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Method for removing fluorine from germanium-containing material

A material and removal technology, applied in the field of germanium-containing material removal of fluorine, can solve the problems of low internal temperature, complicated operation, crystal transformation, etc., and achieve the effect of avoiding transformation and uniform heating

Inactive Publication Date: 2019-08-02
SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this fire process, since the heating components of the muffle furnace are exposed in the gas phase, the heating components have a short life under high temperature conditions and need to be replaced frequently, which makes the operation more cumbersome; moreover, the volatile tail gas needs to be absorbed by lye, and the procedure is complicated; in addition , when calcined in a muffle furnace, the heat gradually reaches the interior from the surface of the germanium-containing material through heat conduction, so that the surface temperature of the germanium-containing material is high, while the internal temperature is low, and the overall temperature is uneven, thereby generating stress inside, which may cause The crystal form of germanium changes, and germanium cannot enter the solution in the subsequent distillation and chlorination process, resulting in a decrease in the recovery rate of germanium

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The method for removing fluorine from germanium-containing materials of the present invention comprises the following steps:

[0018] (1) Microwave drying: 50 kg of germanium-containing materials containing 43.26% germanium, 14.23% fluorine and 68.43% moisture are evenly divided into 8 corundum saggers, and then the corundum saggers are evenly placed In the microwave drying oven, set the microwave temperature to 120°C and the time to 1h through the PLC control program of the microwave drying oven, turn on 4 magnetrons of the microwave drying oven, set the microwave frequency to 2400MHz, the microwave power to 2000W, and the rotation speed of the turntable to be controlled as 2r / min, dry the germanium-containing material at 120°C for 1h. At the same time, open the tail gas discharge valve of the microwave drying oven, control the opening to 1 / 3, and recover the water vapor to the tail gas absorption tower.

[0019] (2) Microwave calcination: after 1 hour, the temperatur...

Embodiment 2

[0023] The method for removing fluorine from germanium-containing materials of the present invention comprises the following steps:

[0024] (1) Microwave drying: 35 kg of germanium-containing materials containing 53.24% germanium, 15.46% fluorine, and 58.46% moisture are evenly divided into 6 corundum saggers, and then the corundum saggers are evenly placed In the microwave drying oven, set the temperature to 200°C and the time to 1h through the PLC control program, turn on 4 magnetrons of the microwave drying oven, set the power to 2000W, and control the rotating speed of the turntable to 1r / min, so that the germanium-containing material is at 200°C Dry for 1h. At the same time, open the tail gas discharge valve of the microwave drying oven, control the opening to 1 / 3, and recover the water vapor to the tail gas absorption tower.

[0025] (2) Microwave calcination: after 1 hour, the temperature was raised to 450°C and the calcination time was set to 0.5h, and the dried germ...

Embodiment 3

[0029] After the fluoride is heated, the fluorine element in it decomposes into fluorine gas and separates from the germanium-containing material, and then the fluorine gas needs to enter the exhaust gas absorption tower for purification and absorption, so it is necessary to set up a pipeline between the microwave equipment and the exhaust gas absorption tower. There may be leakage issues in . If the fluorine gas is absorbed and fixed immediately after leaving the germanium-containing material, there is no need to set up complicated pipelines, which not only saves space, simplifies equipment, but also prevents fluorine gas from leaking in the pipeline. Therefore, the applicant tried to fix the fluorine gas immediately after it separated from the germanium-containing material. The specific defluorination method is as follows:

[0030] (1) Microwave drying: 35 kg of germanium-containing materials containing 53.24% germanium, 15.46% fluorine, and 58.46% moisture are evenly divide...

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PUM

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Abstract

The invention provides a method for removing fluorine from a germanium-containing material. The germanium-containing material is calcined under the microwave condition and is subjected to air pumping.The germanium-containing material is calcined by microwave, the inside and the outside of the germanium-containing material are heated simultaneously by microwave, so that the inside and the outsideof the germanium-containing material are heated uniformly and transformation of germanium crystal form is avoided; meanwhile, fluorine elements distributed in the germanium-containing material are decomposed and volatized uniformly, and the fluorine content of the germanium-containing material after calcination is reduced to be below 0.5 percent.

Description

technical field [0001] The invention relates to the technical field of rare metal smelting, in particular to a method for removing fluorine from germanium-containing materials. Background technique [0002] At present, the production of germanium dioxide mainly adopts chlorination distillation process, and hydrochloric acid, fluorinating agent, oxidizing agent, etc. are used to process germanium-containing lead-zinc ore, germanium-containing coal, iron ore, and other intermediate materials of non-ferrous smelting to obtain germanium-containing Chlorides, other metal chlorides, silicates, fluorides, metal oxides and non-metal oxides containing germanium materials, then purified by rectification, washed with high-purity hydrochloric acid to obtain high-purity germanium tetrachloride, and finally used high-purity water Germanium tetrachloride is hydrolyzed to obtain high-purity germanium dioxide. There is a lot of fluoride in germanium-containing materials, and fluorine severe...

Claims

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Application Information

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IPC IPC(8): C22B41/00C22B1/02
CPCC22B1/02C22B41/00
Inventor 张登凯吴才贵张伟张俊峰曾日明周科华
Owner SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY
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