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Method for recycling germanium from germanium-containing glass

A germanium glass and sodium germanium technology, applied in the field of germanium recovery, can solve the problems of high silicon dioxide content, difficult separation of germanium and silicon, heavy environmental pollution, etc., and achieve the effects of large specific surface area, reduced environmental pollution, and good dispersion performance.

Active Publication Date: 2014-03-05
湖北拓材再生资源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional methods of recovering germanium mainly include: chlorination direct distillation, alkali leaching and alkali roasting, etc., but there are disadvantages such as high energy consumption, heavy environmental pollution, low recovery rate of germanium, and high recovery cost.
The fundamental reason is that the silicon dioxide content in this type of germanium-containing glass is high, and the separation of germanium and silicon is difficult.

Method used

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  • Method for recycling germanium from germanium-containing glass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] combine figure 1 As shown, 500kg of germanium-containing glass was weighed to obtain 200-mesh germanium-containing glass powder containing 0.82% germanium after coarse crushing, medium crushing, and fine grinding. Add 2500kg of NaOH aqueous solution with a mass percentage concentration of 20% to the germanium-containing glass powder, add the germanium-containing glass powder and sodium hydroxide in the NaOH aqueous solution at a ratio of 1:1, and heat it to 130°C with a steam pressure reactor. Insulated and reacted for 9 hours to obtain a mixed solution of sodium silicate and sodium germanate. Dilute the resulting mixed solution of sodium silicate and sodium germanate with water until the molar concentration of sodium silicate is 0.5M, then add 5% electrolyte sodium chloride to it by weight of the diluted solution, and then adjust the pH value to 8.0 with hydrochloric acid , after aging for 2 hours, solid-liquid separation, solid drying to obtain high-purity amorphous ...

Embodiment 2

[0028] 200-mesh germanium-containing glass powder containing about 0.93% germanium is obtained by weighing 300kg of germanium-containing glass through coarse crushing, medium crushing, and fine grinding. Add 1500kg of NaOH aqueous solution with a mass percentage concentration of 10% to the germanium-containing glass powder, the mass ratio of the germanium-containing glass powder to sodium hydroxide in the NaOH aqueous solution is 2:1, heat it to 200°C with an electric heating pressure reactor, and keep it warm for 5 Hours, a mixed solution of sodium silicate and sodium germanate was obtained. Dilute the resulting mixed solution of sodium silicate and sodium germanate with water until the molar concentration of sodium silicate is 0.2 M, then add 10% electrolyte sodium bromide of the weight of the diluted solution to it, and then neutralize it to the pH value with hydrochloric acid After aging for 2 hours, the solid and liquid were separated, and the solid was dried to obtain hi...

Embodiment 3

[0030] 200-mesh germanium-containing glass powder containing 1.63% germanium is obtained by taking 500kg of germanium-containing glass through coarse crushing, medium crushing and fine grinding. Add 2200kg of NaOH aqueous solution with a mass percentage concentration of 15% to the germanium-containing glass powder, and the mass ratio of the germanium-containing glass powder to sodium hydroxide in the NaOH aqueous solution is 1.5:1. Heat it to 150°C with an electric heating pressure reactor, and heat preservation reaction for 8 hours, a mixed solution of sodium silicate and sodium germanate was obtained. Dilute the mixed solution of sodium silicate and sodium germanate with water until the molar concentration of sodium silicate is 1M, then add electrolyte potassium bromide of 20% of the solution weight after dilution, and then adjust the pH value to 9.0 with hydrochloric acid. After aging for 2 hours, the solid and liquid were separated, and the solid was dried to obtain high-p...

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Abstract

The invention discloses a method for recycling germanium from germanium-containing glass, which comprises the following steps: 1) pulverizing germanium-containing glass into germanium-containing glass powder, adding an alkali solution into the germanium-containing glass powder, heating to 120-300 DEG C, and keeping the temperature for 1-10 hours to obtain a water solution containing sodium silicate and sodium germanate; 2) adding an alkali metal salt into the water solution containing sodium silicate and sodium germanate obtained in the step 1), regulating the pH value to 6-9, aging, carrying out solid-liquid separation, drying the solid to obtain amorphous silicon dioxide, and recycling; 3) adding magnesium chloride into the solution obtained by solid-liquid separation in the step 2) to obtain a precipitate containing magnesium germanate; and 4) mixing the precipitate containing magnesium germanate with hydrochloric acid, carrying out chlorination distillation, condensing to collect germanium tetrachloride, and hydrolyzing the germanium tetrachloride to obtain germanium dioxide. The method abandons the pyrogenic process for recycling high-silicon germanium-containing waste, lowers the energy consumption, reduces the environmental pollution, and has the advantages of simple technique, high germanium recycling rate and low recycling cost.

Description

technical field [0001] The invention relates to a germanium recovery process, in particular to a method for recovering germanium from germanium-containing glass. Background technique [0002] Germanium is an important scattered metal and the most important semiconductor material besides silicon. It has extensive and important applications in various fields such as infrared optics, optical fiber communication, aerospace, chemical catalysts, solar cells, and biomedicine. On the other hand, the resources of germanium in the world are relatively poor. The proven reserves of germanium metal in the world are about 8,600 tons, and the global reserves are only enough for 40 years. Now most developed countries are vigorously developing aerospace technology and new energy technology, and the sustainable development of these technologies is inseparable from the application of germanium. As my country's economy continues to develop at a high speed, the level of science and technology c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B41/00C22B3/12C22B3/44
CPCY02P10/20
Inventor 谈发堂
Owner 湖北拓材再生资源有限公司
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