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Method for enriching germanium from low-concentration germanium-containing solution

A low-concentration, solution technology, applied in the field of germanium enrichment, can solve the problems of poor germanium enrichment effect, poor enrichment effect, poor processing effect, etc., achieves good germanium separation effect, easy production and application, and low cost Effect

Active Publication Date: 2014-01-29
SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For the recovery of germanium in the germanium-containing solution, the method of extraction is usually mainly used. For example, the patent CN1552923A discloses a method for enriching germanium with trioctylamine extracted from the germanium-containing acidic solution and back-extracted with NaOH. The extraction rate of germanium can reach 95%-97%, and the enrichment ratio of germanium can reach 15-30 times, but it is only suitable for acidic solutions with Ge content greater than 30mg, and the treatment effect is not good for low-concentration Ge-containing solutions
In addition, some researchers also use the method of precipitation and adsorption to recover germanium from the solution. For example, patent CN101892387A discloses a method for comprehensively recovering germanium in hydrolysis mother liquor and washing water. By adjusting different pH values ​​(pH>7), ferric chloride is fully The germanium in the liquid phase is hydrolyzed and adsorbed, and the germanium-containing filter residue is obtained after filtration. The recovery rate of germanium can reach more than 98.5%, but the process is long and takes more than 72 hours, and it is only applicable to the situation where the solution composition is relatively simple. For multi-metal solution, due to the precipitation of impurity metal ions, it is bound to cause poor germanium enrichment effect
[0004] Therefore, the existing methods for recovering germanium from solutions have many shortcomings, such as narrow application range, long process, poor enrichment effect, etc., and the industry urgently needs to develop new recovery methods for germanium in solutions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Pump 1000ml of a germanium-containing solution with a pH of 3, 12 mg / L germanium, 220 mg / L copper, 326 mg / L zinc, and 48 mg / L iron into the reaction kettle, start stirring, and raise the temperature to 50°C, and then pour into the solution Add 0.2 mol / L sodium silicate solution, and control the ratio of the amount of sodium silicate to Ge to be 12. After the feeding is completed, continue the heat preservation reaction for 2 hours to stop the reaction, vacuum filter, and after the obtained filter residue is dried, about 0.24 g of germanium-rich material can be obtained, which is measured by extraction and separation of benzofluorenone spectrophotometry (GB / T8151.13-2000) In the germanium-rich material, the mass percentage of germanium is about 4.84%, and the recovery rate of germanium can reach 96.32%.

Embodiment 2

[0028] Pump 1000ml of a germanium-containing solution with a pH of 3, 12 mg / L germanium, 220 mg / L copper, 326 mg / L zinc, and 48 mg / L iron into the reaction kettle, start stirring, and raise the temperature to 70°C, and then pour into the solution Add 0.2 mol / L sodium silicate solution, and control the ratio of the amount of sodium silicate to Ge to be 7. After the feeding is completed, continue to keep warm for 3 hours to stop the reaction, vacuum filter, and the obtained filter residue is dried to obtain about 0.17 g of germanium-rich material, which is measured by extraction and separation of benzofluorenone spectrophotometry (GB / T8151.13-2000) Among the germanium-rich materials, the mass percentage of germanium is about 6.34%, and the recovery rate of germanium can reach 91.32%.

Embodiment 3

[0030] Pump 1000ml of a germanium-containing solution with a pH of 3, 12 mg / L germanium, 220 mg / L copper, 326 mg / L zinc, and 48 mg / L iron into the reaction kettle, start stirring, and raise the temperature to 35°C, and then pour into the solution Add 0.25 mol / L sodium metasilicate solution, and control the ratio of sodium metasilicate to Ge to be 18. After the feeding is completed, continue the heat preservation reaction for 2 hours to stop the reaction, vacuum filter, and after the obtained filter residue is dried, about 0.42 grams of germanium-rich material can be obtained, which is measured by extraction and separation of benzofluorenone spectrophotometry (GB / T8151.13-2000) In the germanium-rich material, the mass percentage of germanium is about 2.84%, and the recovery rate of germanium can reach 99.12%.

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Abstract

The invention discloses a method for enriching germanium from a low-concentration germanium-containing solution, and the method is especially suitable for a neutral and acidic complex multicomponent low-concentration germanium-containing solution. According to the invention, a silica gel is generated by adding a silicon reagent to the germanium-containing solution with Ge content less than 30 mg / L; more than 91% of germanium contained in the germanium-containing solution is absorbed and enriched by the silica gel by utilizing the silicon intimate property of the germanium, and then germanium concentrates which contain more than 2% of the germanium are obtained through a filtering reaction solution. The method disclosed by the invention has the advantages of simple technological process, low cost, good separation effect of germanium and other metal ions, high enrichment ratio of the germanium and suitability for industrialized application.

Description

technical field [0001] The invention discloses a method for enriching germanium from a low-concentration germanium-containing solution; it belongs to the technical field of chemical separation. Background technique [0002] Germanium is one of the important scattered metals with unique properties. It is mainly used in the manufacture of semiconductor devices, infrared, optical fibers and chemical catalysts in the electronics industry. It is one of the supporting materials for contemporary high-tech. Because the distribution of germanium is too scattered, its extraction is difficult, so scientific and technological workers have always attached great importance to the extraction of germanium. [0003] For the recovery of germanium in the germanium-containing solution, the method of extraction is usually mainly used. For example, the patent CN1552923A discloses a method for enriching germanium with trioctylamine extracted from the germanium-containing acidic solution and back-e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B41/00
CPCY02P10/20
Inventor 李玉虎张登凯徐毅张伟胡东风曾理
Owner SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY