Method for preparing germanium chloride by microwave one-step method from tannin germanium slag

A germanium chloride and germanium slag technology is applied in the fields of metallurgy and energy, can solve the problems of high energy consumption, long time, low impurity content of germanium tetrachloride, etc., and achieves reduced process energy consumption, easy operation and good wave absorption performance Effect

Active Publication Date: 2021-08-20
KUNMING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] Aiming at the problems of long time consumption and high energy consumption in the prior art, the present invention provides a microwave-one-step method for preparing germanium chloride from tannin germanium slag. In the present invention, tannin germanium slag belongs to a macromolecular organic salt and has good wave-absorbing performance , the energy consumption of the process can be significantly reduced by introducing a microwave external field, the impurity content of germanium tetrachloride is also lower, and the recovery rate of germanium can reach more than 90%.

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  • Method for preparing germanium chloride by microwave one-step method from tannin germanium slag

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Effect test

Embodiment 1

[0018] Embodiment 1: a kind of method for preparing germanium chloride by microwave one-step method of tannin germanium slag (see figure 1 ),Specific steps are as follows:

[0019] (1) Mix tannin germanium slag and chlorine-containing compound (ammonium chloride) to obtain mixture A, add water to mixture A, mix evenly and let it stand for 5 minutes to obtain mixture B; the tannin germanium slag is obtained through the lead-zinc smelting process The residue is obtained by leaching germanium-containing zinc oxide fumes obtained by volatilization in a fuming furnace, and precipitating germanium with tannic acid. The content of Zn is 5%, the content of S is 5%, the content of Ge is 0.5%, and the content of other impurity elements is 5%; The mass ratio of germanium tannin slag and chlorine-containing compound (ammonium chloride) is 5:1, and the liquid-solid ratio mL:g of water to mixture A is 1:3;

[0020] (2) Step (1) The mixture B is subjected to microwave roasting, and the roas...

Embodiment 2

[0024] Embodiment 2: a kind of method that tannin germanium slag microwave one-step method prepares germanium chloride (see figure 1 ),Specific steps are as follows:

[0025] (1) Mix tannin germanium slag and chlorine-containing compound (commercially available hydrochloric acid) to obtain mixture A, add water to mixture A, mix evenly and let it stand for 20 minutes to obtain mixture B; the tannin germanium slag is obtained through the lead-zinc smelting process The residue is obtained by leaching germanium-containing zinc oxide dust obtained by volatilization in a fuming furnace, and precipitating germanium with tannic acid. The content of Zn is 15%, the content of S is 10%, the content of Ge is 2.0%, and the content of other impurity elements is 15%; The mass ratio of germanium tannin slag and chlorine-containing compound (commercially available hydrochloric acid) is 1:1, and the liquid-solid ratio mL:g of water to mixture A is 1:1;

[0026] (2) Step (1) The mixture B is su...

Embodiment 3

[0029] Embodiment 3: a kind of method that tannin germanium slag microwave one-step method prepares germanium chloride (see figure 1 ),Specific steps are as follows:

[0030] (1) Mix tannin germanium slag and chlorine-containing compound (calcium chloride) to obtain mixture A, add water to mixture A, mix evenly and let it stand for 30 minutes to obtain mixture B; the tannin germanium slag is obtained through the lead-zinc smelting process The residue is obtained by leaching germanium-containing zinc oxide fumes obtained by volatilization in a fuming furnace, and precipitating germanium with tannic acid. The content of Zn is 30%, the content of S is 20%, the content of Ge is 5%, and the content of other impurity elements is 30%; The mass ratio of germanium tannin slag and chlorine-containing compound (calcium chloride) is 1:5, and the liquid-solid ratio mL:g of water to mixture A is 3:1;

[0031] (2) Step (1) The mixture B is subjected to microwave roasting, and the roasting s...

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Abstract

The invention relates to a method for preparing germanium chloride by a microwave one-step method from tannin germanium slag, and belongs to the technical field of metallurgy and energy. In the present invention, the tannin germanium slag and the chlorine-containing compound are uniformly mixed to obtain a mixture A, water is added to the mixture A, mixed uniformly, and left to stand for 5 to 30 minutes to obtain a mixture B; the mixture B is subjected to microwave roasting, and the roasting steam is condensed to obtain germanium tetrachloride . The method of the invention can effectively shorten the time for preparing germanium tetrachloride from industrial tannin germanium slag, improve the complex process of washing-roasting-chlorination distillation, and the tannin germanium slag belongs to a macromolecular organic salt, has good wave-absorbing performance, and can significantly reduce the process. energy consumption, and the impurity content of the prepared germanium tetrachloride is also lower. The method of the invention has the advantages of simple process, high efficiency, easy operation, high sample purity and the like.

Description

technical field [0001] The invention relates to a method for preparing germanium chloride by a microwave one-step method from tannin germanium slag, and belongs to the technical field of metallurgy and energy. Background technique [0002] Smelting enterprises mainly use the tannin slag produced by the tannin sinking germanium method as raw materials, which are washed, filtered, dried, roasted in sequence, and then separated and purified by chlorination distillation to produce germanium tetrachloride, and finally the germanium tetrachloride is Hydrolysis, reduction and regional purification to get metal germanium. The traditional production method not only has the problem of complicated process, but also consumes a lot of energy and the production efficiency is not high. Contents of the invention [0003] Aiming at the problems of long time consumption and high energy consumption in the prior art, the present invention provides a microwave-one-step method for preparing ge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B41/00C22B1/02
CPCC22B1/02C22B41/00
Inventor 张利波狄浩凯杨坤彭金辉杨芳芳
Owner KUNMING UNIV OF SCI & TECH
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