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LEACHING of CHALCOPYRITE By LEACHING OF CHALCOPYRITE by R.C.H. FERREIRA Eng. Qidmico Industrial (I.S.T) - Lisbon A thesis submitted for the degree of Doctor of Philosopy of the University of London April, 1972 - 2 -- ABSTRACT Two forms of chalcopyrite were synthesized. A I3-form, cubic, of composition CuFeS1.83, and an a-form, apparently tetragonal and with composition near to Cu1.12Fel.09S2, having about 10.7% excess copper and 8.3% excess iron over the stoichiometric CuFeS2. Samples of the two synthetic materials were crushed and sieved, and the fractions obtained were leached with acidic ferric sulphate solutions. Leaching with hydrogen peroxide was also used on the8--form, and the effect of chloride ion on the leaching rate of the a-form was studied. The effects of some leach variables, for example, temperature and ferric ion concentration, were investigated. 8-chalcopyrite was leached in three stages, the first and second being mainly diffusion controlled and the third chemically controlled. a-chalcopyrite was found to be metastable, changing with age. The dissolution rate-curves altered as this change took place, until a stable form was reached. This form was leached in two stages, the first corresponding to the removal of the 10.7% excess copper over the stoichiometric CuFeS2, and the second the straightforward dissolution of the remaining, nearly stoichiometric, residue to produce elemental sulphur. Natural chalcopyrite is leached in a manner very similar to this second stage, involving nearly stoichiometric chalcopyrite. The change in both a- and form leach residues were studied using X-ray powder diffraction techniques, electron probe microanalysis and microscopic examination. Finally the use of E-pH diagrams for temperatures other than 298°K was studied for the systems sulphur-water, copper oxides and sulphides-water, iron oxides and sulphides-water, and special attention was paid to the use of half-cell reactions and the thermodynamic properties of the electron, in the calculations. • - 3 CONTENTS Page ABSTRACT 2 INTRODUCTION 7 SECTION 1 - LITERATURE SURVEY 8 1.1 Previous Work on the Leaching of Chalcopyrite 8 1.2 Chalcopyrite Structures 33 1.3 Phase Relations in the Cu-Fe-S System 55 1.4 Previous Work on the Synthesis of Chalcopyrite 64 1.5 Sulphur Vapour Pressure 66 1.6 Thermal Behaviour of Chalcopyrite. 71 Thermodynamic Properties 1.7 Complexing of the Ferric Ion in the Leach 83 Solution. Jarosite-type Species. SECTION 2 - EXPERIMENTAL PROCEDURES. 88 2.1 Synthesis of Chalcopyrite 88 2.1.1 13-Chalcopyrite 92 2.1.2 a-Chalcopyrite 96 2.2 Leaching Apparatus and Experimental 100 Procedure 2.3 Analytical Methods 104 2.3.1 Atomic Absorption 104 2.3.2 Nephelometry 106 2.3.3 UV Spectrophotometer. Elemental 107 Sulphur Determinations. 2.3.4 X-ray Powder Diffraction 108 2.3.4.1 Choice of Radiation 108 2.3.4.2 Measurement of Line Positions 109 2.3.4.3 Measurement and Calculation of the 109 Intensities of X-ray Reflections. 2.3.5 Other Methods 112 2.4 Purity of Materials 113 Page SECTION 3 - -CHALCOPYRITE. RESULTS AND DISCUSSION 117 3.1 Ferric Sulphate Leaching. Kinetic Rate- 117 Curves. Effect of the Leach Variables on the Rate of Reaction. 3.1.1 Temperature 117 3.1.2 Particle Size and Sample Weight 127 3.1.3 Ferric Ion Concentration 131 3.2 X-ray Powder Diffraction Study of the Leach 134 Residues 3.3 Electron Probe Microanalysis 141 3.4 Change of Colour 143 3.5 Leaching with Hydrogen Peroxide 144 3.6 Microscope Examination 149 SECTION 4 - a-CHALCOPYRITE. RESULTS AND DISCUSSION 151 4.1 Ferric Sulphate Leaching. Kinetic Rate- 151 Curves. 4.1.1 Effect of Storage Time 151 4.1.2 Effect of Ferric Ion Concentration 156 4.2 Electron Probe Microanalysis 158 4.3 Leaching with Hydrochloric Acid. Effect of 161 Chloride Ion on the Leaching Rate, 4.4 X-ray Powder Diffraction Study of the Leach_ 167 Residues 4.5 Microscope Examination 169 SECTION 5 - CONCLUSIONS 170 5.1 Summary of Results 170 5.2 Comparison of the Present Investigation 173 with PrevioUS Work APPENDIX A -• HIGH TEMPERATURE POTENTIAL --pH. DIAGRAMS FOR 178 THE SULPHUR-WATER,' COPPER OXIDES AND SULPHIDES- WATER AND IRON OXIDES AND SULPHIDES--WATER SYSTEMS Page A-1. Introduction 179 A-2. Relations Used 180 A-2.1 Non-Redox Reactions 180 A-2.2 Redox Reactions 180 A-2.3 Calculation of AGT° 180 A-2.4 Use of Half-Cell Reactions - 182 Thermodynamic Properties of the Electron A-2.5 Variation of Activity Coefficients 185 and pH with Temperature A-3. Simplified Relations for Each Temperature 188 A-3.1 t = 25°C T = 298°K 188 A-3.2 t = 100°C T = 373°K 188 A-3.3 t = 150°C T = 4230K 188 A-4 Sulphur-Water System 190 A-4.1 Reactions -190 A-4.2 Potential-pH Relationships 192 A-4.2.1 t = 25°C T = 298°K 192 A-4.2.2 t = 100°C T = 373°K 193 A-4.2.3 t = 150°C T = 14230K 194 A-4.3 Discussion on the Sulphur-Water 195 System A-5 Copper Oxides and Sulphides-Water System 201 A-5.1 Reactions 201 A-5.2 Potential-pH Relationships 203 A-5.2.1 t = 25°C T = 298°K 203 A-5.2.2 t = 100°C T = 373°K 2014 A-5.2.3 t = 150°C T = 4230K 205 A-5.3 Conclusions on Copper Oxides and 206 Sulphides-Water System A-6 Iron Oxides and Sulphides-Water System. 213 A-6.1 Reactions 213 A-6.2 Potential-pH Relationships 215 A-6.2.1 t = 25°C T = 298°K 215 A-6.2.2 t = 100°C T = 373°K 216 A-6.2.3 t = 150°C T = 4230K 217 A-6.3 Conclusions on Iron Oxides and Sulphides- Water System 218 - 6 Page A-7 Some Comparisons with Results of Other 223 Authors A-8 Auxiliary Thermodynamic Data 227 APPENDIX B - EXPERIMENTAL RESULTS FROM THE LEACHING RUNS 231 B-1 Leach Liquor 232 B-1.1 f3-Chalcopyrite 232 B-1.2 a-Chalcopyrite 248 B-2 Solid Residues 256 B-2.1 Atomic Absorption and Electron Probe 256 Analyses B-2.2 X-ray Powder Diffraction Analyses 258 B-2.3 X-ray Powder Photographs 293 B-2.4 Photomicrographs of the Residues. 302 APPENDIX C OPEN FURNACE AND PRESSURE FURNACE DESIGN 316 C-1 Basic Relations 317 C-2 Open Furnace 319 C-2.1 Calculations of the External Surface 319 Temperature C-2.2 Determination of the Number of Turns 321 in the Winding C-3 Pressure Furnace 322 C-3.1 Calculation of the Thickness of the 322 Insulating Layer C-3.2 Calculation of the Wail and Cover 324 Plates Thickness for the Pressure Vessel C-3.3 Design of Welded Connections and Fittings 325 C-4 Workshop Drawings 327 ACKNOWLEDGEMENTS------------ 332 REFERENCES 333 - 7 INTRODUCTION Copper sulphide minerals are the largest source of copper in the world and chalcopyrite is one of the most important of them. Smelting of the ores containing these minerals contributes to the pollution of the atmosphere due to the production of sulphur dioxide. With the introduction of increasing restrictions on the permitted pollution level, hydrometallurgy became a short term solution of the problem. However, chalcopyrite is the copper sulphide which presents the greatest resistance to dissolution, and even drastic processes using high temperatures and pressures are still relatively slow. A process normally used for low grade ores is dump leaching, and in the case of chalcopyrite the use of ferric sulphate as an oxidising agent is quite common, although having the disadvantage of being a very lengthy recovery method. Most of these dissolution processes are based on an old fashion empiricism of successive trial of conditions, some of them leading to expensive technological solutions. The aim of this work is to try and clarify some points in the mechanism of leaching of chalcopyriteend obtain information that will allow the handling of the recovery process in such a way to increase yields and reduce prices. Thus, attempts were made to obtain pure chalcopyrite by synthetic methods, since the natural ores seem to be affected by the impurities they normally contain, changing the reactivity and masking the true mechanism. Ferric sulphate was found to be a suitable oxidizing agent, since it led to a very slow dissolution process, and allowed the transformation of the solid to be followed in relative detail. SECTION I LITERATURE :SURVEY 1.1 Previous work on the Leaching of Chalcopyrite The leaching of chalcopyrite has been the subject of many investigations(1-20 ) covering the three main points normally known as - Atmospheric leaching - Pressure leaching - Bacterial leaching The first major contribution was given by WARREN( 1 in 1958. He studied in detail the acid pressure leaching of the -100 + 200 mesh fraction of a chalcopyrite concentrate containing approximately 20 per cent of pyrite, and reported the influence of temperature, acidity, oxygen partial pressure and surface area on the oxidation rate of that concentrate. Theranges of aridity considered were described by Warren as "moderate" - between pH 1.0 and 1.5 -- and "high" - below pH 1.0. The effect on the rate of leaching copper, and oxidation of sulphur to sulphate by increasing the temperature from 1200C to 1800C is shown in Fig. 1 . As can be seen, this effect is more pronounced at "moderate" acidity (pH 1.0 1.5). The lower values at "high" acidity were due to the formation of a coating of molten elemental sulphur* (less sulphur oxidized to sulphate) at the temperatures used (M.P.
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