Method for selective extraction of gallium and germanium from oxalic acid solution containing gallium and germanium

A technology of oxalic acid solution and acid solution is applied in the field of extraction of gallium and germanium, which can solve the problems of low cost, inability to separate, and short process, and achieve the effects of low cost, low consumption of chemical reagents, and short process.

Active Publication Date: 2014-08-27
SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the prior art, the leaching solution obtained by leaching zinc replacement slag with oxalic acid solution has the defect that gallium germanium cannot be further extracted from the oxalic acid leaching solution and separated from impurities such as copper and zinc. The purpose of the present invention is to provide a A method for selectively and efficiently extracting gallium and germanium from the oxalic acid solution of gallium and germanium to realize the separation of gallium, germanium and various impurities such as copper and zinc. This method has a short process, low cost, and is easy to realize industrial production

Method used

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  • Method for selective extraction of gallium and germanium from oxalic acid solution containing gallium and germanium
  • Method for selective extraction of gallium and germanium from oxalic acid solution containing gallium and germanium
  • Method for selective extraction of gallium and germanium from oxalic acid solution containing gallium and germanium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Aqueous phase feed solution: oxalic acid leaching solution of zinc replacement slag, which contains 0.274g / L gallium, 0.511g / L germanium, 0.065g / L copper, and 0.55g / L zinc, and the pH value of the feed solution is 0.51;

[0019] Organic phase: the extractant is tertiary amine N235, its volume fraction is 20%, and the diluent in the organic phase is sulfonated kerosene, its volume fraction is 80%.

[0020] Extraction and separation: The organic phase and the feed liquid are subjected to single-stage extraction under the condition of a ratio of 1 / 1, the extraction equilibrium time is 10 minutes, and the temperature is 25°C. The experimental results are shown in Table 1.

[0021] Table 1 Tertiary amine N235 is to the extraction rate (%) of metal ion in the oxalic acid leach solution

[0022] Metal ion

[0023] It can be seen from Table 1 that the tertiary amine extractant has excellent extraction selectivity for gallium and germanium in the oxalic acid leach so...

Embodiment 2

[0025] Water phase material liquid is with embodiment 1;

[0026] Prepare two organic phases with different compositions numbered 1 and 2 respectively, the diluent in the organic phase is sulfonated kerosene, the No. 1 organic phase is the sulfonated kerosene solution of 20% N235+10% sec-octanol, and the No. 2 organic phase is 20% N235+10% TBP sulfonated kerosene solution.

[0027] Extraction and separation: the above two organic phases are subjected to single-stage extraction at a ratio of 1:1 to the feed liquid, the extraction equilibrium time is 10 minutes, and the temperature is 25°C. The experimental results are shown in Table 2.

[0028] Table 2 The influence of different phase regulators on the extraction rate of each metal ion in the oxalic acid leachate (%)

[0029] Metal ion

[0030] It can be seen from Table 2 that the extraction rate of gallium and germanium in the 20% N235 + 10% 2-octanol + sulfonated kerosene system is above 99%, and the extraction r...

Embodiment 3

[0032] The aqueous phase feed solution is oxalic acid leaching solution of zinc replacement slag, which contains 0.386g / L gallium, 0.477g / L germanium, 0.12g / L copper, and 0.6g / L zinc, and the pH value of the feed solution is 1.5;

[0033] The organic phase is No. 260 solvent oil solution of 5% N235+10% sec-octanol.

[0034] The organic phase and the aqueous phase feed liquid are subjected to single-stage extraction, the extraction ratio (O / A)=5 / 1, the extraction time is 10 min, and the temperature is 25°C. The experimental results are shown in Table 3.

[0035] Table 35% N235+10% secondary octanol extraction metal ion results in oxalic acid leachate (%)

[0036] Metal ion

[0037] The results show that during the extraction process, the extraction rates of gallium and germanium can reach more than 97%, and copper and zinc are basically not extracted. Reaching above 2500 and 3500 respectively, the separation effect is good.

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Abstract

The invention discloses a method for selective extraction of gallium and germanium from an oxalic acid solution containing gallium and germanium. The method comprises the following steps of carrying out single-stage or multistage countercurrent extraction on the oxalic acid solution containing gallium and germanium by an organic phase, carrying out single-stage or multistage countercurrent selective gallium-back-extraction on the carrying organic phase obtained by the above single-stage or multistage countercurrent extraction to extract gallium, and carrying out germanium back-extraction on the organic phase obtained by the gallium-back-extraction by an alkali solution to respectively obtain a gallium-containing aqueous solution and a germanium-containing aqueous solution. The method effectively realizes separation of gallium and germanium from impurities such as copper and zinc, has a short flow process, small chemical reagent consumption and a low cost and can easily realize industrialization.

Description

technical field [0001] The invention relates to a method for extracting gallium and germanium from an oxalic acid solution containing gallium and germanium, belonging to the technical field of extraction and separation. Background technique [0002] Gallium and germanium are important strategic scattered metals, which are widely used in information electronics and other fields. The gallium-germanium slag obtained by replacing zinc powder in the smelting process of the zinc plant is an important raw material for the extraction of gallium and germanium. The wet process of extracting gallium germanium from gallium germanium slag is generally leaching with sulfuric acid first, and then extracting gallium germanium from the leaching solution by solvent extraction. A lot of research has been done on the recovery of gallium and germanium by solvent extraction at home and abroad. For example, LIX63 has good selectivity for extracting germanium from high-concentration sulfuric acid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/26C22B41/00C22B58/00
CPCY02P10/20
Inventor 曾理徐毅刘野平张登凯周科华张伟胡东风李玉虎
Owner SHENZHEN ZHONGJIN LINGNAN NONFEMET COMPANY
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