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A kind of stripping germanium method from germanium-containing fluorosilicate solution

A fluosilicic acid and extraction technology, applied in the field of hydrometallurgy, can solve the problems of poor organic phase regeneration ability, large amount of washing liquid, and large amount of wastewater, and achieve the effects of improving regeneration ability, reducing production cost, and reducing loss rate

Inactive Publication Date: 2017-06-16
GUIZHOU HONGDA ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction rate of Ge in this process is all above 90%, but its stripping is not complete, and the purity of stripped germanium is low, and then causes, N 235 The regeneration of the organic phase is not good, and the extraction rate is getting lower and lower as the extraction-stripping cycle continues
Even if it is N 235 Poor regeneration of the organic phase, which in turn makes the extraction and stripping of germanium more expensive
And the reason that produces such technical problem is: N 235 While Ge is extracted, Si and F are also partially extracted, but only NaOH stripping is used, and the stripping of Ge, Si, and F is not complete; and the stripped Si exists in the NaOH solution in the form of sodium silicate. Solubility is not high, and the solubility of F in NaOH solution is not high in the form of NaF, which is easy to produce crystal precipitation, which affects the phase separation resolution and phase separation speed of alkali stripping, and then hinders the carrying out of alkali stripping germanium, increasing The cost and difficulty of alkali stripping treatment
[0003] For this reason, further research and discussion have been made by researchers in combination with the above-mentioned defects, that is, CaCl is used before and after alkali stripping. 2 The solution is washed with the organic phase in order to replace Si with CaSiO 3 , F and CaF 2 eluted, but due to CaSiO 3 and CaF 2 Both are compounds with low solubility, when CaCl 2 When the washing solution is repeatedly washed, a large amount of sediment will be produced, which will separate the organic phase and make it difficult to settle. CaCl must be replaced every time. 2 washing solution, resulting in CaCl 2 The amount of washing liquid is large, and the amount of waste water generated is large
At the same time Cl - Under alkaline conditions to be N 235 Partial extraction, the regeneration of the organic phase is not good, and the extraction rate of Ge will be affected when it is returned to use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for stripping germanium from germanium-containing fluorosilicate solution, using N 235 Extract the germanium from the germanium-containing fluorosilicate solution to obtain the raffinate; then use the sodium hydroxide solution containing ammonium ions to perform back-extraction treatment on the extracted organic phase to obtain the back-extraction solution; then add sulfuric acid solution to the back-extraction solution The pH is adjusted to 9, so that the germanium undergoes hydrolysis treatment, and the filter residue is obtained by filtering; the filter residue is calcined at a temperature of 400° C. to obtain the germanium concentrate. The finally obtained germanium concentrate contains 7% germanium, 0.5% F and 4% Si.

[0026] In the above with N 235 Extract germanium from germanium-containing fluorosilicate solution by using N 235 - Kerosene system extracts germanium from germanium-containing fluorosilicate solution. where N 235 - The kerosene system i...

Embodiment 2

[0033] A method for back-extracting germanium from a germanium-containing fluorosilicate solution, using N235 to extract germanium from the germanium-containing fluorosilicate solution to obtain an extraction residue; and then using a sodium hydroxide solution containing ammonium ions to reverse the extracted organic phase Extraction treatment to obtain a back-extraction solution; adding sulfuric acid solution to the back-extraction solution to adjust the pH to 11, so that the germanium undergoes hydrolysis treatment, filtering to obtain a filter residue; calcining the filter residue at a temperature of 500°C to obtain a germanium concentrate. The finally obtained germanium concentrate contains 10% germanium, 0.3% F and 3% Si.

[0034] In the above, using N235 to extract germanium from the germanium-containing fluorosilicate solution is to use the N235-kerosene system to extract germanium from the germanium-containing fluorosilicate solution. The N235-kerosene system is 30% N2...

Embodiment 3

[0040] A method for back-extracting germanium from a germanium-containing fluorosilicate solution, using N235 to extract germanium from the germanium-containing fluorosilicate solution to obtain an extraction residue; and then using a sodium hydroxide solution containing ammonium ions to reverse the extracted organic phase Extraction treatment to obtain a back-extraction solution; adding sulfuric acid solution to the back-extraction solution to adjust the pH to 10, so that the germanium undergoes hydrolysis treatment, filtering to obtain a filter residue; calcining the filter residue at a temperature of 450°C to obtain a germanium concentrate. The finally obtained germanium concentrate contains 8% germanium, 0.1% F and 2% Si.

[0041] In the above, using N235 to extract germanium from the germanium-containing fluorosilicate solution is to use the N235-kerosene system to extract germanium from the germanium-containing fluorosilicate solution. The N235-kerosene system is 30% N23...

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Abstract

The invention relates to the technical field of hydrometallurgy, in particular to a method for back extraction of germanium from a germanium-contained fluosilicic acid solution. The germanium-contained fluosilicic acid solution is extracted with an N235-kerosene system serving as an organic phase, a sodium hydroxide solution containing ammonium ions is adopted for treating the organic phase, sulfuric acid is added to a back extraction solution to adjust the PH value, then, germanium hydrolysis treatment is performed, obtained precipitate is calcined, germanium is obtained, and the quality of germanium concentrate is further improved, so that in the germanium concentrate, the content of germanium is larger than or equal to 7%, the content of F is smaller than 0.5%, and the content of Si is smaller than 4%; the extraction rate of germanium in germanium-contained fluosilicic acid is increased, and the extraction cost of germanium in the germanium-contained fluosilicic acid solution is reduced.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for stripping germanium from a germanium-containing fluorosilicate solution. Background technique [0002] The raw material containing germanium and high silicon is treated by acid leaching with fluoride, and then produced by tannin precipitation method, which has high production cost and low yield. Therefore, some researchers applied N to the germanium-containing fluorosilicate solution obtained after the germanium-containing high-silicon raw material was treated with fluoride acidic leaching. 235 Ge was extracted under the condition of adding Ge complexing agent, and NaOH solution was used for alkaline stripping. The extraction rate of Ge in this process is all above 90%, but its stripping is not complete, and the purity of stripped germanium is low, and then causes, N 235 The regeneration of the organic phase is not good, and the extraction rate is getting l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B41/00C22B3/26
CPCY02P10/20
Inventor 李世平倪常凯陈磊王志斌
Owner GUIZHOU HONGDA ENVIRONMENTAL PROTECTION TECHNOLOGY CO LTD
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