Method for producing germanium concentrated ore from germanium-containing industrial liquor

A germanium concentrate and industrial technology, applied in the field of non-ferrous metallurgy, can solve the problems of difficult filtration, large use restrictions, large alkali consumption and large extraction agent, and achieve good stripping effect, low cost, high germanium precipitation rate and recovery rate Effect

Active Publication Date: 2009-09-23
YUNNAN WUXIN IND
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Problems solved by technology

This technology can only be used for the separation of germanium and zinc, and its use is limited; the stripping rate is 97%, the germanium precipitation rate is 95%, and it is difficult to filter, so the alkali consumption and extraction agent are large, and the material cost is not as good as that of the tannin extraction method, so it is not suitable for industrial production.

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  • Method for producing germanium concentrated ore from germanium-containing industrial liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1: The germanium-containing industrial feed solution is a sulfuric acid solution containing Ge 100-200 mg / L, In 10000±500 mg / L, and pH 0.5-1.5. Add citric acid at a weight ratio of citric acid: germanium = 4 to 5: 1, and dissolve at room temperature. Then use 30% volume percent N 263 (tetraalkylamine) kerosene solution extractant, carry out five-stage countercurrent extraction in the mixed sedimentation box-type extraction tank, use the NaOH aqueous solution of 20% to do three-stage countercurrent back extraction with the weight percent concentration, the sulfuric acid of weight percent concentration 10% Aqueous primary organic phase regeneration. The extraction rate of germanium is 98.5%, and the stripping rate is 99%. The NaOH back-extraction solution contains 19.78g / L of germanium, adjusts the pH to 8-10 with sulfuric acid for the first hydrolysis, heats and filters, and obtains a germanium concentrate containing 32.7% of germanium (weight ratio). After...

Embodiment 2

[0013] Embodiment 2: The germanium-containing industrial feed solution is a sulfuric acid solution containing Ge30-200mg / L, Zn2-3g / L, Fe61-200mg / L, pH2±0.5. Add tartaric acid by tartaric acid: germanium=8~10: 1 (weight ratio), then be 30% N with weight percentage concentration 235 (Trialkylamine) kerosene solution is used as the extraction agent, three countercurrent extractions are carried out in a box-type extraction tank, two-stage countercurrent back extraction is performed with a 30% NaOH aqueous solution, and the organic phase is regenerated with a 10% sulfuric acid aqueous solution. The extraction rate of germanium is 96.88%, and the stripping rate is 98.18%. Adjust the pH of the stripping solution to 9-11 with sulfuric acid, and add ZnSO at the same time 4 .7H 2 O is hydrolyzed according to Zn / Ge=4.5:1 (weight ratio), and the germanium concentrate contains 10.66% (weight ratio) of germanium. The equipment has been in operation for 1.5 months, processing 300 cubic me...

Embodiment 3

[0014] Example 3: Industrial feed liquid contains Ge 0.075g / L, Zn 80g / L, Fe1.3g / L, As0.9g / L, Cd 0.3g / L, In 0.011g / L, Cl - 0.56g / L,H 2 SO 4 5g / L, temperature 25°C. Potassium hydrogen tartrate is added according to potassium hydrogen tartrate: germanium=6.4:1 (weight ratio), or industrial citric acid is added according to citric acid: germanium=3:1 (weight ratio). Then use 30% volume percent N 263 (Tetraalkylamine) kerosene solution is the extractant, carries out five-stage extraction respectively in 2 escalating extractors, uses the NaOH aqueous solution of 25% to do two-stage back-extraction with weight percentage concentration, and 15% sulfuric acid aqueous solution primary organic phase regeneration. When potassium hydrogen tartrate is added, the extraction rate: Ge99.3%, In2.14%, Zn0.2%, Fe3.4%, As6.9%, Cd0.6%; the back extraction rate of Ge is 99.15%. When citric acid is added, the Ge extraction rate is 99%, and the stripping rate is 99%, and the Cl in the raffinate is...

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Abstract

The invention relates to a method for producing germanium concentrated ore from germanium-containing industrial liquor, and belongs to the technical field of nonferrous metallurgy. The method comprises that: a, a germanium complexing agent is added into the germanium-containing industrial liquor of which pH is 0.5 to 3, wherein the complexing agent is organic acid containing hydroxyl or carboxyl or/and salt of the organic acid, and the weight ratio of the complexing agent to the germanium is 3-10:1; b, an organic reagent of quaternary ammonium with an R4N structure or tertiary amine with an R3N structure is used as an extracting agent to extract the germanium in the liquor obtained in step a, wherein R is hydrocarbyl or alkyl or fatty group, N is organic ammonium salt, and the extracting agent accounts for 10 to 50 percent of the extracted liquor by volume; c, NaOH water solution or Na2CO3 water solution of which the concentration in percentage by weight is 5 to 30 percent is used for reversely extracting the germanium-containing organic phase obtained in step b; and d, the pH of the obtained reverse extracted liquor is adjusted to 8 to 12 by acid, then the liquor is dehydrated twice and filtered, and the sediment is dried to form the germanium concentrated ore. The method can produce the germanium concentrated ore from various germanium industrial liquors, the extracting agent and the complexing agent are easily obtained, the extracting and reverse extracting effects are good, and the yield of the germanium is high.

Description

technical field [0001] The invention belongs to the technical field of nonferrous metallurgy. Background technique [0002] The traditional process of extracting germanium from germanium-containing industrial feed liquid to produce germanium concentrate is the tannin method: at about pH=2, use tannic acid or tannin-containing tannic acid for complexation, and combine with Zn 2+ , Fe 2+ , Fe 3+ and so on to generate double salt precipitation, then press filter and calcinate to make germanium concentrate containing 10-25% germanium. Although the tannin method is simple to operate, tannin has a wide range of uses and a special source, so it is rare and expensive. For every kilogram of germanium extracted, 30 kilograms of tannin and 45-50 kilograms of tannin are needed, accounting for 1 / 3-1 / 2 of the production cost. In addition, the precipitated liquid has adverse effects on the extraction of other metals, increasing the extraction cost. Therefore, people have been looking ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B41/00
CPCY02P10/20
Inventor 李世平余树华张本聪
Owner YUNNAN WUXIN IND
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