Preparation method of germanium dioxide powder

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...

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

Images