Process for producing germanium tetrachloride by regenerated germanium

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 ...

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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.

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