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Method for recovering germanium from germanium-containing material

A material and waste technology, applied in the field of recycling germanium in germanium-containing waste, can solve the problems of insufficient utilization of germanium resources, low germanium recovery rate, difficulty in filtration, etc., so as to avoid sewage treatment problems, reduce production costs, and avoid low recovery rates Effect

Inactive Publication Date: 2017-01-18
王朋
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional methods include (1) grinding the germanium-containing material and adding an oxidizing agent to direct chlorination and distillation. This process can hardly extract germanium from the raw material
(2) The germanium-containing material is oxidized and roasted and then chlorinated and distilled. The recovery rate of germanium is low due to the packaging problem of silicon dioxide. Secondly, silicon dioxide forms silica gel in acidic medium, which makes filtration difficult.
(3) After grinding germanium-containing materials, carry out high-temperature alkali dissolution to obtain sodium silicate and sodium germanate solutions, add electrolyte and adjust the pH value to carry out the process of precipitating silicon and precipitating germanium. Although this process can effectively separate germanium, but The silicon sinking time is long, and a large amount of germanium is precipitated together with the silicon during the silicon sinking process, so that the recovery rate of germanium is lower than 75%, and germanium resources are not fully utilized.
(4) Dissolve the germanium-containing material with hydrofluoric acid after grinding, and tannin sinks germanium. This process has high production costs, serious corrosion of equipment, and pollution to the environment due to the existence of fluoride ions
At present, all smelters use the fire method to treat acid slag, but when the fire method is used to treat acid slag, the volatilization temperature of germanium is higher than 1100°C, which produces a large amount of toxic fumes, which puts a lot of pressure on the company's environmental protection and severely corrodes the equipment. high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take by weighing 200Kg germanium and be used for the germanium-containing material that produces when producing optical fiber and infrared optical glass, germanium content is 0.6%, obtain 300 mesh germanium-containing silica powders after crushing and pulverizing, adding silica powder mass concentration is 30 % sodium hydroxide solution, the quality of the sodium hydroxide solution is 1000Kg; the reaction solution is pumped into the autoclave with a pump, heated to 150° C., and incubated for 3 hours to obtain a sodium silicate alkaline solution containing sodium germanate; Add the solution to a volume of 1m 3 Quality is housed in the tank of the D301 weakly basic epoxy series anion exchange resin of 2.4kg, the sodium silicate solution obtained is evaporated and concentrated, the water of mother liquor quality 15% is evaporated, and the output water glass product; Pass 100L of 0.5mol / L dilute sulfuric acid through the above tank with resin to obtain a solution containing...

Embodiment 2

[0023] Weigh 300Kg germanium for the germanium-containing material produced when producing optical fiber and infrared optical glass. The germanium content is 0.8%. After crushing and grinding, 200 mesh germanium-containing silica powder is obtained, and the silica powder is added at a concentration of 30%. In the sodium hydroxide solution, the quality of the sodium hydroxide solution is 1200Kg; the reaction solution is pumped into the autoclave with a pump, heated to 180°C, and incubated for 2 hours to obtain a sodium silicate alkaline solution containing sodium germanate; The solution passes through a volume of 1m 3 Quality is housed in the tank of the D201 weakly basic epoxy anion exchange resin of 3.6kg, the sodium silicate solution that obtains is carried out evaporation concentration, evaporates the water of 25% of mother liquor quality, produces water glass product; Concentration Pass 100L of 0.5mol / L dilute sulfuric acid through the above-mentioned tank containing the r...

Embodiment 3

[0025] Weigh 500Kg germanium for the germanium-containing material produced when producing optical fiber and infrared optical glass. The germanium content is 0.4%. After crushing and grinding, 200 mesh germanium-containing silica powder is obtained, and the silica powder is added at a concentration of 30%. In the sodium hydroxide solution, the quality of the sodium hydroxide solution is 1400Kg; the reaction solution is pumped into the autoclave with a pump, heated to 120 ℃, and incubated for 2 hours to obtain a sodium silicate alkaline solution containing sodium germanate; The solution passes through a volume of 1m 3 Quality is housed in the tank of the 201 * 7MB weakly basic styrene-based anion exchange resin of 3kg, the sodium silicate solution obtained is evaporated and concentrated, evaporates the water of 30% of the mother liquor quality, and produces the water glass product; 100L of dilute sulfuric acid with a concentration of 0.5mol / L passes through the above-mentioned ...

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Abstract

The invention discloses a method for recovering germanium from a germanium-containing material. According to the method, a resin adsorption principle is adopted in the germanium separation process so as to thoroughly adsorb germanium into resin and let silicon enter a solvent in the form of sodium silicate. Therefore, germanium is separated thoroughly, recovery rate of germanium reaches about 95%, and the problem that lots of germanium is brought into silica precipitate in the silicon precipitation process of electrolyte produced by the electrolyte separation method of germanium is avoided. After resin adsorption, part of water is evaporated from a sodium silicate solution and then the product can be used as a soluble glass product for sale. Thus, sewage treatment problem is avoided, and production cost is reduced. Defects of a hydrofluoric acid method for processing a germanium-containing material, such as high production cost, severe equipment corrosion and environmental pollution, are eliminated; and the problem of low recovery rate in an alkali dissolution precipitation method is avoided. By the method of the invention, equipment corrosion, environmental pollution and other problems are not caused in the germanium-containing waste material dissolving process.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for recovering germanium in germanium-containing waste materials. Background technique [0002] Germanium is a kind of scattered metal with few reserves in nature, mainly associated with lignite, lead-zinc ore and copper mine in South Africa. The proven reserves of germanium in the world are 8,600 tons, which is only enough for more than 40 years based on the current consumption of germanium; germanium is an important strategic resource, which is used in high-tech fields such as aerospace, optical fiber communication, infrared optics, and new energy All have irreplaceable applications. With the development of high-tech in my country and the continuous upgrading of industrial structure, the consumption level of germanium will maintain a rapid growth. [0003] At present, the raw materials for germanium production include two aspects. One is to extract germanium fr...

Claims

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Application Information

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IPC IPC(8): C22B41/00C22B7/00C01B33/32
CPCC01B33/32C01G17/02C01P2006/80C22B7/006C22B41/00Y02P10/20
Inventor 王朋
Owner 王朋
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