Method for extracting germanium from germanium-containing smoke dust

A germanium fume and extraction technology, applied in the field of chemical metallurgy, can solve the problems of difficult operation, low production efficiency, high processing cost, and achieve the effects of strong operability, stable recovery rate and cost reduction

Active Publication Date: 2015-07-22
HEBEI UNIV OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

With the continuous expansion of the use of germanium, the purity requirements for germanium, such as germanium tetrachloride, are also getting higher and higher. In the prior art, extraction and leaching distillation processes are usually use

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  • Method for extracting germanium from germanium-containing smoke dust

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Embodiment 1

[0031] In this example, the stationary phase and separation column for filtration are mainly prepared. The stationary phase is prepared by the following method: first, under the condition of 80°C, use 1 mol of hydrochloric acid to acidify the silica gel powder with a particle size of 1 μm, and the treatment time is 12 hours. After cooling to room temperature, filter, wash and Dry the pretreated silica gel powder; then, add the pretreated silica gel powder into a vacuum reactor filled with anhydrous toluene, and then add γ-aminopropyltriethoxysilane dropwise at 60°C , stirred and reacted for 12 h; then added tri-n-octylamine, stirred and reacted for 8 hours; then added methacrylic acid, stirred and reacted for 6 hours; then filtered, washed and dried to obtain the stationary phase; wherein, the pretreatment The mass ratio of silica gel powder, γ-aminopropyltriethoxysilane, tri-n-octylamine and methacrylic acid is 100:10:15:3.

[0032] The separation column used is a cylindrica...

Embodiment 2

[0034] In this embodiment, the content of germanium in the germanium-containing fume is 9.2wt%. Add HCl containing 200g / L, 15g / L H 2 o 2and an acid solution with the balance of water; then, add 500 g of the germanium-containing dust under stirring conditions, and the mass ratio of the acid solution to the germanium-containing dust is 3:1; then pass through chlorine gas at a temperature of 60°C for leaching Until the introduced chlorine no longer absorbs; then the temperature is raised to 90°C, and germanium tetrachloride is distilled to obtain a gas containing germanium tetrachloride. The gas containing germanium tetrachloride was cooled to room temperature to obtain a crude germanium tetrachloride solution, which was extracted and filtered. For the first extraction, 10 mol / L hydrochloric acid containing saturated chlorine was used, the extraction temperature was controlled at 0-10 °C by using a brine bath, and the extraction time was 60 min. The extracted germanium tetrach...

Embodiment 3

[0036] In this embodiment, the content of germanium in germanium-containing fumes is 12.3wt%. Add HCl containing 200g / L, 20g / L H 2 o 2 and an acid solution with the balance of water; then, add 500 g of the germanium-containing dust under stirring conditions, and the mass ratio of the acid solution to the germanium-containing dust is 10:1; then pass through chlorine gas at a temperature of 60°C for leaching Until the introduced chlorine no longer absorbs; then the temperature is raised to 85°C, and germanium tetrachloride is distilled to obtain a gas containing germanium tetrachloride. The gas containing germanium tetrachloride was cooled to room temperature to obtain a crude germanium tetrachloride solution, which was extracted and filtered. For the first extraction, 10 mol / L hydrochloric acid containing saturated chlorine was used, the extraction temperature was controlled at 0-10 °C by using a brine bath, and the extraction time was 60 min. The extracted germanium tetrach...

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Abstract

The invention relates to a method for extracting germanium from germanium-containing smoke dust, and belongs to the technical field of chemical metallurgy. The method adopts the germanium-containing smoke dust, which is obtained by dry distillation of lignite and has the germanium content of 8.0-30.0wt%, as a raw material to perform extraction, and comprises the following steps: performing leaching distillation on the germanium-containing smoke dust; cooling the obtained gas containing germanium tetrachloride to obtain a crude germanium tetrachloride solution; performing first-time extraction on the crude germanium tetrachloride solution; filtering the germanium tetrachloride solution obtained by the first-time extraction by using a separating column; performing second-time filtration on the obtained germanium tetrachloride solution to obtain a refined germanium tetrachloride solution; and hydrolyzing the obtained refined germanium tetrachloride solution into germanium dioxide, and reducing the germanium dioxide to obtain germanium. According to the method provided by the invention, the technological process is easy to control and strong in operability, the germanium recovery rate is stable, the cost is significantly reduced relative to that of a continuous distillation or continuous extraction process, the purity of germanium can reach more than 99.999%, and the resistivity of germanium is more than 15 ohm cm.

Description

technical field [0001] The invention belongs to the technical field of chemical metallurgy, and more specifically, the invention relates to a method for extracting germanium from germanium-containing fumes. Background technique [0002] Germanium, in terms of its ability to conduct electricity, is superior to general non-metals and inferior to general metals, which is called "semiconductor" in physics and plays an important role in the development of solid-state physics and solid-state electronics. For example, the world's first integrated circuit was made of germanium as a substrate. Then germanium was used as a semiconductor material, and the metallurgical technology and purification technology of germanium also developed rapidly. The content of germanium in the earth's crust is 7ppm, and its abundance is higher than that of iodine, silver, gold, arsenic, uranium, mercury and other elements. However, there is almost no relatively concentrated germanium ore, but germanium ...

Claims

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Application Information

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IPC IPC(8): C22B7/02C22B41/00
CPCY02P10/20
Inventor 孙玉壮张海岛林明月骈炜金瞰昆石志祥孟志强
Owner HEBEI UNIV OF ENG
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