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Preparation method of germanium dioxide powder

A germanium dioxide and powder technology, which is applied in the field of semiconductor oxide preparation technology, can solve the problems of entering the surrounding environment, increase production costs, environmental pollution, etc., and achieve the effects of being environmentally friendly, reducing washing water, and reducing production costs.

Pending Publication Date: 2020-08-04
湖北联合贵稀资源再生科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing production of germanium dioxide is mainly prepared by hydrolysis of germanium tetrachloride. The main process includes hydrolysis of germanium tetrachloride, suspension of germanium dioxide, solid-liquid separation, and germanium dioxide filter cake containing hydrochloric acid. The germanium dioxide filter cake is washed with high-purity water or distilled water for many times to obtain a germanium dioxide filter cake containing a small amount of hydrogen chloride. During the washing process, the water consumption is generally 40-80 times the mass of germanium dioxide, and some germanium dioxide Dissolved in dilute hydrochloric acid to become germanium-containing mother liquor, this part of germanium-containing mother liquor needs to be recovered by methods such as neutralization or precipitation, which will increase production costs, and in the process of filtration or operation, part of germanium tetrachloride in the solution will be Volatilizes and enters the surrounding environment, causing pollution to the environment and at the same time causing loss of germanium, so there is an urgent need for a preparation method that is simpler, lower in cost, and less in loss of germanium tetrachloride

Method used

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  • Preparation method of germanium dioxide powder

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preparation example Construction

[0023] The preparation method of the germanium dioxide powder provided in the following examples uses germanium tetrachloride hydrolysis to obtain a germanium dioxide suspension, solid-liquid separation to obtain a germanium dioxide filter cake, and then germanium dioxide filter cake. The germanium dioxide powder is obtained by drying and pulverizing, which greatly reduces the water consumption for washing the filter cake of germanium dioxide. The escape and loss of germanium. At the same time, the germanium tetrachloride obtained after the germanium-containing acid gas is condensed and the germanium-containing acidic solution are recycled, the germanium tetrachloride is returned to the hydrolysis system for hydrolysis, and the germanium-containing acidic solution can be returned to the germanium leaching process for production or The germanium contained therein is recovered by using methods such as tannin precipitation and extraction, so as to overcome the shortcomings of the...

Embodiment 1

[0026] A kind of preparation method of germanium dioxide powder, see figure 1 As shown, add 40L of secondary reverse osmosis high-purity water to the 100L enamel hydrolysis kettle, put -10°C ethylene glycol freezing liquid into the interlayer of the enamel kettle, start the agitator to stir, and start to use the peristaltic pump to pump the high-purity water when the water temperature drops to 10°C Add germanium tetrachloride, flow rate is 80ml / min, after 10L germanium tetrachloride is all added, continue to stir for 30min, obtain the suspension of germanium tetrachloride, utilize vacuum filtration, obtain the mother liquor containing germanium and germanium dioxide Wet filter cake, transfer the wet filter cake into an electric heating drying oven at a drying temperature of 200° C., and pulverize the dried germanium dioxide with a pulverizer to obtain germanium dioxide powder.

[0027] During the drying process, germanium-containing acid gases including hydrogen chloride, germ...

Embodiment 2

[0032] A kind of preparation method of germanium dioxide powder, see figure 1 As shown, add 60L of secondary reverse osmosis high-purity water to the 100L enamel hydrolysis kettle, put -10°C ethylene glycol freezing liquid into the interlayer of the enamel kettle, start the stirrer to stir, and start to use the peristaltic pump to pump the high-purity water when the water temperature drops to 0°C Add germanium tetrachloride at a flow rate of 50ml / min. After 10L of germanium tetrachloride is added, continue to stir for 30 minutes to obtain a suspension of germanium tetrachloride. Vacuum filtration is used to obtain germanium-containing mother liquor and germanium dioxide. Wet filter cake, transfer the wet filter cake into an electric heating drying oven at a drying temperature of 300° C., and pulverize the dried germanium dioxide with a pulverizer to obtain germanium dioxide powder.

[0033] During the drying process, germanium-containing acid gases including hydrogen chloride,...

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Abstract

The invention discloses a preparation method of germanium dioxide powder, and relates to the technical field of semiconductor oxide preparation. The preparation method specifically comprises the following steps: uniformly adding germanium tetrachloride liquid into high-purity water or secondary distilled water with the temperature of 0-10 DEG C, stirring for hydrolysis reaction to form turbid liquid, performing solid-liquid separation to obtain a germanium dioxide filter cake and germanium-containing mother liquor, and drying and crushing the germanium dioxide filter cake to obtain the germanium dioxide powder, wherein germanium-containing acid gas generated in the drying process of germanium dioxide is subjected to secondary condensation recovery, acid germanium-containing waste liquid returns to germanium extraction production, and the germanium tetrachloride returns to hydrolysis production of the germanium dioxide. According to the method, the traditional germanium tetrachloride hydrolysis, repeated washing and drying processes are abandoned, so that the washing water of the germanium dioxide filter cake is greatly reduced, and the amount of the germanium-containing mother liquor is reduced; and the generated germanium-containing acid gas is subjected to fractional condensation recovery, so that the germanium loss caused by volatilization of the germanium tetrachloride in the process of producing the germanium dioxide by hydrolysis, washing and drying is reduced.

Description

technical field [0001] The invention relates to the technical field of semiconductor oxide preparation technology, in particular to a preparation method of germanium dioxide powder. Background technique [0002] Germanium dioxide, molecular formula GeO 2 , is the semiconductor germanium dioxide, white powder, hexagonal, tetragonal or amorphous solid. Germanium dioxide can be used as an intermediate product for the production of germanium ingots and fiber-grade germanium tetrachloride, and can also be used as a catalyst for the production of polyester fiber (PET). The application ratio of germanium dioxide catalyst accounts for about 16% of the total consumption of germanium. %. [0003] The existing production of germanium dioxide is mainly prepared by hydrolysis of germanium tetrachloride. The main process includes hydrolysis of germanium tetrachloride, suspension of germanium dioxide, solid-liquid separation, and germanium dioxide filter cake containing hydrochloric acid...

Claims

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Application Information

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IPC IPC(8): C01G17/02
CPCC01G17/02Y02P10/20
Inventor 谈发堂马伟涛
Owner 湖北联合贵稀资源再生科技有限公司
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