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Method for recycling indium and germanium from chlorination distillation residual liquor containing indium and germanium

A chlorination distillation and raffinate technology, which is applied in the field of indium germanium recovery, can solve the problems of high cost and unsatisfactory separation effect, and achieve the effects of convenient operation, reduced separation cost, and reduced separation difficulty

Active Publication Date: 2018-05-22
GUIZHOU HONGDA ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, since the content of indium in the raffinate is less than 5g / L, the metal replacement method is used to separate indium and germanium, which has high cost and unsatisfactory separation effect.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] After chlorination and distillation of indium-germanium-rich raw materials in a certain enterprise, it is specifically carried out by mixing the indium-germanium-rich raw materials with a mixed solution, wherein the mixed solution is hydrochloric acid with a mass fraction of ≥12% and hydrochloric acid with a mass fraction of 10-20% Calcium chloride solution is mixed according to equal volume ratio, and after it is distilled, the distilled residual liquid is obtained. The distillation raffinate contains 720mg / L indium, 83mg / L germanium, 6N hydrochloric acid, and 285g / L chloride ions.

[0042] In the distillation raffinate, add tartaric acid according to tartaric acid / germanium=5, after dissolving, use 30% by volume of N235 and kerosene to form extraction agent, carry out 4 grades of extraction, compare (has / water)=1, temperature is normal temperature, The organic phase loaded with indium germanium and the extraction raffinate are obtained.

[0043] The raffinate contain...

Embodiment 2

[0049] After chlorination and distillation of indium-germanium-rich raw materials in a certain enterprise, it is specifically carried out by mixing the indium-germanium-rich raw materials with a mixed solution, wherein the mixed solution is hydrochloric acid with a mass fraction of ≥12% and hydrochloric acid with a mass fraction of 10-20% Calcium chloride solution is mixed according to equal volume ratio, and after it is distilled, the chlorination distillation raffinate is obtained. Chlorination distillation raffinate contains indium 530mg / L, germanium 98mg / L, hydrochloric acid 6.5N, chloride ion 280g / L.

[0050] Add tartaric acid to the chlorinated distillation raffinate according to tartaric acid / germanium=5, and dissolve it. With 40% by volume of N 235 With the extractant composed of kerosene, a 5-stage extraction is carried out, compared with (with / water)=1, and the temperature is normal temperature.

[0051] The raffinate contains 21.5mg / L of indium and 1.2mg / L of germ...

Embodiment 3

[0055] Use the chlorinated distillation raffinate of Example 1 to carry out indium and germanium extraction according to the N235 extraction agent and extraction conditions of Example 2, and use 3% tartaric acid solution to carry out indium stripping. The primary stripping solution contains 892.5 mg / L of indium and 0.5 mg / L, and then use 40% sodium hydroxide solution for germanium stripping, the primary stripping solution contains germanium 365mg / L, indium 8.5mg / L. The lean organic phase was returned for extraction. The acid stripping solution of indium does not extract indium, return to continue the stripping and enrichment of indium, the alkaline stripping solution of germanium does not extract germanium, return to continue the stripping and enrichment of germanium. Continue to carry out 5 times of recycling, the average extraction rate of indium is 93.8%, the stripping rate is 97.5%, and the primary stripping solution contains 4.2g / L of indium. The average extraction rate ...

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Abstract

The invention relates to the technical field of hydrometallurgy, in particular to a method for recycling indium and germanium from chlorination distillation residual liquor containing the indium and the germanium. The method comprises the steps that tartaric acid is added to the distillation residual liquor, so that mixed liquor containing InCl4 or InCl6<3> germanium tartrate acid radical anions (Ge(A)3<2>), A representing the tartaric acid) is obtained; indium extraction and germanium extraction are conducted at the same time through a N235-kerosene system extraction agent; and then, indium reverse extraction is conducted through dilute acid, and germanium reverse extraction is conducted through a sodium hydroxide solution. By means of the method, the indium and germanium separation costis lowered; the extraction agent is high in regeneration capacity; the separation difficulty is lowered; the process is easy to implement; and operation is easy and convenient to conduct.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for recovering indium and germanium from chlorinated distillation raffinate containing indium and germanium. Background technique [0002] The hard zinc produced by pyro-method zinc smelting, after distilling zinc in a vacuum furnace, the content of indium and germanium in the obtained residue reaches more than 1%, and its treatment mainly includes the following three methods: (1) after the residue is oxidized and roasted, it can be Directly carry out chlorination and distillation of germanium chloride, and indium enters the distillation raffinate; (2) the indium, germanium, lead and zinc materials are subjected to neutral leaching for many times, and indium and germanium are enriched in the neutral leaching residue, and can also be directly chlorinated distilled GeCl 4 , indium enters the distillation raffinate; (3) after acid leaching, the tannin sinks germani...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B58/00C22B41/00
CPCC22B7/006C22B41/00C22B58/00Y02P10/20
Inventor 李世平卢宇王志斌韦国龙
Owner GUIZHOU HONGDA ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
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