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Method for recovering germanium from germanium-containing materials

A technology of material and germanium slag, which is applied in the field of hydrometallurgy, can solve problems such as difficult and efficient leaching of germanium, and achieve excellent leaching kinetics, increased dissolution speed, and obvious leaching effect

Inactive Publication Date: 2014-07-30
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the inventors further studied complex phases, especially multi-metal germanium-containing materials, they found that using the existing leaching technology, when the coating layer is dissolved or destroyed, other cations must enter the leaching solution, and the leaching of germanium is often inhibited by other metal ions ; this is one of the reasons why the existing technology is difficult to efficiently leach germanium
[0005] So far, there is no report in the relevant literature on the efficient leaching of germanium using leaching aids combined with low-concentration inorganic strong acids

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] First prepare 105g / L H 2 SO 4 Solution is used as leaching agent, takes by weighing 200Kg particle size and is -100 purpose germanium-containing 0.23wt%, zinc-containing 12.6wt%, copper-containing 4.65wt%, iron-containing 5.82wt% material in the reactor, according to the liquid-solid mass ratio is 5: Add leaching agent at a ratio of 1. Then, start stirring, add 85kg of tartaric acid as a leaching aid (that is, the molar ratio of tartaric acid to germanium in the germanium-containing material used is tartaric acid:germanium=89.5:1), and the above-mentioned material solution is heated to 85° C. for leaching for 2 hours. After the leaching reaction is finished, the leaching solution containing germanium can be obtained through liquid-solid separation. The leaching rate of germanium is greater than or equal to 93.1%.

[0034] Pump the leaching solution obtained above into the reaction kettle, start stirring, add lye to pH=6.5, and separate the liquid and solid to obtain ...

Embodiment 2

[0036] First prepare 60g / L H 2 SO 4 Solution is used as leaching agent, takes by weighing 200Kg particle size and is -100 purpose germanium-containing 0.23wt%, zinc-containing 12.6wt%, copper-containing 4.65wt%, iron-containing 5.82wt% material in the reactor, according to the liquid-solid mass ratio is 9: Add leaching agent at a ratio of 1. Then, start stirring, add 110kg of sodium citrate as a immersion aid (that is, the mol ratio of sodium citrate to germanium in the germanium-containing material used is sodium citrate:germanium=30.37:1), and the temperature of the above-mentioned feed liquid is raised to 90°C Leach for 2h. After the leaching reaction is finished, the leaching solution containing germanium can be obtained through liquid-solid separation. The leaching rate of germanium is greater than or equal to 91.7%.

[0037] Pump the leaching solution obtained above into the reaction kettle, start stirring, add lye to pH = 8.2, and separate liquid and solid to obtain...

Embodiment 3

[0039] First prepare 90g / L H 2 SO 4 Solution is used as leaching agent, and 200Kg particle size is taken by weighing 0.23wt% germanium-100 purpose, 12.6wt% zinc, 4.65wt% copper, 5.82wt% iron-containing material in the reactor, according to the liquid-solid mass ratio is 6: Add leaching agent at a ratio of 1. Then, start stirring, add 48kg of oxalic acid as a leaching aid (that is, the molar ratio of oxalic acid to germanium in the germanium-containing material used is oxalic acid: germanium = 118.7:1), and raise the temperature of the above-mentioned feed solution to 55° C. for leaching for 2 hours. After the leaching reaction is finished, the leaching solution containing germanium can be obtained through liquid-solid separation. The leaching rate of germanium is greater than or equal to 95.2%.

[0040] Pump the leaching solution obtained above into the reaction kettle, start stirring, add lye to pH=7.4, and separate the liquid and solid to obtain germanium slag. The obtain...

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Abstract

The invention relates to a method for recovering germanium from germanium-containing materials, particularly relates to a method for recovering germanium from germanium-containing materials of non-ferrous smelting industry, and belongs to the technical field of hydrometallurgy. The method comprises the steps of leaching germanium-containing materials as raw materials of which the particle sizes are 100 meshes with inorganic strong acid as an leaching agent of which the concentration is 50-120g / L and an aid-leaching agent at 35-95 DEG C and filtering to obtain a germanium-containing leaching solution, adjusting the pH value of the germanium-containing leaching solution to be 6-9, stirring and carrying out liquid-solid separation to obtain germanium residues, and calcining the germanium residues at 350-500 DEG C to obtain a crude germanium dioxide product, wherein the aid-leaching agent is one of tartaric acid, water-soluble tartrate, citric acid, water-soluble citrate, oxalic acid and water-soluble oxalate. The method disclosed by the invention has the advantages of simple process, easiness in operation, high recovery ratio of germanium, large enrichment ratio, and convenience in industrial production and application.

Description

technical field [0001] The invention relates to a method for recovering germanium from germanium-containing materials, in particular to a method for recovering germanium from germanium-containing materials in the non-ferrous smelting industry; it belongs to the technical field of hydrometallurgy. Background technique [0002] Germanium is a dispersed element, and it is mainly dispersed in nature and associated with polymetallic deposits. At present, germanium is mainly extracted from lead-zinc and copper sulfide ores in industry. In the conventional hydrometallurgy process, when the pH of the leaching system is high, germanium mainly enters the leaching slag, such as the leaching slag in zinc hydrometallurgy; while when the pH of the leaching system is low, most of the germanium is leached into solution, and enriched in the purification slag in the subsequent impurity removal process, such as zinc powder replacement slag, copper cadmium slag, etc. However, these germanium-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B41/00C22B3/06C22B3/46
CPCY02P10/20
Inventor 李玉虎刘志宏刘付朋李启厚刘智勇谢勇贤
Owner CENT SOUTH UNIV
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