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A method for extracting germanium from germanium-containing acidic solution with tio2 nh2o

An acid solution, H2SO4 technology, applied in the field of germanium extraction, can solve the problems of low production speed and scale, high price of exchange resin, large amount of tannin, etc., and achieves the effects of low price, low cost and low use cost.

Active Publication Date: 2016-01-20
六盘水中联工贸实业有限公司
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Problems solved by technology

This method sinks germanium fast and has high efficiency, but due to the high price of tannin, large usage and high production cost
Due to the large amount of tannin used, the amount of tannin remaining in the solution after germanium precipitation is also large, which will affect the electrolysis of zinc and reduce the current efficiency
Simultaneously, the mechanism of tannin sinking germanium is compound salt precipitation, zinc, iron, copper will participate in the formation of tannin zinc, tannin iron, tannin copper compound salt precipitation, causing the loss of zinc, people in order to overcome tannin sinking germanium Due to the disadvantages of high cost and high loss of zinc, the organic solvent extraction method has been studied. Hydroxamic extractants such as Lix63 and Kelex100 have been studied abroad, and N235 amine extractants and 7815 and P204-YW100 hydroxamic acid extractants have been studied domestically. The above-mentioned extractants can extract and separate germanium from acidic solution, and have been industrially produced. The production cost is low, and the comprehensive recovery rate of other valuable metals is also higher than that of the tannin method, but its production speed and scale are not as good as the tannin precipitation method.
At present, some people have studied the organic ion exchange method, but it is still in the exploratory stage, and the exchange resin is expensive and the efficiency is not high, and it cannot be compared with the tannin precipitation and the organic solvent benzene method.
TiO has not been used 2 ·nH 2 O patent report on extracting germanium from germanium-containing zinc sulfate solution

Method used

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  • A method for extracting germanium from germanium-containing acidic solution with tio2 nh2o

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Embodiment 1: TiO 2 ·nH 2 O is put into a glass tube, the effective column height is 130mm, and then the zinc sulfate solution of PH=1.5, Ge50mg / l, Zn100g / l, Fe0.6g / l passes through the above-mentioned exchange column, exchanged for natural infiltration, and the infiltration speed is 2-2.5m / min, the temperature is normal temperature, after adsorption, wash with water once, then use 20% NaOH aqueous solution for alkali washing, then rinse with 80 ℃ hot water, and then carry out the adsorption of germanium. A total of 7 cycles are carried out to treat zinc sulfate containing germanium Solution 1570ml, the average adsorption extraction rate of Germanium is 85.7%, Zn6.4%, Fe0.67%;

[0034] The germanium-containing washing solution obtained by the above process is washed with H 2 SO 4 Neutralize to pH 8-10 to hydrolyze germanium, and get germanium concentrate after drying.

Embodiment 2

[0035] Embodiment 2: TiO 2 ·nH 2 O is placed in a ceramic microporous funnel of medium 100, the thickness of the material layer is 10mm, installed on a vacuum filter bottle and poured into the leaching solution containing germanium and zinc sulfate, the solution PH=3, containing Ge65mg / l, containing Zn106g / l, and vacuum pumping Filtration, suction filtration speed 80ml / min, normal temperature operation, and 4 cycles, after adsorption, the liquid pH=3.4, Ge7-8.2mg / l, Zn105g / l, adsorption rate Ge86.3%, Zn0.009%;

[0036] The germanium-containing washing solution obtained by the above process is washed with H 2 SO 4 Neutralize to pH 8-10 to hydrolyze germanium, and get germanium concentrate after drying.

Embodiment 3

[0037] Embodiment 3: with TiO 2 ·nH 2 O According to the liquid-solid ratio l:s=5, add TiO to the immersion solution containing germanic acid 2 ·nH 2 O, stirring and adsorbing germanium at 40-60°C, the composition of the germanium-containing acidic leach solution is Ge400-550g / l, In26.5-2090mg / l, Zn21.8-25.9g / l, PH=0.5-2.5, stirring and adsorption time 60 minutes. At PH=2.5, the adsorption rate is: Ge73.2%, In31.42%, Zn1.6%;

[0038] The germanium-containing washing solution obtained by the above process is washed with H 2 SO 4 Neutralize to pH 8-10 to hydrolyze germanium, and get germanium concentrate after drying.

[0039] The germanium-containing TiO used in embodiment 3 by stirring adsorption pressure filtration 2 ·nH 2 O, according to the process of "first water washing→second alkali washing→second alkali washing→first water washing→drying", the alkali elution germanium experiment was carried out. The liquid-solid ratio of water washing and alkali washing is l:s=...

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Abstract

The invention provides a method for extracting germanium from a germanium-containing acidic solution by using TiO2.nH2O. The method is characterized in that TiO2.nH2O is used as an exchange medium, and germanium is adsorbed by adopting one of the following three technologies: (1) ion exchange column natural penetration process, (2) ion exchange column vacuum filtration method, and (3) stirring filter press filter-pressing method; germanium in the germanium-containing TiO2.nH2O obtained by adsorption according to one of the three technologies is eluted by using a NaOH aqueous solution or a NaOH and NH4OH mixed solution, and germanium-containing eluate is hydrolyzed and dried so as to obtain germanium concentrate; TiO2.nH2O without germanium is washed with clear water and then returns for use. The method has the advantages that TiO2.nH2O is simple to prepare and easy to obtain and selectively adsorbs germanium in the germanium-containing acidic solution, germanium-containing TiO2.nH2O is subjected to alkaline cleaning, TiO2.nH2O without germanium is washed with water to be regenerated and then returns for use, the technological process is short, and the operation is convenient and fast; the loss of TiO2.nH2O in adsorption, desorption and regeneration processes is small, and the using cost is low; the germanium concentrate obtained by using H2SO4 for neutralizing and hydrolyzing germanium-containing alkali wash water has good acid solubility; compared with a tannin precipitation method and an organic solvent benzene extraction method, the method is low in production cost.

Description

technical field [0001] A TiO 2 ·nH 2 O method for extracting germanium from germanium-containing acidic solution. technical field [0002] The present invention relates to hydrometallurgy technology, specifically a kind of using TiO 2 ·nH 2 O method for extracting germanium from germanium-containing zinc sulfate solution. Background technique [0003] The germanium-containing lead-zinc material or other materials can be obtained through acid leaching to obtain a germanium-containing zinc sulfate solution or an acidic solution containing germanium, from which the traditional method of producing germanium concentrate is the tannin precipitation method. This method sinks germanium quickly and has high efficiency, but due to the high price of tannin, large usage and high production cost. Due to the large amount of tannin used, the amount of tannin remaining in the solution after germanium precipitation is also large, which will affect the electrolysis of zinc and reduce t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/24C22B3/42C22B41/00
CPCY02P10/20
Inventor 李世平钟波张彬
Owner 六盘水中联工贸实业有限公司
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