philosophy Swinburne University of Technology Melbourne, Australia September 2017 Abstract Waste of electronics and electrical equipment (WEEE or e-waste) and other end-of- life (eol) high technology products can be viewed as resources for metals, as they do not only contain the common metals like iron (Fe), aluminium (Al), lead (Pb) and copper (Cu) but also trace valuable and rare elements such as gold (Au), silver (Ag), tin (Sn), selenium (Se), tellurium (Te), platinum (Pt), palladium (Pd), tantalum (Ta), cobalt (Co) and indium (In). The recovery of these trace elements is vital, not just because it has high commercial values, but also for resources efficiency. One of the existing industrial routes for processing of e-waste is through the primary and secondary copper smelting processes. During these processes, the trace elements are distributed in different phases, i.e., in metal/matte, slag and gas. Different elements have different thermodynamic properties that govern the partitioning behaviour during the process. There has been a number of studies on the distribution behaviour of the trace elements relevant to primary copper smelting (extraction of metals from virgin ores). However, there are only limited thermodynamic data relevant to secondary copper smelting (extraction of metals from secondary/recycled sources). The main purpose of the present study is to investigate the thermodynamic behaviour of germanium (Ge), palladium (Pd) and tantalum (Ta) metals and determine their distribution-ratio in slag-metal equilibrium reaction during black copper processing. A secondary aim is to examine the FeOx-CaO-SiO2-MgO and FeOx-CaO-SiO2-MgO-Cu2O- (GeO2/PdO) slag using vibrational spectroscopy (i.e., Fourier Transform Infrared) to understand the effect of experimental parameters on the silicate slag structure. Furthermore, a correlation between the degree of polymerization and distribution-ratio was developed using multiple regression analysis. / The distribution-ratio of germanium (Ge), L , during equilibrium reactions between s m magnesia saturated FeOx-CaO-SiO2 (FCS) slag Geand molten copper was measured using vertical tube furnace. The results showed that the Ge distribution-ratio increases with increasing oxygen partial pressure, and with decreasing temperature. It was also observed that the distribution-ratio is strongly dependant on the slag basicity. At fixed CaO concentration (in the slag), the distribution-ratio was found to increase with increasing / Fe/SiO2 ratio, tending to a plateau at L = 0.8. This result, together with the assessment of s m ionic bond fraction carried out in this study,Ge suggested the acidic nature of germanium oxide iii (GeO2) in the slag system. The characterisation results of the quenched slag suggested that o Ge is present in the FeOx-CaO-SiO2-MgO slag predominantly as GeO2. At 1300 C (1573 -8 K) and = 10 atm, the activity coefficient of GeO2 in the slag was calculated to be in the range of O0.242 to 1.50. The results from the present study suggested that less-basic slag, high operating temperature, and low oxygen partial pressure promote a low Ge distribution-ratio. / The slag-to-metal distribution-ratio of palladium (Pd), L , in the range of oxygen s m -10 -7 o partial pressure ( ) from 10 to 10 atm at 1473 to 1623KPd (1200 to 1350 C) was 2 / investigated. The resultsO showed that L increased with increasing and with decreasing s m / 2 temperature. It was also observed thatPd the L is strongly dependantO on slag basicity, i.e., s m as defined using the mass ratio of (CaO+MgO)/SiOPd 2 or optical basicity. The present results 2+ suggested that Pd is present in the FeOx-CaO-SiO2-MgO slag predominantly as Pd . The o -8 activity coefficient of PdO in the slag at 1573K (1300 C) and = 10 atm was calculated -3 -2 and found between the range of 3.89×10 to 2.63×10 . TheO 2results from the Pd study suggested that to promote the recovery of palladium from Pd-containing e-waste during a secondary copper smelting process, a slag with lower silica content, high temperature with reducing atmosphere, are highly desired. / This study also examined the distribution-ratio of tantalum (Ta), L , in the range s m -16 -12 o of oxygen partial pressure ( ) from 10 to 10 atm at 1673 and 1873KTa (1400 C and o 1600 C). It was found that TaO2 mostly partitions to slag phase and very small amount of Ta is found in liquid copper at high temperature and reduced condition. The slag structure study focused on the structure of silicate units in the FeOx-CaO- SiO2-MgO and FeOx-CaO-SiO2-MgO-Cu2O-(GeO2/PdO) slags. It was found that the slags structure is affected by the experimental parameters and slag compositions. The present results suggested that the degree of polymerization Q3/Q2 is strongly related with thermophysical and thermodynamic properties of the slag melt. A correlation based on experimental results was suggested between distribution-ratio and the degree of polymerization is presented as follows: / 181 61422 365 115 L = log + 3 S m 75 T 36 8 Ge 2 2 / 74 724− 8 � − 2 L = log + + 3 S m 9999 21 5 2 Pd − � 2 iv The novel aspect of the present study is that the distribution behaviour of valuable metals (Ge, Pd, Ta) between copper and FCS slags has been determined. The oxidation state and activity coefficient of these valuable metals oxide (GeO2, PdO) in the FeOx-CaO-SiO2 system and their acid/base character have also been determined. The thermodynamic data generated from this study can be used for process modelling purposes to improve the recovery of valuable metals in primary and secondary copper smelting processes. These data can further be used to update the database of thermochemical software. It was recommended from the slag structure analysis that, Q3/Q2 is a good candidate for practical measurement of the degree of networking that relates slag structure to thermodynamics and properties. v Acknowledgements I would like to express sincere gratitude to my principle supervisor Associate Professor M Akbar Rhamdhani for his continuous support throughout the period of my doctoral study. He has excellent knowledge in the field of process metallurgy, and his right guidance helped me all the time of research and thesis writing. His sincere devotion to research and tremendous patience of reading my thesis helped me to produce this thesis. He was very friendly in discussion and supportive in case of social aspects. I could not have imagined someone in replacement of Akbar, and I always feel proud to become his student. I would like to acknowledge the support and guidance received from other members of my supervisor team. I am grateful to Professor Geoffrey Brooks for his encouragement, guidance and support during my study. His valuable suggestion helped me to improve my research and analytical skills. I am also thankful to Professor Syed Masood for his precious advice and support. I would also thankful to my associate supervisor Professor Markus Reuter (Director, Helmholtz Institute Freiberg for Resource Technology, Freiberg, Germany), for his valuable support and guidance. It is an honour to work with him and his guidance helped me a lot. I wish to thank Dr James Wang and Dr Deming Zhu for their assistance in performing XRD and Raman at Swinburne. My sincere thankfulness goes to technical staffs at Faculty of Science, Engineering and Technology: Walter Chetcuti, Yeannette Lizama, Savithri Galappathie and Aidan O’Keefee. I wish to acknowledge Mr Bernard Hedger from Spectrometer Service Pty Ltd, for assisting me in ICP-AES analysis. I would like to acknowledge the Swinburne University Postgraduate Research Award (SUPRA) support. The author would like to also recognise the support of the Wealth from Waste Research Cluster, a collaborative program between the Australian CSIRO (Commonwealth Scientific Industrial Research Organisation); University of Technology, Sydney; The University of Queensland, Swinburne University of Technology, Monash University and Yale University, USA. I would like to thank my research fellows of high temperature processing (HTP) group: Dr Reiza Mukhlis, Dr Sazzad Ahmed, Dr Saiful Islam, Dr Mehedi Mohammed, Jaefer Yenus, Muhamad Firdaus, Bapin Kumar Route, and Epma Lupita Putri. I would like vii to specially thank Dr Sazzad, Jaefer, Bapin and Firdaus for their all discussion and sharing of knowledge. My profound love and appreciation go to my parents, parents-in-law, sisters and brothers for their support. I would like to honestly thankful to my wife, Nasrin Akter Shipon. She was very patience throughout my study and her on going encouragement and care helped me to finish this PhD journey. This thesis is dedicated to my lovely wife and my entire family viii Declaration The author declares that this thesis on the “Analysis of Thermodynamic Behaviour of Valuable Elements and Slag Structure during E-Waste Processing through Copper Smelting”, is produced from my own work which contains no material that has been accepted for the award to the candidate of any other degree or diploma where due reference is made in the text of this thesis. The results presented in this thesis have been published in different journals and conferences. The papers published from this study are listed below: o Shuva, M.A.H., Rhamdhani, M.A., Brooks, G. A, Masood, S., and Reuter, M.A, “Thermodynamics of palladium (Pd) and tantalum (Ta) relevant to secondary copper smelting”, Metallurgical and Material Transactions B, 48 (1) (2017), 317-327. o Shuva, M.A.H., Rhamdhani, M.A., Brooks, G.A, Masood, S., and Reuter, M.A, “Thermodynamics behaviour of germanium during equilibrium reactions between FeOx-CaO-SiO2-MgO slag and molten Copper,” Metallurgical and Material Transactions B, 47 (5) (2016), 2889-2903.
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