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Technique for recovering germanium from electric furnace germanium slag

A germanium slag and electric furnace technology is applied in the technical field of recovering germanium from electric furnace germanium slag, which can solve the problems of high processing cost, low production efficiency, difficult operation and the like, and achieves high recovery rate, stable recovery rate and strong operability. Effect

Inactive Publication Date: 2015-08-05
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 chlorination distillation processes are usually used, although this treatment method can obtain high-purity tetrachloride Germanium, but due to the multi-stage distillation method, not only the operation is difficult, but also the production efficiency is low and the processing cost is high

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  • Technique for recovering germanium from electric furnace germanium slag

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Embodiment 1

[0025] 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 100:10:12:4.

[0026] The separation column used is a cylindrica...

Embodiment 2

[0028] In this embodiment, the content of germanium in the germanium slag of electric furnace is 4.93wt%, the content of lead is 30.2wt%, the content of zinc is 12.5wt%, the content of arsenic is 7.12wt%, and the content of copper is 1.65wt%, The content of iron is 18.1, in addition to some other components. Add HCl containing 50g / L, FeCl 20g / L in the reaction kettle 3 , 15g / L of H 2 o 2and an acid solution with the balance of water; then, add 500 g of the above-mentioned electric furnace germanium slag under stirring conditions, and the mass ratio of the acid solution to the electric furnace germanium slag is 10:1; 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 is cooled to room temperature to obtain crude germanium tetrachloride liquid, which is extracted and filtered. The concentration of hydroc...

Embodiment 3

[0030] In this embodiment, the content of germanium in the germanium slag of electric furnace is 5.17wt%, the content of lead is 26.9wt%, the content of zinc is 15.1wt%, the content of arsenic is 8.73wt%, and the content of copper is 1.65wt%, The content of iron is 18.3, in addition to some other components. Add HCl containing 48g / L, FeCl 20g / L in the reaction kettle 3 , 20g / L of H 2 o 2 and an acid solution with the balance of water; then, add 500 g of the above-mentioned electric furnace germanium slag under stirring conditions, and the mass ratio of the acid solution to the electric furnace germanium slag is 10:1; 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 is cooled to room temperature to obtain crude germanium tetrachloride liquid, which is extracted and filtered. The concentration of hydro...

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Abstract

The invention relates to a technique for recovering germanium from electric furnace germanium slag, belonging to the technical field of chemical metallurgy. The technique for recovering germanium from electric furnace germanium slag comprises the following steps: carrying out chlorination distillation on the electric furnace germanium slag, cooling germanium-tetrachloride-containing gas obtained by chlorination distillation to obtain a crude germanium tetrachloride liquid, carrying out primary extraction on the crude germanium tetrachloride liquid by using hydrochloric acid containing saturated chlorine, filtering the germanium tetrachloride liquid obtained by primary extraction through a solid-filled separating column, and carrying out secondary extraction on the filtered germanium tetrachloride liquid by using hydrochloric acid containing saturated chlorine, thereby obtaining refined germanium tetrachloride. The technique has the advantages of controllable process, high operability, high and stable germanium recovery rate and high purity of the recovered germanium, and obviously lowers the cost as compared with the continuous distillation or continuous extraction technique.

Description

technical field [0001] The invention belongs to the technical field of chemical metallurgy, and more specifically, the invention relates to a process for recovering germanium from germanium slag in an electric furnace. 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, bu...

Claims

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Application Information

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IPC IPC(8): C22B41/00C22B7/04
CPCY02P10/20
Inventor 孙玉壮张海岛林明月骈炜金瞰昆孟志强
Owner HEBEI UNIV OF ENG
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