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Microwave-assisted method for efficiently extracting germanium from low-grade germanium-containing material

A microwave-assisted, low-grade technology, applied in the fields of metallurgy and energy, can solve the problem of low germanium recovery rate, achieve the effects of increasing germanium content, low germanium loss rate, and shortening the process technology

Inactive Publication Date: 2020-04-07
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Low-grade germanium-containing materials are subjected to acid leaching to obtain germanium-precipitated liquid, then add tannic acid to precipitate germanium to obtain tannin slag, tannin slag is then burned to obtain germanium concentrate, and germanium concentrate is then chlorinated to obtain tetrachloride Germanium is the classic process for processing low-grade germanium-containing materials in factories at present, but the recovery rate of germanium is not high, only about 70%

Method used

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  • Microwave-assisted method for efficiently extracting germanium from low-grade germanium-containing material
  • Microwave-assisted method for efficiently extracting germanium from low-grade germanium-containing material
  • Microwave-assisted method for efficiently extracting germanium from low-grade germanium-containing material

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: A kind of microwave-assisted method for efficiently extracting germanium in low-grade germanium-containing materials (see figure 1 ),Specific steps are as follows:

[0022] (1) Mix the low-grade germanium-containing material with alkali (potassium hydroxide) to obtain mixture A, heat the mixture A to 200 ° C and keep it warm for 60 minutes, cool to room temperature, and crush to obtain mixture B; the low-grade germanium-containing The composition of the material is shown in Table 1. The mass ratio of low-grade germanium-containing material to alkali (potassium hydroxide) is 1:3; low-grade germanium-containing material and alkali (potassium hydroxide) form germanate, and the reaction formula is

[0023] GeO 2 +2KOH=K 2 GeO 3 +H 2 o

[0024] Table 1 Components of low-grade germanium-containing materials

[0025]

[0026] (2) Add water to the mixture B in step (1) for water immersion reaction for 5 minutes to remove the soluble impurities in the mixt...

Embodiment 2

[0032] Embodiment 2: A kind of microwave-assisted method for efficiently extracting germanium in low-grade germanium-containing materials (see figure 1 ),Specific steps are as follows:

[0033] (1) Mix the low-grade germanium-containing material with alkali (sodium hydroxide) to obtain a mixture A, heat the mixture A to 400 ° C and keep it warm for 30 minutes, cool to room temperature, and crush to obtain a mixture B; the low-grade germanium-containing The composition of the material is shown in Table 3. The mass ratio of low-grade germanium-containing material to alkali (sodium hydroxide) is 1:1; low-grade germanium-containing material and alkali (sodium hydroxide) form germanate, and the reaction formula is

[0034] GeO 2 +2NaOH=Na 2 GeO 3 +H 2 o

[0035] Table 3 Components of low-grade germanium-containing materials

[0036]

[0037] (2) Add water to mixture B in step (1) for water immersion reaction for 15 minutes to remove soluble impurities in mixture B, and sep...

Embodiment 3

[0043] Embodiment 3: A kind of microwave-assisted method for efficiently extracting germanium in low-grade germanium-containing materials (see figure 1 ),Specific steps are as follows:

[0044] (1) Mix low-grade germanium-containing materials with alkali (calcium hydroxide) to obtain mixture A, heat mixture A to 600°C with microwave ovens and keep it warm for 10 minutes, cool to room temperature, and crush to obtain mixture B; among them, low-grade germanium-containing materials The composition of the material is shown in Table 5. The mass ratio of low-grade germanium-containing material to alkali (calcium hydroxide) is 3:1; low-grade germanium-containing material and alkali (calcium hydroxide) form germanate, and the reaction formula is

[0045] GeO 2 +Ca(OH) 2 = Ca 2 GeO 3 +H 2 o

[0046] Table 5 Components of low-grade germanium-containing materials

[0047]

[0048] (2) Add water to the mixture B in step (1) for water immersion reaction for 30 minutes to remove t...

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Abstract

The invention relates to a microwave-assisted method for efficiently extracting germanium from a low-grade germanium-containing material, which belongs to the technical field of metallurgy and energy.The method comprises the following steps of: uniformly mixing a low-grade germanium-containing material with alkali to obtain a mixture A, carrying out microwave heating reaction on the mixture A for10-60 minutes, cooling to room temperature, and crushing to obtain a mixture B, adding water into the mixture B to carry out water leaching reaction for 5-30 minutes, and carrying out solid-liquid separation to obtain water leaching residues and water leaching liquid, adding hydrochloric acid into the water leaching residues, uniformly mixing, distilling, and condensing steam to obtain germaniumtetrachloride. According to the method, the low-grade germanium-containing material is subjected to alkali fusion and then subjected to water leaching and chlorination distillation of germanate to extract germanium, so that the process for preparing germanium tetrachloride from the low-grade germanium-containing material in the prior art can be greatly shortened, the germanium loss rate is low, and the purity of germanium tetrachloride is high.

Description

technical field [0001] The invention relates to a microwave-assisted method for efficiently extracting germanium in low-grade germanium-containing materials, which belongs to the technical field of metallurgy and energy. Background technique [0002] Germanium is a kind of scattered metal with very unique and excellent physical and chemical properties. It is an important material in the semiconductor industry and is widely used in high-tech fields such as defense industry, aerospace, electronics, optoelectronics, medicine, energy and modern information. There are three main sources of germanium: germanium processing waste, various products of coal combustion, and germanium enrichment in the non-ferrous metal smelting process. [0003] Low-grade germanium-containing materials are subjected to acid leaching to obtain germanium-precipitated liquid, then add tannic acid to precipitate germanium to obtain tannin slag, tannin slag is then burned to obtain germanium concentrate, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B41/00C22B7/00C22B9/02C01G17/04
CPCC22B41/00C22B7/008C22B9/02C01G17/04Y02P10/20
Inventor 张利波杨坤梁明彭金辉曾翰林
Owner KUNMING UNIV OF SCI & TECH
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