Process for producing germanium tetrachloride by regenerated germanium

A germanium tetrachloride and process technology, applied in the field of GeCl4 preparation, can solve the problems of low germanium recovery rate, complex process, high residual acid content in products, etc., and achieve the effects of improving recovery rate, low impurity content and reducing cost

Inactive Publication Date: 2018-08-24
衡阳恒荣高纯半导体材料有限公司
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Problems solved by technology

[0005] The above two traditional preparation techniques have the following disadvantages: (1) the amount of residual acid in the product is large, and germanium is discharged below 50mg / L; (2) the recovery rate of germanium is relatively low, between 90% and 95%; (3) the process Complex operation, high labor intensity, daily production of GeCl 4 (4) There is a large amount of waste acid discharge, which causes serious environmental pollution; (5) High energy consumption and high cost make it difficult to promote and apply on a large scale
Although this method can obtain high-purity germanium tetrachloride with a transition metal impurity content of less than 3ppb and a hydrogen-containing impurity of less than 1ppm through germanium concentrate, the process is very complicated, the energy consumption is high, and the problems such as waste acid pollution are not solved.

Method used

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  • Process for producing germanium tetrachloride by regenerated germanium

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Embodiment 1

[0030] Taking the annual production of 20T area molten germanium ingots of Hengyang Hengrong Semiconductor Materials Co., Ltd. as the raw material of regenerated germanium for the preparation of germanium tetrachloride, an example is given.

[0031] Prepare the hydrochloric acid solution that concentration is 6mol / L in reactor, and add ferrous chloride, the mass percentage concentration of ferrous chloride in hydrochloric acid solution is 10%. Add the regenerated germanium powder into the reaction kettle. The amount of germanium powder added is 20% of the mass of the hydrochloric acid solution. The particle size of the germanium powder meets a 100-mesh sieve and the pass rate reaches more than 98%. Stir for 40 minutes to make the solution system mix evenly and control the reaction. The temperature in the kettle is 30°C, and then chlorine gas is continuously fed into the hydrochloric acid solution for reaction. The amount of chlorine gas introduced is calculated according to the...

Embodiment 2

[0033] Taking the annual production of 20T area molten germanium ingots of Hengyang Hengrong Semiconductor Materials Co., Ltd. as the raw material of regenerated germanium for the preparation of germanium tetrachloride, an example is given.

[0034] Prepare the hydrochloric acid solution that concentration is 7mol / L in reactor, and add ferrous chloride, the mass percentage concentration of ferrous chloride in hydrochloric acid solution is 9%. Add the regenerated germanium powder into the reaction kettle. The amount of germanium powder added is 40% of the mass of the hydrochloric acid solution. The particle size of the germanium powder meets the 100-mesh sieve and the pass rate reaches more than 98%. Stir for 60 minutes to make the solution system mix evenly and control the reaction. The temperature in the kettle is 50°C, and then chlorine gas is continuously introduced into the hydrochloric acid solution for reaction. The amount of chlorine gas introduced is calculated accordin...

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Abstract

The invention discloses a process for producing germanium tetrachloride by regenerated germanium. According to the process, regenerated germanium raw materials are added into hydrochloric acid solution containing FeCl2 catalysts, chlorine is continuously led in to perform chlorination, and germanium tetrachloride products are recovered by distillation separation after chlorination. The process issimple and low in energy consumption and cost, waste acid closed recycling is effectively realized, environmental problems are solved, the recovery rate of the regenerated germanium raw materials is increased, and higher economic values are generated.

Description

technical field [0001] The invention relates to a preparation process of germanium tetrachloride, in particular to a process for preparing GeCl by using regenerated germanium raw material through catalytic chlorination of ferric dichloride 4 The new technology belongs to GeCl 4 Preparation technology field. Background technique [0002] In prior art, GeCl 4 It is mainly prepared by using regenerated germanium raw materials for the preparation of GeCl 4 Germanium accounts for 70-80% of the total annual production of germanium. Recycling germanium in secondary germanium to produce GeCl 4 The traditional craft mainly includes the following two kinds: [0003] 1) the caustic soda NaOH and H 2 o 2 、H 2 O, according to the mass ratio of 1:2:1, is heated, melted and oxidized by steam to produce sodium metagermanate, then neutralized with sulfuric acid to acidity, and distilled with hydrochloric acid to produce germanium tetrachloride. [0004] 2) Regenerated germanium raw ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
Inventor 陈建国
Owner 衡阳恒荣高纯半导体材料有限公司
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