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Production process for transforming tetragonal crystal germanium oxide into hexagonal acid soluble germanium

A technology of tetragonal crystal form and production process, applied in the field of metallurgy, can solve the problems of poor purity and difficult use

Inactive Publication Date: 2019-02-22
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

[0004] Germanium dioxide has two crystal forms, among which, tetragonal germanium dioxide is insoluble in water and is difficult to make better use of
Moreover, the purity of tetragonal germanium dioxide is poor, and most of them will be doped with various impurities. At present, there is no effective way to convert it into another crystal form.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The production process for converting tetragonal germanium oxide into hexagonal acid-soluble germanium comprises the following steps:

[0031] The first step is to take the raw material containing tetragonal germanium oxide, put it into the reaction kettle, add water, the mass volume ratio of raw material and water is 1kg: 15L, and then add sodium hydroxide therein, and the weight of sodium hydroxide is equal to that of the raw material. The weight ratio is 0.3:1, sodium hydroxide is added in three times, 1 / 5 of the total weight is added for the first time, it is added at the beginning of the reaction, 1 / 2 of the total weight is added for the second time, and it is added after 30 minutes of reaction. Add all the rest for the third time, and add it after 1.5 hours of reaction. The step-by-step addition method can ensure that the germanium oxide in the raw material is fully dissolved by alkali. Stir at a rate of 60 rpm to control the reaction temperature of the reactor. 8...

Embodiment 2

[0038] The production process for converting tetragonal germanium oxide into hexagonal acid-soluble germanium comprises the following steps:

[0039] The first step is to take the raw material containing tetragonal germanium oxide, put it into the reaction kettle, add water, the mass volume ratio of raw material and water is 1kg: 18L, and then add sodium hydroxide therein, and the weight of sodium hydroxide is equal to that of the raw material. The weight ratio is 0.7:1. Sodium hydroxide is added in three times, 1 / 5 of the total weight is added for the first time, it is added at the beginning of the reaction, 1 / 2 of the total weight is added for the second time, and it is added after 30 minutes of reaction. Add all the rest for the third time, and add it after 1.5 hours of reaction. The step-by-step addition method can ensure that the germanium oxide in the raw material is fully dissolved by alkali. Stir at a rate of 60 rpm to control the reaction temperature of the reactor. 8...

Embodiment 3

[0046] The production process for converting tetragonal germanium oxide into hexagonal acid-soluble germanium comprises the following steps:

[0047]The first step is to take the raw material containing tetragonal germanium oxide, put it into the reaction kettle, add water, the mass volume ratio of raw material and water is 1kg:16L, and then add sodium hydroxide therein, and the weight of sodium hydroxide is equal to that of raw material The weight ratio is 0.5:1, sodium hydroxide is added in three times, 1 / 5 of the total weight is added for the first time, it is added at the beginning of the reaction, 1 / 2 of the total weight is added for the second time, and it is added after 30 minutes of reaction. Add all the rest for the third time, and add it after 1.5 hours of reaction. The step-by-step addition method can ensure that the germanium oxide in the raw material is fully dissolved by alkali. Stir at a rate of 60 rpm to control the reaction temperature of the reactor. 83°C, re...

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Abstract

The invention discloses a production process for transforming tetragonal crystal germanium oxide into hexagonal acid soluble germanium. The process includes the steps: firstly, adding a raw material containing the tetragonal crystal germanium oxide into a reaction kettle, adding water into the reaction kettle, adding sodium hydroxide into the reaction kettle, and performing stirring reaction for 2-3 hours; secondly, heating and evaporating a material acquired in the first step to obtain concentrated solution, cooling the concentrated solution, and adjusting pH (potential of hydrogen) to reach4.5-6.0 by the aid of hydrochloric acid; thirdly, adding sodium chlorate, uniformly stirring mixture, and heating and stirring the mixture for 3-5 hours; fourthly, adding the hydrochloric acid into the material acquired in the third step, heating and distilling mixture, and collecting fraction; fifthly, adding the fraction into distilled water with the volume of 6.5 times, stirring mixture for 2-3hours, standing the mixture for a period of time, leading oxygen into the reaction kettle during standing to generate precipitate, washing the precipitate by the aid of cold water until washing liquid does not contain chloride ions, and drying the washed precipitate at the temperature of 200 DEG C to obtain the hexagonal acid soluble germanium. The tetragonal crystal germanium oxide is transformed into the hexagonal acid soluble germanium by the aid of the reasonable process.

Description

technical field [0001] The invention relates to the technical field of metallurgy, in particular to a production process for converting tetragonal germanium oxide into hexagonal acid-soluble germanium. Background technique [0002] The chemical properties of germanium are stable, and it does not interact with air or water vapor at room temperature, but it will quickly form germanium dioxide at 600-700 °C. It does not work with dilute sulfuric acid and hydrochloric acid, but when heated in concentrated sulfuric acid, germanium will slowly dissolve. Germanium is easily soluble in nitric acid and aqua regia. The action of germanium and alkaline solution is very weak, but the molten alkali can quickly dissolve germanium in the air. Germanium does not interact with carbon, so germanium is melted in a graphite crucible without contamination by carbon. [0003] Germanium dioxide is widely used in industrial production and science and technology fields. Such as optical phosphor,...

Claims

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Application Information

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IPC IPC(8): C01G17/02
CPCC01G17/02
Inventor 陈建国聂玉
Owner 衡阳恒荣高纯半导体材料有限公司