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Method for selectively extracting and recycling gallium, germanium and indium from sulfuric acid leach liquid of zinc displacement residues

The technology of slag sulfuric acid and leaching solution is applied in the field of selective extraction and recovery of gallium germanium indium, which can solve the problems of large damage degree of extractant, high water solubility and high alkali concentration, and achieves good back-extraction effect, good dispersion performance and high recovery rate. Effect

Active Publication Date: 2015-10-07
CENT SOUTH UNIV +1
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Problems solved by technology

A lot of research has been done on the recovery of gallium, germanium and indium by solvent extraction at home and abroad. For example, LIX63 has good selectivity for extracting germanium from high-concentration sulfuric acid solution, but the concentration of alkali required for reverse extraction with organic loads is high, which will damage the extractant. Large, resulting in short service life of the extractant; Kelex100 extracts gallium from alkaline sodium aluminate solution, and then applies it to sulfuric acid solution to extract germanium
Both of the above two extractants have the disadvantages of difficult synthesis, high price, and large loss during the extraction process.
The YW100 and G315 hydroxamic acid extractants synthesized in my country can also selectively extract germanium from the sulfuric acid medium containing germanium, but they have the disadvantages of high water solubility and the third phase of the extraction process.
However, there are few reports on the selective extraction of gallium indium from sulfuric acid solutions containing a large amount of impurities such as zinc, iron, nickel, cobalt, and cadmium.

Method used

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  • Method for selectively extracting and recycling gallium, germanium and indium from sulfuric acid leach liquid of zinc displacement residues
  • Method for selectively extracting and recycling gallium, germanium and indium from sulfuric acid leach liquid of zinc displacement residues
  • Method for selectively extracting and recycling gallium, germanium and indium from sulfuric acid leach liquid of zinc displacement residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Aqueous phase material solution: sulfuric acid leaching solution of zinc replacement slag, containing germanium 0.254g / L, gallium 0.311g / L, indium 0.06g / L, iron 1.07g / L, zinc 16.55g / L, nickel 0.58g / L, cobalt 0.87g / L, cadmium 4.6g / L, sulfuric acid concentration of feed liquid 100g / L;

[0040] Extract germanium organic phase: the extractant is 0.2mol / L HBL101+0.1mol / L P507, and the diluent is sulfonated kerosene.

[0041] 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.

[0042] Table 1 Extraction rate (%) of metal ions in sulfuric acid leaching solution of zinc replacement slag extracted by HBL101+P507 co-extraction system

[0043]

[0044]

[0045] It can be seen from Table 1 that the HBL101+P507 co-extraction system has excellent extraction selecti...

Embodiment 2

[0047] The aqueous phase material liquid is the extracting germanium raffinate solution in Example 1, containing about 100g / L of sulfuric acid, after diffusion dialysis, the concentration of sulfuric acid in the dialysate is only 5g / L, adding concentrated NaOH solution to adjust the pH value to 3.0 as the extraction of gallium , The raw material solution of indium, the concentration of metal ions remains basically unchanged;

[0048] Gallium indium extraction organic phase: extractant is 0.1mol / L HBL101+0.1mol / L Versatic 10, diluent is No. 260 solvent naphtha.

[0049] 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 2.

[0050] Table 2 HBL101+Ver.10 co-extraction system extraction extraction rate of metal ions in germanium raffinate (%)

[0051]

[0052] It c...

Embodiment 3

[0054] Water phase feed liquid is identical with embodiment 1;

[0055] The organic phase is an extractant of 0.2mol / L HBL101+0.2mol / L P507, and the diluent is aviation kerosene.

[0056] Stripping agent: 0.5mol / L NaOH solution.

[0057] Extraction and separation: the above-mentioned organic phase and the aqueous phase feed liquid are subjected to 3-stage countercurrent extraction under the condition of 1 / 5 of the ratio, and single-stage stripping is performed under the condition of 1 / 1 of the ratio of the stripping agent used for the loaded organic phase. The mixing time for both extraction and back extraction was 10 min, and the temperature was 25 °C. Table 3 shows the experimental results after extraction-stripping reached equilibrium.

[0058] Table 3 HBL101+P507 multistage countercurrent cascade extraction simulation test results

[0059]

[0060] Note: -- not detected

[0061] It can be seen from Table 3 that after three stages of countercurrent extraction, the ge...

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Abstract

The invention discloses a method for selectively extracting and recycling gallium, germanium and indium from sulfuric acid leach liquid of zinc displacement residues. The method includes selectively extracting the germanium from the sulfuric acid leach liquid of the zinc displacement residues by the aid of synergistic extraction systems comprising hydroxamic chelate extraction agents and acidic phosphorus type extraction agents; recycling acid from germanium extraction raffinate by the aid of a diffusion dialysis process and finely adjusting the germanium extraction raffinate until a pH (potential of hydrogen) value of the germanium extraction raffinate is appropriate; selectively extracting the gallium and the indium from the germanium extraction raffinate by the aid of synergistic extraction systems comprising hydroxamic chelate extraction agents and carboxylic acid extraction agents. The method has the advantages that the germanium, the gallium and the indium can be effectively separated from foreign metal ions of iron, zinc, cadmium, nickel, cobalt and the like; the germanium, the gallium and the indium are high in recycling rate, good germanium, gallium, indium and foreign matter separation effects can be realized, technological processes are short, the extraction agents are long in service life and low in loss, and the method is low in cost and easy to industrialize.

Description

technical field [0001] The invention relates to a method for selectively extracting and recovering gallium, germanium and indium from sulfuric acid leaching solution of zinc replacement slag, and belongs to the technical field of hydrometallurgy. Background technique [0002] Germanium and gallium indium 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 germanium and gallium-indium. The wet process of extracting gallium germanium indium from zinc replacement slag is generally leaching with sulfuric acid first, and then extracting and recovering gallium germanium indium from the leaching solution by solvent extraction. A lot of research has been done on the recovery of gallium, germanium and indium by solvent extraction at home and abroad. For example, LIX63 has goo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B41/00C22B58/00C22B3/30
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 CENT SOUTH UNIV
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