Method for extracting germanium, indium and zinc from high iron, silicon and manganese materials containing germanium, indium and zinc

A technology of high iron and indium zinc, applied in the direction of improving process efficiency, etc., can solve the problems of frequent alkaline washing of organic phases, difficult extraction and production, and complex components.

Inactive Publication Date: 2012-08-01
YUNNAN WUXIN IND
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  • Abstract
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Problems solved by technology

With conventional sulfuric acid leaching, indium and zinc are easily leached, but when P204 is used to extract indium, P204 is seriously poisoned and aged, and the organic phase is frequently washed with alkali, so the extraction production is very difficult
Use zinc powder, iron filings, sodium sulfite, etc. to reduce ferric iron. Due to the complex composition, the content of indium is low, and the content of ferric iron is as high as 20g / l. The production cost of indium is high, and the leaching rate of germanium is low, about 20- 30%. Adding sodium chloride or hydrochloric acid for mixed leaching, the leaching rate of germanium does not increase significantly, without using a large amount of reducing agent, tannin or / and extracting germanium, or extracting germanium is also very difficult. Indium and zinc are easy to volatilize and collect dust, and the volatilization rate of germanium is below 10%, and the energy consumption is high and the pollution is large

Method used

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  • Method for extracting germanium, indium and zinc from high iron, silicon and manganese materials containing germanium, indium and zinc
  • Method for extracting germanium, indium and zinc from high iron, silicon and manganese materials containing germanium, indium and zinc
  • Method for extracting germanium, indium and zinc from high iron, silicon and manganese materials containing germanium, indium and zinc

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1. The raw material containing 0.0294% of germanium, 0.069% of indium, 8.9% of ferric iron, 12.7% of zinc, 24.5% of calcium, and 4.8% of silicon dioxide is first carried out neutral leaching with sulfuric acid, and the pH5.2 infiltration solution contains Germanium 0.28mg / l, indium 0 zinc 34.6g / l, medium leaching residue was acid leached twice with sulfuric acid according to the conventional method (sulfuric acid 100g / l, temperature 95-100 ℃) two leaching total leaching rate germanium 21.5%, indium 98.2%, leaching 0.0245% germanium, micro-indium, and 0.57% iron from tailings. The tailings were acid leached with sulfuric acid and 20g / l sodium chloride, 20% hydrochloric acid, sulfuric acid and 20g / l ammonium fluoride , PH≤0.5, temperature above 80°C, time 2-3 hours, liquid / solid=3. The leaching results of the sulfuric acid and sodium chloride group contained germanium 18.1mg / l, the slag contained germanium 0.0235%, and the leaching solution of the 20% hydrochlor...

Embodiment 2

[0013] Embodiment 2. Raw material composition contains germanium 0.0245%, indium 0.08%, ferric iron 8, % zinc 11.2%, silicon dioxide 5.2%, manganese 1.5%, after middle dipping dezincification, slag is treated with sulfuric acid and ammonium fluoride (fluorine ion 20g / l) to carry out acid leaching once, the leaching solution contains germanium 65.2mg / l, indium 241mg / l, iron 22.7g / l, the leaching residue is carried out the second acid leaching with sulfuric acid and ammonium fluoride (fluoride ion 10g / l) For leaching, the immersion solution contains germanium 10.75mg / l, indium 38mg / l, iron 4.78g / l, the secondary leaching tailing slag contains 0.0011% germanium, and the leaching rate of slag is 98.3%.

Embodiment 3

[0014] Example 3. The raw material contains 0.0219% germanium and 0.08% indium. After intermediate leaching, the leaching residue is acid-leached twice with hydrogen fluoride (fluoride ion 20g / l) and sulfuric acid. The leaching tailings contain 0.0048% germanium, and the leaching rate is 88.2%. After intermediate leaching with this raw material, acid leaching was carried out twice with sodium fluoride (fluoride ion 20g / l), leaching 0.0069% of tailing germanium, and the leaching rate was 87.9%.

[0015] Embodiment 4. Carry out the P204 kerosene system extraction indium with the one-time pickling solution of example 2, three-stage extraction rate 98%, ferric iron 5.2%. Raffinate is precipitated germanium with tannin / germanium=30, precipitation rate 98.6%, With tannin extract / germanium=90, the precipitated germanium precipitation rate is 94.5%, and with N235 kerosene system, under the condition of adding 5 times of germanium complexing agent, the three-stage extraction rate is 89....

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Abstract

A method for extracting germanium, indium and zinc from high iron, silicon and manganese materials containing germanium, indium and zinc belongs to the technology of hydrometallurgy. Sulfuric acid and fluoride are adopted for acid leaching for two times, leaching rate of germanium can reach 90% above, and secondary acid leaching slag contains germanium equal to and less than 0.005%. The total leaching rate of indium reaches 95% above, and tailings contain indium equal to and less than 0.003%. Germanium concentrate obtained by germanium extraction through an extraction method contains fluorine less than 1%. Low temperature leaching is performed at 70+-10 DEG C, the structure of iron vitriol slag is damaged as little as possible, and the concentration of ferric iron in leaching liquid is reduced. Ammonium iron hexafluoride produced in the leaching process shields the ferric iron, P204 indium extraction, N235 germanium or tannin extraction and tannin extract germanium deposit are improved, and the poisoning phenomenon in ferric iron of P204 and N235 is reduced. Comprehensive recovery utilization rate of germanium, indium and zinc in high iron, silicon and manganese materials is greatly improved.

Description

technical field [0001] The invention belongs to hydrometallurgy technology. Background technique [0002] High-iron silicomanganese materials containing germanium, indium, and zinc are residues of materials containing germanium, indium, zinc, and silicon dioxide or lead-zinc oxide ore leached by oxidative acid. Alkaline neutralization and oxidation treatment waste residue of zinc, iron and silicon dioxide wastewater. This kind of material is characterized by complex composition, low content of germanium, indium, and zinc, but high content of iron, with ferric iron accounting for more than 99%. Germanium mainly exists in the form of silicon-wrapped germanium, accounting for 80%, and 20% of which is absorbed by alum slag and calcium germanate. Zinc and indium are mainly in the state of hydrolysis precipitation and adsorption of alum slag. Indium and zinc are easily leached by conventional sulfuric acid leaching, but when P204 is used to extract indium, P204 is seriously poi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/08C22B3/26C22B19/20C22B58/00C22B41/00
CPCY02P10/20
Inventor 李世平张本聪余树华
Owner YUNNAN WUXIN IND
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