Method for extracting germanium from fluorine-containing germanium concentrate through distillation

A technology of distillation extraction and germanium concentrate, applied in the field of distillation extraction of germanium, can solve the problems of low production efficiency, increased production cost, increased loss of germanium, etc., and achieve the effects of low cost, high recovery rate and short process

Active Publication Date: 2019-11-15
FIRST RARE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Need to use a large amount of water when washing the germanium concentrate containing fluorine like this, and a large amount of germanium will be dissolved in water simultaneously, in order to reclaim germanium, the dissolved germanium needs to be precipitated, so many and complicated steps will increase the loss of germanium Large, resulting in low production efficiency and a significant increase in production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for distilling and extracting germanium from fluorine-containing germanium concentrate as an embodiment of the present invention, the method comprises the following steps:

[0029] (1) Add 1800L of 10mol / L hydrochloric acid into a 3000L enamel reaction kettle, add alumina as a fluorine-fixing agent, and stir for 30 minutes to obtain a mixed system A;

[0030] (2) Add 200 kg of dried fluorine-containing germanium concentrate into the mixed system A, add 700 L of industrial hydrochloric acid of 10 mol / L to the mixed system A and stir for 1 hour to obtain the reaction system B. After the dried The weight content of fluorine element in the fluorine-containing germanium concentrate is 6.34%, and the weight content of germanium element in the fluorine-containing germanium concentrate after drying is 40.25%. The mass-molar ratio of elements is 1:4;

[0031] (3) The concentration of hydrochloric acid in the detection reaction system B is 6.9mol / L;

[0032] (4) Reacti...

Embodiment 2

[0037] A method for distilling and extracting germanium from fluorine-containing germanium concentrate as an embodiment of the present invention, the method comprises the following steps:

[0038] (1) Add 1800L of 10mol / L hydrochloric acid into a 3000L enamel reaction kettle, add alumina as a fluorine-fixing agent, and stir for 30 minutes to obtain a mixed system A;

[0039] (2) Add 200 kg of dried fluorine-containing germanium concentrate into the mixed system A, add 700 L of industrial hydrochloric acid of 10 mol / L to the mixed system A and stir for 1 hour to obtain the reaction system B. After the dried The weight content of fluorine element in the fluorine-containing germanium concentrate is 6.34%, and the weight content of germanium element in the fluorine-containing germanium concentrate after drying is 40.25%. The mass-molar ratio of elements is 1:8;

[0040] (3) The concentration of hydrochloric acid in the detection reaction system B is 6.9mol / L;

[0041] (4) Reacti...

Embodiment 3

[0046] A method for distilling and extracting germanium from fluorine-containing germanium concentrate as an embodiment of the present invention, the method comprises the following steps:

[0047] (1) Add 1800L of 10mol / L hydrochloric acid into a 3000L enamel reaction kettle, add alumina as a fluorine-fixing agent, and stir for 30 minutes to obtain a mixed system A;

[0048] (2) Add 200 kg of dried fluorine-containing germanium concentrate into the mixed system A, add 700 L of industrial hydrochloric acid of 10 mol / L to the mixed system A and stir for 1 hour to obtain the reaction system B. After the dried The weight content of fluorine element in the fluorine-containing germanium concentrate is 9.46%, and the weight content of germanium element in the fluorine-containing germanium concentrate after drying is 12.81%. The mass-molar ratio of elements is 1:4;

[0049] (3) The concentration of hydrochloric acid in the detection reaction system B is 6.8mol / L;

[0050] (4) Reacti...

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PUM

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Abstract

The invention provides a method for extracting germanium from fluorine-containing germanium concentrate through distillation. The method includes the following steps that a fluorine fixing agent is added into a hydrochloric acid solution to be evenly dispersed, and a mixed system A is obtained, wherein the fluorine fixing agent is an aluminum compound; the fluorine-containing germanium concentrateis added into the mixed system A, stirring is carried out for 0.8 h-1.2 h, and a reaction system B is obtained; after it is confirmed that the concentration of hydrogen chloride in the reaction system B is 6.0 mol/L-8.0 mol/L, chlorine and water vapor are used for carrying out chlorination distillation on the reaction system B; and a gas-state germanium tetrachloride obtained through chlorinationdistillation is condensed. The process method is simple, short in flow path, low in cost and high in recovery rate, the germanium is extracted from the fluorine-containing germanium concentrate safely and environmentally friendly, and the recovery rate of the germanium directly extracted from the fluorine-containing germanium concentrate can reach 99.9%.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for distilling and extracting germanium from fluorine-containing germanium concentrate. Background technique [0002] Germanium is a rare metal element, mostly dispersed in lignite and lead-zinc ore. Most of the extraction methods of germanium are enrichment first and then refining. Germanium concentrates generally contain about 0.5-15% fluorine. Since most of the chlorination distillation reactors use glass-lined reactors and borosilicate glass condensers, during the distillation process of fluorine-containing germanium concentrates, the glass-lined and borosilicate glass condenser. The fluorine-containing germanium concentrate raw material is usually washed with tap water to reduce the fluorine in the germanium concentrate to less than 0.5% as much as possible, and then the obtained germanium concentrate is chlorinated and distilled. Need to use a large amoun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B41/00C22B9/02
CPCC22B41/00C22B9/02Y02P10/20
Inventor 彭伟校陈应红彭永延符积高梁水强刘留朱刘
Owner FIRST RARE MATERIALS CO LTD
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