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Gallium and Germanium Recovery from Domestic Sources

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Gallium and Germanium Recovery from Domestic Sources RI 94·19 REPORT OF INVESTIGATIONS/1992 r---------~~======~ PLEASE DO NOT REMOVE FRCJIiI LIBRARY "\ LIBRARY SPOKANE RESEARCH CENTER RECEIVED t\ UG 7 1992 USBOREAtJ.OF 1.j,'NES E. S15't.ON1"OOMERY AVE. ~E. INA 00207 Gallium and Germanium Recovery From Domestic Sources By D. D. Harbuck UNITED STATES DEPARTMENT OF THE INTERIOR BUREAU OF MINES Mission: As the Nation's principal conservation agency, the Department of the Interior has respon­ sibility for most of our nationally-owned public lands and natural and cultural resources. This includes fostering wise use of our land and water resources, protecting our fish and wildlife, pre­ serving the environmental and cultural values of our national parks and historical places, and pro­ viding for the enjoyment of life through outdoor recreation. The Department assesses our energy and mineral resources and works to assure that their development is in the best interests of all our people. The Department also promotes the goals of the Take Pride in America campaign by encouragi,ng stewardship and citizen responsibil­ ity for the public lands and promoting citizen par­ ticipation in their care. The Department also has a major responsibility for American Indian reser­ vation communities and for people who live in Island Territories under U.S. Administration. TIi Report of Investigations 9419 Gallium and Germanium Recovery From Domestic Sources By D. D. Harbuck I ! UNITED STATES DEPARTMENT OF THE INTERIOR Manuel lujan, Jr., Secretary BUREAU OF MINES T S Ary, Director - Library of Congress Cataloging in Publication Data: Harbuck, D. D. (Donna D.) Ga1lium and germanium recovery from domestic sources / by D.D. Harbuck. p. cm. - (Report of investigations; 9419) Includes bibliographical references (p. 25). Supt. of Docs. no.: I 28.22:9419. 1. Gallium-Metallurgy. 2. Germanium-Metallurgy. 3. Leaching. 4. Solvent extraction. 1. Title. II. Series: Report of investigations (United States. Bureau of Mines); 9419. TN23.U43 [TN799.G3] 622 s-dc20 [669'.79] 92-6230 elP T I f f- CONTENTS Page Abstract ................................... ; . 1 Introduction . ... 2 Identifying domestic sources ............................................................ 2 Leaching of zinc residue ........................................... , . 3 Background . 3 Statistical determination of significant variables ............................................ 3 Batch testing of significant variables .................................................... 3 Improving germanium extraction from zinc residues . 6 Germanium insolubility during roasting . 6 Germanium insolubility during leaching . 7 Methods for overcoming germanium insolubility ......................................... 9 Leaching of germanium-gallium ore ...................................................... 10 Background ...................................................................... 10 Results and discussion .............................................................. 10 Germanium extraction ............................................................ 11 Two-stage countercurrent leaching ................................................... 11 Increasing germanium extraction . 13 Gallium and germanium solvent extraction from H 2S04 solutions ............ 14 Gallium solvent-extraction background .................................................. 14 Germanium solvent-extraction background ............................................... 14 Solution preparation and analysis ...................................................... 15 Initial solvent-extraction testing . 15 Gallium solvent extraction ........................................................... 15 Iron versus gallium loading . 15 OPAP and DEHPA . 16 Rate and equilibrium analysis .............................................. '. 17 Gallium loading .............................. '. 17 Gallium stripping .......... '. ~ ...' . 17 Ferric stripping ................................................................ 17 Continuous solvent extraction of gallium . 17 System design ........................,....................................... 17 System operation ........ , ............. , . 1.8 Strip liquor purification ......................................................... 1.8 Germanium solvent extraction ................. , .......................... , .... , . 18 Effect of copper and iron .............. , ................................... , . 19 Synergism ... , ............................................. ,., ..... ,........... 20 Effect of acid concentration .................... ,................................... 20 Germanium stripping ............................................. , . 20 Germanium rate and equilibrium analysis .............................................. 21 Germanium loading .... , ... , ................................. , . 21 Germanium stripping ................................ , . 21. Iron scrubbing .......................................................... : . 21 Continuous solvent extraction of germanium ........ , . 22 System design ........................ ; ........... ,........................... 22 System operation ................................. , . 22 Gallium and germanium coextraction ..... " ........... , .. ,', ......... ,.,., ..... , .. , .... ,' 23 Experimental results , . , , , , , . , , , . , , , , , , , , . , , , , , .. , .. , . , , . , . , , , , .. , , , ...... , .. , . , . , . 23 Industrial application .... "." ......... , ... ,., ......... , ....... , ... " ...... , ..... ".. 24 Summary ,.,", ... ,', ... ,. , , , , .. , , .. , , . , .. , .. , , , , . , , , .. , .... , . , , , ... , , .. , , .... , , .. , 24 References , , , , .. , . , ............. , , .. , ...... , ... , ....... , .. , . , , . , .. , , , ... , , , ... , . , . 25 - II II ILLUSTRATIONS Page 1. Stages of zinc .processing .......................................................... 3 2. Effect of percent solids on metal extraction from zinc residue ............................... 4 3. Effect of H2S04 addition on metal extraction from zinc residue ........... , .................. 4 4. Effect of leach time on metal extraction from zinc residue ................................. 4 5. Effect of temperature on metal extraction from zinc residue ................................ 4 6. Effect of adding S02 to H2S04 leach on gallium and germanium extraction from zinc residue ........ 5 7. Effect of H2S04 molarity on gallium and germanium extraction from zinc residue ................ 5 8. Solubility of Ge02 in H 2S04 , ....................................................... 5 9. XRD printouts of ZnO-Ge02 mixtures at 650°,800°, and 950° C ............................. 6 10. XRD printouts of ZnO-Si02 mixtures at 900°, 1,000°, and 1,100° C ........................... 7 II. Shift of 28 quartz angle with increasing amounts of Ge02 .................................. 7 12. SEM photograph of Si02-Ge02 solid solution ........................................... 8 13. Effect of HF concentration on germanium extraction from H 2S04-leached residue ................ 10 14. Effect of H 2S04 concentration on metal extraction from gallium-germanium ore ................. 11 15. Effect of leach temperature on metal extraction from gallium-germanium ore ................... 12 16. Effect of leach time at various acid concentrations on metal extraction from gallium-germanium ore .. 12 17. Proposed two-stage leach system .................................................... 13 18. Photomicrographs of gallium-germanium ore ........................................... 13 19. Gallium and iron extraction from reduced and reoxidized solutions ........................... 16 20. Effect of pH on gallium extraction using the solvents OPAP and DEHPA ...................... 16 2l. Gallium equilibrium loading and stripping on 0.3M OPAP ................................. 17 22. McCabe-Thiele analysis loading 0.32-g/L-Ga aqueous on 0.3M OPAP .............' ............ 17 23. McCabe-Thiele analysis stripping 0.32-g/L-Ga loaded organic using 1.5M H 2S04 ................. 18 24. McCabe-Thiele analysis stripping ferric iron with 50 pct H3P04 .............................. 18 25. Germanium equilibrium loading and stripping on 0.2M OPAP-30 pct LIX 63 .................... 21 26. McCabe-Thiele analysis of germanium-loading isotherm, 4O-g/L-lIzS04 solution ................. 21 27. McCabe-Thiele analysis of germanium-loading isotherm, 60-g/L-lIzS04 solution ................. 22 28. McCabe-Thiele analysis stripping 0.3- or 0.6-g/L-Ge loaded organic using 75° C HzO ............. 22 29. McCabe-Thiele analysis stripping iron with 3M H 2S04 , .................................... 22 30. Effect of multiple contacts in the coextraction of germanium and gallium from zinc processing liquors 24 TABLES 1. Analyses of potential gallium and germanium ores ........................................ 2 2. Elemental analyses of studied materials ................................................ 2 3. Results of statistically designed experiments ............................................. 3 4. 28 angles for Si02 under various conditions ................. :........................... 7 5. Typical analyses of leach solutions .................................................... 8 6. Selectivity of silica gel for germanium . ... 8 7. Effect of ZnSi04 addition on gallium and germanium extraction .............................. 8 8. Effect of silica on germaliium extraction . 9 9. Effect of "weak acid" leach pH on subsequent germanium extraction from fmal zinc residue. 9 10. Effect
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