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Method for green production of germanium tetrachloride from germanium mud

A germanium tetrachloride and green production technology, applied in the direction of germanium halide, etc., can solve the problems of blocked pipelines and low direct yield, achieve uniform heating speed, improve reaction efficiency, and improve mixing effect

Pending Publication Date: 2021-02-19
云南驰宏国际锗业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of method of green production germanium tetrachloride from germanium mud, adopt hydrogen peroxide oxidation-hydrochloric acid chlorination distillation method to produce germanium tetrachloride, this technique uses hydrogen peroxide solution as oxidant, distillation residual The liquid does not contain solid waste residue, which will not cause blockage of the production pipeline. The production process is assisted by ultrasonic vibration and microwave heating, and the reaction process is completed in the oxidation kettle and the distillation kettle respectively. Precise control improves the production of tetrachloride from germanium mud. The direct recovery rate of germanium solves the problem that the existing iron trichloride oxidation-hydrochloric acid chlorination distillation process is prone to produce a large amount of acid-containing ferrous chloride waste residue. low rate problem

Method used

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Effect test

Embodiment 1

[0024] The invention is a method for green production of germanium tetrachloride from germanium mud, comprising the following steps:

[0025] S1: germanium mud pretreatment, the germanium mud is ground into fine particles through a ball mill, and the particle size of germanium mud grinding is set to 80-100 mesh;

[0026] S2: Slurry germanium and heat, the germanium slurry ground in S1 is mixed with water at a ratio of 1:3, that is, 1kg of germanium slurry is added to 3L of water, and then microwave heating is used to raise the temperature to 65°C and keep it warm 3min, the heating rate is set at 8~10℃ / min;

[0027] S3: Add 35% hydrogen peroxide solution dropwise for oxidation, slowly add 35% hydrogen peroxide solution dropwise to the slurry after heat preservation in S2, germanium mud and 35% hydrogen peroxide solution are added in a ratio of 1:3, that is, 1 kg Add 3L35% hydrogen peroxide solution to the germanium mud, and add sodium hydroxide during the whole reaction proces...

Embodiment 2

[0031] The invention is a method for green production of germanium tetrachloride from germanium mud, comprising the following steps:

[0032] S1: germanium mud pretreatment, the germanium mud is ground into fine particles through a ball mill, and the particle size of germanium mud grinding is set to 80-100 mesh;

[0033] S2: Slurry germanium and heat, the germanium slurry ground in S1 is mixed with water at a ratio of 1:3.5, that is, 1kg of germanium slurry is added to 3.5L of water, and then microwave heating is used to raise the temperature to 62.5°C, and Keep warm for 4 minutes, and set the heating rate at 8-10°C / min;

[0034] S3: Add 35% hydrogen peroxide solution dropwise for oxidation, slowly add 35% hydrogen peroxide solution dropwise to the slurry after heat preservation in S2, germanium mud and 35% hydrogen peroxide solution are added in a ratio of 1:3.5, that is, 1 kg Add 3.5L 35% hydrogen peroxide solution to the germanium mud, and add sodium hydroxide during the w...

Embodiment 3

[0038] The invention is a method for green production of germanium tetrachloride from germanium mud, comprising the following steps:

[0039] S1: germanium mud pretreatment, the germanium mud is ground into fine particles through a ball mill, and the particle size of germanium mud grinding is set to 80-100 mesh;

[0040] S2: Slurry germanium and heat. Add water to slurry the ground germanium slurry in S1 at a ratio of 1:4, that is, add 4L water to 1㎏ germanium slurry, and then use microwave heating to raise the temperature to 60°C and keep it warm. 5min, the heating rate is set at 8-10°C / min;

[0041] S3: Add 35% hydrogen peroxide solution dropwise for oxidation, slowly add 35% hydrogen peroxide solution dropwise to the slurry after heat preservation in S2, germanium mud and 35% hydrogen peroxide solution are added in a ratio of 1:4, that is, 1 kg Add 4L 35% hydrogen peroxide solution to the germanium mud, and add sodium hydroxide during the whole reaction process to keep the...

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Abstract

The invention discloses a method for green production of germanium tetrachloride from germanium mud, and relates to the technical field of chemical production. The method comprises the following steps: S1, pretreating germanium mud; S2, slurrying and heating the germanium mud; S3, dropwise adding a 35% hydrogen peroxide solution for oxidation; S4, conducting filter pressing and drying; and S5, adding hydrochloric acid for distillation. Germanium tetrachloride is produced by adopting a hydrogen peroxide oxidation and hydrochloric acid chlorination distillation method, a hydrogen peroxide solution is used as an oxidizing agent in the process, distillation raffinate does not contain solid waste residues, a production pipeline is not blocked, the production process is assisted by ultrasonic oscillation and microwave heating, and the reaction process is completed in an oxidation kettle and a distillation kettle. The direct recovery rate of germanium tetrachloride produced from germanium mudis increased through accurate control, and the problems that a large amount of acid-containing ferrous chloride waste residues are easily generated in an existing ferric trichloride oxidation and hydrochloric acid chlorination distillation process, a large amount of crystals are separated out to block a pipeline after distillation raffinate is cooled, and the direct recovery rate is not high aresolved.

Description

technical field [0001] The invention belongs to the technical field of chemical production, in particular to a method for green production of germanium tetrachloride from germanium mud. Background technique [0002] Germanium tetrachloride can be used as an optical fiber dopant, can be used to make germanium dioxide, etc., to produce germanium tetrachloride from germanium mud, the traditional process is to use ferric chloride oxidation-hydrochloric acid chlorination distillation, the process treatment The direct recovery rate of germanium mud is not high, only 92%. After distillation, a large amount of acid-containing ferrous chloride waste residue is produced, which needs to be processed at a large cost. Ferric chloride is difficult to regenerate. After the distillation raffinate is cooled, there is a large amount of The crystals precipitated and blocked the pipeline, causing the production to be unable to proceed normally. [0003] Therefore it is necessary to improve the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
CPCC01G17/04
Inventor 崔丁方朱家义何兴军朱恩福李恒方杨金彩子光平陈知江廖吉伟周雪娟
Owner 云南驰宏国际锗业有限公司
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