Method for recovering germanium from flyash by wet process

A technology of fly ash and wet method, applied in the field of wet recovery of germanium and secondary recovery of germanium by wet method, can solve the problems of low recovery rate, high recovery cost, occupation of large land, etc., to reduce pollution, low cost, The effect of high recovery rate

Inactive Publication Date: 2010-12-08
JIUJIANG BAIDUN VANADIUM TECH TRADING
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the content of silicon in these tailings is relatively high, and magnesium also occupies a large proportion, but the increase of magnesium due to the addition of lime is not large, and the proportion of magnesium oxide only increases from less than 1% to less than 4%. , and the content of calcium varies greatly depending on whether lime is added when extracting germanium, GW in the table 1 , GW 3 The group is the fly ash after using the method of extracting germanium without adding lime, and GW 2 , GW 4 The first group is the use of fly ash after the method of adding lime to

Method used

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  • Method for recovering germanium from flyash by wet process
  • Method for recovering germanium from flyash by wet process
  • Method for recovering germanium from flyash by wet process

Examples

Experimental program
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Embodiment 1

[0030]Embodiment 1: Take 1000g of wet fly ash which is pulverized to 200 mesh by ball milling and place it in a 3000mL beaker. The moisture mass percentage in the wet fly ash is 25.1%. The mass percentage of silicon is 70.23%, the mass percentage of calcium oxide is 0.57%, and the mass percentage of magnesium oxide is 0.52%. Add 0.5mol / L sulfuric acid of 1000g, add 4g sodium chlorate, 25g ammonium fluoride, After stirring and mixing, raise the temperature to 80°C and keep the temperature at 80-85°C, start the mechanical stirring at a speed of 110-120 revolutions per minute, perform the first stirring and leaching for 3 hours, and then filter to obtain a leaching solution 980mL, the germanium content is 126mg / L, adopt the same conditions as the first leaching, and then carry out the second oxidation leaching, after liquid-solid separation, wash the acid solution in the fly ash with 400g hot water, and use pH test paper Check the washing water so that the pH of the washing water...

Embodiment 2

[0031] Example 2: Take 1000 g of wet fly ash crushed by ball milling to 200 mesh and place it in a 3000 mL beaker. The moisture mass percentage in the wet fly ash is 29.3%, the germanium content is 380 g / t, and the silica mass percentage is 69.31%, the mass percentage of calcium oxide is 4.07%, and the mass percentage of magnesium oxide is 0.61%. Add 1500 g of 0.5 mol / L sulfuric acid, add 5 g of sodium chlorate, and 30 g of ammonium fluoride. After stirring and mixing, Raise the temperature to 80°C and keep the temperature at 80-85°C, start mechanical stirring at a speed of 110-120 revolutions per minute, stir and leach for 4 hours, and then filter to obtain 1550mL of leaching solution with a germanium content of 81mg / L. Under the same conditions as the first leaching, carry out the second oxidative leaching of the fly ash after the first leaching. After liquid-solid separation, wash the acid in the fly ash with 400g of hot water, and then use a ball mill to crush it to 200-400...

Embodiment 3

[0032] Example 3: Take 1000g of wet fly ash crushed to 200 mesh by ball milling in a 3000mL beaker, the moisture mass percentage in the wet fly ash is 20.70%, the germanium content is 212g / t, and the silica mass percentage is 66.57 %, the mass percentage of calcium oxide is 38.82%, the mass percentage of magnesium oxide is 0.64%, add the sulfuric acid of 2000g0.5mol / L, add 2.5g sodium chlorate, 20g ammonium fluoride, after stirring and mixing, heat up to 80°C, and keep the temperature at 80-85°C, start mechanical stirring at a speed of 110-120 revolutions per minute, stir and leach for 5 hours, and then filter to obtain 1980mL of primary leachate with a germanium content of 68mg / L, using the conditions of primary leaching Carry out the second oxidative leaching of the fly ash after the first leaching, and after the liquid-solid separation, wash the acid solution in the fly ash with 400g hot water, then crush it to 200-400 mesh with a ball mill, and put it into the In the origi...

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Abstract

The invention relates to a method for recovering germanium from flyash by a wet process, belonging to the technical field of wet-process metallurgy. The method comprises the following steps of: (1) crushing flyash to more than 200 meshes by a wet process; (2) carrying out oxidizing leaching twice on wet flyash by using a sulfuric acid solution, sodium chlorate and ammonium fluoride; (3) crushing the flyash to 200-400 meshes for a second time; (4) leaching 3 or 4 times by using the same condition as that of the first leaching; (5) regulating the pH value of the first leached liquid to 2-2.5 by using ammonia water, and then precipitating and leaching out germanium in the liquid by using tannin with a weight percentage content of 80-99 percent; (6) drying and roasting the germanium precipitate to prepare a germanium concentrate; distilling the germanium concentrate with hydrochloric acid by using a conventional method to obtain germanium tetrachloride; and redistilling, rectifying, purifying and hydrolyzing to obtain high-purity germanium dioxide. The invention is used for flyash after recovering germanium by a fire process, sufficiently utilizes rare germanium metal, reduces the pollution of tailings to the environment, and has the advantages of low cost and high recovery rate.

Description

technical field [0001] The invention relates to a method for recovering germanium by wet method, in particular to a method for secondary recovery of germanium by wet method from fly ash after extracting germanium by fire method, and belongs to the technical field of hydrometallurgy. Background technique [0002] Germanium metal is a relatively scarce strategic resource, which is widely used in optical fiber communication, infrared optics, chemical catalysts, photovoltaic industry, aerospace, military industry, medical and health products and other fields. Most germanium elements are associated in lignite mines, and the fire method is generally used to extract germanium from lignite. When germanium is extracted by lignite fire method, the recovery rate of germanium is generally 70-85%, and the recovery rate is related to the recovery method adopted. Some lignite mining areas in my country have used different fire methods to extract germanium for many years, and the fly ash a...

Claims

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Application Information

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IPC IPC(8): C22B7/04C22B3/08C22B3/46C22B41/00
CPCY02P10/20
Inventor 葛启明李巴克谢迅杨兴林周权
Owner JIUJIANG BAIDUN VANADIUM TECH TRADING
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