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Method for extracting GeCl4 from smoke dust containing Ge

A germanium fume, microwave heating technology, applied in germanium halide and other directions, can solve the problems of large discharge of harmful waste liquid, slow heating of steam heating, unstable temperature control, etc., to improve recovery rate, fast heating speed, and reduce energy consumption Effect

Inactive Publication Date: 2016-10-26
INNER MONGOLIA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This enrichment and purification method has the following defects: (1) steam heating is slow, uneven heating, and high energy consumption; (2) temperature control is unstable and fluctuates greatly, and some impurities in germanium dust, such as arsenic, will be distilled into GeCl 4 Medium; (3) The time is long; (4) The consumption of hydrochloric acid is large, and the discharge of harmful waste liquid is large

Method used

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  • Method for extracting GeCl4 from smoke dust containing Ge
  • Method for extracting GeCl4 from smoke dust containing Ge
  • Method for extracting GeCl4 from smoke dust containing Ge

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The composition content of germanium-containing fume is shown in Table 1:

[0029] Table 1 Composition of germanium-containing raw materials / %

[0030]

[0031] Such as figure 2 , dry the germanium-containing fumes at 50°C for 24h, then mix the germanium-containing fumes and 8mol / L hydrochloric acid in a ratio of 1:1.25 by weight and add them to the three-necked flask 101, and place the middle bottle of the three-necked flask 101 The mouth is connected with the condensation pipe 300, and the condensed water enters the condensation pipe 300 from the condensed water inlet 301, and is discharged from the condensation pipe outlet 302. A bottle mouth of the three-necked flask 101 is inserted into a gas stirring tube 102, and the gas stirring tube 102 is connected with a nitrogen tank. Put the three-necked flask 101 and the gas stirring tube 102 into a microwave oven. Insert a thermocouple 201 into the other mouth of the three-diameter flask 101, connect it to the micr...

Embodiment 2

[0033] Such as figure 2 , dry germanium-containing fumes at 40°C for 16h, then mix germanium-containing fumes and 8.5mol / L hydrochloric acid in a ratio of 1:5 by weight, and mix in potassium permanganate, the weight of potassium permanganate is 4.5% by weight of germanium soot. After mixing, add it to the three-necked flask 101 and connect the mouth of the three-necked flask 101 to the condenser tube 300 . A bottle mouth of the three-necked flask 101 is inserted into a gas stirring tube 102, and the gas stirring tube 102 is communicated with air. Put the three-necked flask 101 and the gas stirring tube 102 into a microwave oven. A thermocouple 201 is inserted into the other mouth of the three-diameter flask 101, connected to the microwave controller 202 through the thermocouple 201, the heating rate of the microwave oven is set to 8°C / min, the heating temperature is 105°C, and the holding time is 60min. Air was introduced into the flask 101 for extraction. The extracted p...

Embodiment 3

[0035] Such as figure 2 , dry the germanium-containing dust at 30°C for 30h, then mix the germanium-containing dust with 9mol / L hydrochloric acid in a weight ratio of 1:13.5, and mix in potassium permanganate, the weight of potassium permanganate is the weight of the germanium-containing dust 7.5% of the mixture was added to the three-necked flask 101 after mixing. The mouth of the three-diameter flask 101 is connected to the condenser pipe 300 , and the condensed water enters the condenser pipe 300 from the condensed water inlet 301 and is discharged from the condenser pipe outlet 302 . A gas stirring tube 102 is inserted into one mouth of the three-necked flask 101 . Put the three-necked flask 101 and the gas stirring tube 102 into a microwave oven, and the gas stirring tube 102 is connected with an argon tube. A thermocouple 201 is inserted into the other mouth of the three-diameter flask 101, connected to the microwave controller 202 through the thermocouple 201, the he...

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Abstract

The invention relates to a method for extracting GeCl4 from smoke dust containing Ge. The method comprises following steps: material mixing: the smoke dust containing Ge and HCl are mixed in a weight ratio being (1:1.25)-(1:13.5); microwave heating: the mixed materials are subjected to microwave heating to reach the GeCl4 distillation temperature or higher for distillation, and stirring is performed simultaneously; collecting: products after distillation are collected, and GeCl4 is obtained. The method for extracting GeCl4 from the smoke dust containing Ge is uniform in heating, high in heating speed, good in controllability, energy-saving and efficient and can accelerate the chemical reaction, thereby accelerating the distillation process, reducing the use amount of HCl, reducing energy consumption and emission and increasing the recovery rate of Ge.

Description

technical field [0001] The invention relates to a method for extracting GeCl from germanium-containing dust 4 Methods. Background technique [0002] The Ulan Tuga Coal Mine in Xilingol League, Inner Mongolia, has a huge reserve of lignite resources, which is the largest germanium mine in my country. Germanium resources are associated with lignite. After the lignite is ground and dried, it is added to the vortex furnace for combustion to provide heat and generate electricity. During the combustion process, a bag filter is used to collect the dust, and the content of germanium in the dust is relatively high, reaching about 1%. This kind of dust factory is called germanium dust. The content of germanium in germanium dust is low and needs to be further enriched and purified. The current enrichment and purification method is: put germanium dust and concentrated hydrochloric acid with a mass ratio of 1:3.5 into a reactor, heat it to 90°C to 110°C with steam, and keep it warm for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/04
CPCC01G17/04
Inventor 彭军刘丽霞张磊安胜利李文挺薛应东刘伟张雷涛
Owner INNER MONGOLIA UNIV OF SCI & TECH
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