A method for preparing high-grade germanium concentrate from germanium-containing leaching solution

A technology of leaching solution and germanium concentrate, applied in the field of hydrometallurgy, can solve the problems that the quality of germanium concentrate is difficult to meet the market demand and the grade of germanium concentrate is low, and achieves easy industrial production, high germanium recovery rate and simple process. Effect

Active Publication Date: 2019-10-25
YUNNAN CHIHONG INT GE CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are many raw materials for extracting germanium. If the germanium content in the germanium-containing raw material is too low and the impurity elements such as arsenic and iron are high, then the germanium-containing leachate obtained by sulfuric acid leaching has a low germanium content and a high impurity content. The arsenic content in the germanium concentrate produced by Ningshen Germanium exceeds the standard, and the content of other impurities is also high. The grade of the germanium concentrate is low, making it difficult for the quality of the germanium concentrate to meet the market demand.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The germanium-containing leaching solution in this embodiment is a first-stage acid leaching solution for zinc oxide soot sulfuric acid leaching, and its main components are: pH=3.0-3.5, Zn 141.63g / L, Ge 83.5mg / L, As 0.61g / L, Fe 2+ 5.50g / L, FeT 5.75g / L. Firstly, the germanium-containing leaching solution was added to the germanium-containing leaching solution at a temperature of 60°C, and a tannic acid solution with an acidity of 10.0 g / L that was 25 times the germanium content was added, stirred for 20 minutes, and filtered to obtain No. 1 germanium tannin slag and the solution after germanium precipitation. Liquid back electro-zinc system: Use sulfuric acid solution to carry out 3-stage countercurrent washing on the above-mentioned No. 1 tannin germanium slag, the sulfuric acid concentration is 60g / L, the liquid-solid ratio is 4:1, the washing temperature is 60°C, and the washing time of the first stage is 3h , the washing time of stage II and III is 1h, filter to obt...

Embodiment 2

[0023] The germanium-containing leaching solution in this embodiment is a first-stage acid leaching solution for zinc oxide soot sulfuric acid leaching, and its main components are: pH=3.0-3.5, Zn 141.63g / L, Ge 83.5mg / L, As 0.61g / L, Fe 2+ 5.50g / L, FeT 5.75g / L. Firstly, the germanium-containing leaching solution was added with a tannic acid solution with an acidity of 5.0 g / L that was 30 times the germanium content at a temperature of 60°C, stirred for 15 minutes, and filtered to obtain No. Liquid back electro-zinc system: Use sulfuric acid solution to carry out 2-stage countercurrent washing on the above-mentioned No. 1 germanium tannin slag, the sulfuric acid concentration is 10g / L, the liquid-solid ratio is 3 / 1, the washing temperature is 50°C, and the washing time of the first stage is 2h , the washing time of stage II is 1h, filter to obtain No. 2 germanium tannin slag and lotion, and return the lotion to the leaching process; dry the above-mentioned No. 2 germanium tannin...

Embodiment 3

[0025] The germanium-containing leaching solution of the present embodiment is the sulfuric acid leaching solution containing germanium slag, and its main component is: H 2 SO 4 11.99g / L, Zn 127.75g / L, Ge 193.8mg / L, As 0.44g / L, Fe 2+ 8.15g / L, FeT 8.15g / L. First, use germanium slag to adjust the pH value of the germanium-containing leaching solution to 2.0, and at a temperature of 60°C, add a tannic acid solution with an acidity of 10.0 g / L that is 25 times the germanium content, stir for 20 minutes, and filter to obtain No. 1 tannin germanium slag And the liquid after germanium sinking, the liquid after sinking germanium is back to the zinc system; the above-mentioned No. 1 germanium tannin slag is subjected to 3-stage countercurrent washing with sulfuric acid solution, the sulfuric acid concentration is 20g / L, the liquid-solid ratio is 5:1, and the washing temperature is 55°C, the washing time of stage I is 3h, and the washing time of stages II and III is 1h, filter to obt...

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Abstract

The invention relates to a method for preparing high-grade germanium concentrate from a germanium-containing leaching solution, and belongs to the technical field of hydrometallurgy. The method comprises the steps that the pH value of the germanium-containing leaching solution is adjusted to 2.0-3.5, and a tannin solution with the acidity of 5.0-10.0 g / L is added under the temperature of 50-70 DEGC and stirred for 15-20 min to obtain first tannin-germanium residues after filtering is conducted; 2-4 sections of counter-current washing is conducted on the first tannin-germanium residues by adopting a sulfuric acid solution, and second tannin-germanium residues are obtained after filtering is conducted; the second tannin-germanium residues are dried for 4-8 hours under the temperature of 80-100 DEG C to obtain third tannin-germanium residues; the third tannin-germanium residues are roasted for 3-5 hours under the temperature of 450-600 DEG C to obtain black germanium concentrate. By means of the method, the high-grade germanium concentrate can be prepared, the recovery rate of germanium is 85.0% or above, the germanium content of the germanium concentrate is 35.0%, and the arsenic content of the germanium concentrate is 1.0%; by means of the method, traditional technology process is optimized, the procedures are simple, the recovery rate of the germanium is high, the operation iseasy, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of hydrometallurgy, and in particular relates to a method for preparing high-grade germanium concentrate from germanium-containing leaching solution. Background technique [0002] The crude germanium produced in modern industry is mainly recovered from roasted sphalerite, lead-zinc oxide ore and germanium-containing coal soot or soot. When germanium is extracted from these materials, sulfuric acid leaching is generally used first to obtain germanium-containing leachate, and then germanium is precipitated with tannic acid or tannin extract. The germanium concentrate is then chlorinated and distilled to extract the germanium. [0003] At present, the grade requirement for germanium concentrate on the market is above grade five, that is, the content of germanium is required to be above 15.0%, and the content of arsenic to be below 1.5%. There are many raw materials for extracting germanium. If the germanium c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B1/02C22B3/44C22B41/00
CPCC22B1/02C22B3/44C22B41/00Y02P10/20
Inventor 杨大锦李衍林张候文杨伟代龙果
Owner YUNNAN CHIHONG INT GE CO LTD
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