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Preparation method of germanium dioxide

A technology of germanium dioxide and manganese dioxide, which is applied in the direction of germanium dioxide, etc., can solve the problems of high cost, waste, and low recovery rate of germanium, and achieve the effects of high recovery rate, low use cost, and less residual liquid production

Inactive Publication Date: 2019-02-12
衡阳恒荣高纯半导体材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of germanium in the hydrolyzate after hydrolysis of high-purity germanium tetrachloride is generally 2-4g / L, and this part of germanium cannot be recovered reasonably, resulting in waste. At present, the method of directly adding chlorine salt to the hydrolyzate or adding The hydrochloric acid of equal quality carries out the method recovery wherein germanium, and germanium is recovered in the form of germanium tetrachloride, but the cost of this method is higher, the difficulty is bigger during environmental protection treatment and the recovery rate of germanium is not high

Method used

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Examples

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Effect test

preparation example Construction

[0020] The present invention provides a method for preparing germanium dioxide, which includes the following steps:

[0021] (1) Germanium ore, industrial hydrochloric acid, industrial sulfuric acid, and iron trichloride are added to the chlorination distillation kettle according to the proportions. After heating, a reaction occurs to obtain gas germanium tetrachloride, which is condensed into liquid crude germanium tetrachloride;

[0022] (2) Mix the crude germanium tetrachloride, pure hydrochloric acid, and manganese dioxide in proportions, perform simple distillation, add pure hydrochloric acid and manganese dioxide again, and perform purification distillation to obtain high-purity germanium tetrachloride;

[0023] (3) Transfer the high-purity germanium tetrachloride obtained by rectification and purification to the gasification device, heat the high-purity germanium tetrachloride, and then use high-purity nitrogen to vaporize the high-purity germanium tetrachloride;

[0024] (4) Su...

Embodiment 1

[0034] The present invention provides a method for preparing germanium dioxide, which includes the following steps:

[0035] (1) Add germanium ore, industrial hydrochloric acid, industrial sulfuric acid, and iron trichloride into the chlorination distillation kettle according to the proportions. The solid-liquid ratio of germanium ore and industrial germanium dioxide is 1:4-1 :8, the volume of concentrated sulfuric acid is 2%-5% of hydrochloric acid, and the weight of ferric chloride is 5%-10% of hydrochloric acid. After heating, a reaction occurs to obtain gas germanium tetrachloride, which is condensed into liquid crude tetrachloride Germanium chloride

[0036] (2) Mix the crude germanium tetrachloride, pure hydrochloric acid, and manganese dioxide according to the proportions, where the volume ratio of crude germanium tetrachloride to pure hydrochloric acid is 1:1 to 1:2, perform simple distillation, and add pure hydrochloric acid and Manganese dioxide is purified and distilled...

Embodiment 2

[0043] The present invention provides a method for preparing germanium dioxide, which includes the following steps:

[0044] (1) Add germanium ore, industrial hydrochloric acid, industrial sulfuric acid, and iron trichloride into the chlorination distillation kettle according to the proportions. The solid-liquid ratio of germanium ore and industrial germanium dioxide is 1:4-1 :8, the volume of concentrated sulfuric acid is 2%-5% of hydrochloric acid, and the weight of ferric chloride is 5%-10% of hydrochloric acid. After heating, a reaction occurs to obtain gas germanium tetrachloride, which is condensed into liquid crude tetrachloride Germanium chloride

[0045] (2) Mix the crude germanium tetrachloride, pure hydrochloric acid, and manganese dioxide according to the proportions, where the volume ratio of crude germanium tetrachloride to pure hydrochloric acid is 1:1 to 1:2, perform simple distillation, and add pure hydrochloric acid and Manganese dioxide is purified and distilled...

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PUM

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Abstract

The invention discloses a preparation method of germanium dioxide, and relates to the field of rare metal metallurgy. The preparation method sequentially includes the steps of chlorinating and distilling germanium ore, re-steaming the germanium ore, rectifying and purifying the germanium ore to obtain germanium tetrachloride, hydrolyzing the germanium tetrachloride to prepare germanium dioxide andhydrolysis supernatant, precipitating the hydrolysis supernatant to prepare magnesium germanate filter residues, and distilling the magnesium germanate filter residues to obtain the germanium tetrachloride for reutilization. The preparation method has the advantages of high recovery rate, low use cost, less residual liquid, energy conservation and environment protection.

Description

Technical field [0001] The invention relates to the field of rare metal metallurgy, in particular to a method for preparing germanium dioxide. Background technique [0002] Germanium is a rare and dispersed metal with an abundance of only 4×10-4% in the crust. It mainly occurs in non-ferrous metal mines and coal mines. Except for a very small amount of germanium ore, there is almost no independent germanium ore. . At present, the raw materials for extracting germanium are mainly germanium-enriched materials in various metal smelting processes, germanium-containing coal combustion products and germanium processing wastes. Germanium is mainly used in the electronics industry, optical fiber communications, infrared optics, chemical catalysts, and medical germanium. [0003] Germanium products mainly include: germanium dioxide, high-purity germanium tetrachloride, reduced germanium, high-purity germanium, germanium single crystal, germanium mirror, organic germanium, etc. Germanium ...

Claims

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Application Information

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IPC IPC(8): C01G17/02
Inventor 陈建国聂玉
Owner 衡阳恒荣高纯半导体材料有限公司
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