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Method for extracting and separating tungsten from molybdate solution

A molybdate and solution technology is applied in the field of extraction and separation of tungsten, which can solve the problems of difficulty in separation and removal of tungsten and high separation cost, and achieve the effects of reducing the amount of co-extraction, improving the separation effect, and simplifying the synthesis process.

Inactive Publication Date: 2019-06-11
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the problems of difficulty in separating and removing tungsten from molybdate solution and high separation cost in the prior art, the purpose of the present invention is to provide a method for extracting and separating tungsten from molybdate solution, aiming at improving separation efficiency and shortening the separation process ,cut costs

Method used

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  • Method for extracting and separating tungsten from molybdate solution
  • Method for extracting and separating tungsten from molybdate solution
  • Method for extracting and separating tungsten from molybdate solution

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Feed liquid: ammonium molybdate solution containing tungsten, WO 3 27.95g / L, Mo 28.45g / L, WO 3 / Mo=0.982, pH value is 8.01.

[0044] Organic phase: 5% volume of mixed amine extractant + 65% volume of sulfonated kerosene + 30% volume of isooctyl alcohol, subjected to 0.20mol / L H 2 SO 4 acidification.

[0045] The acidification time is 30min, the acidification ratio is O / A=1:1 (V / V), the extraction ratio is O / A (the volume ratio of the acidified organic phase to the solid liquid)=1:1, and the temperature is 25°C. The equilibration time is 10min. The results are as follows: the raffinate (raffinate aqueous phase) contains WO 3 12.24g / L, Mo 27.01g / L, tungsten extraction rate 56%, molybdenum extraction rate 4.75%, tungsten-molybdenum separation coefficient β WO3 / Mo =25.77.

Embodiment 2

[0047] Feed liquid: ammonium molybdate solution containing tungsten, WO 3 21.77g / L, Mo 20.96g / L, WO 3 / Mo=1.04, pH value is 7.4.

[0048] Organic phase: 5% volume of mixed amine extractant + 55% volume of sulfonated kerosene + 40% volume of isooctyl alcohol, with 0.05mol / L H before extraction 2 SO 4 The organic phase is acidified according to O / A=1 / 1 (volume ratio of organic phase to acid) (acidified organic phase is obtained).

[0049] Acidifying agent (for acidifying the organic phase and the organic phase after stripping): 0.05mol / L H 2 SO 4 aqueous solution

[0050] Extraction agent: 0.2mol / L NH 3 ·H 2 O aqueous solution

[0051] Stripping agent: 3.0mol / LNH 3 ·H 2 O aqueous solution

[0052] Operation: first heat the feed liquid to volatilize and deammoniate (or directly use H 2 SO 4 ) the pH value of the seasoning liquid is reduced to 7.4, and it is used as the feed liquid for extraction and removal of tungsten after cooling to room temperature.

[0053] Th...

Embodiment 3

[0057] Feed liquid: sodium molybdate solution containing tungsten, WO 3 38.85g / L, Mo 60.35g / L, WO 3 / Mo=0.644, pH value is 8.5.

[0058] Organic phase: the sulfonated kerosene of the isooctyl alcohol+50% volume of the mixed amines extraction agent+40% volume of 10% volume, before the extraction with the HCl of 1.4mol / L to organic phase by comparison O / A=1 / 1 for acidification.

[0059] Extraction agent: 0.25mol / L NaOH aqueous solution

[0060] Stripping agent: 2.0mol / L NaOH aqueous solution

[0061] The feed liquid and the acidified organic phase are subjected to multi-stage countercurrent extraction. During the countercurrent extraction process, tungsten is enriched in the loaded organic phase (extraction layer), and molybdenum is enriched in the raffinate aqueous phase; the loaded organic phase is extracted and washed. The stripping agent is subjected to multi-stage countercurrent stripping to obtain a tungsten-rich stripping liquid. The organic phase after back-extrac...

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Abstract

The invention discloses a method for extracting and separating tungsten from a molybdate solution, and belongs to the field of extraction and separation of rare metals. The concentration of tungsten in the molybdate solution is firstly adjusted before extraction, so that the concentration of WO3 is not lower than 5 g / L, the mass ratio of WO3 to Mo in the solution is 1 / 50 to 1 / 1, the pH of the tungsten-containing molybdate solution is adjusted to be 7.5-8.0, an organic phase containing a mixed amine extractant is in contact with the tungsten-containing molybdate solution for single-stage or multi-stage countercurrent extraction, the tungsten is enriched in the loaded organic phase, and molybdenum remains in a raffinate aqueous phase; and the loaded organic phase is washed by the extractantand then de-extracted by a stripping agent to obtain a tungsten-rich stripping solution, the organic phase obtained after reverse extraction is acidified, circulated and used in an extraction section.The mixed amine extractant used in the method has the advantages of low cost, large saturation capacity and the like, and the effect of removing tungsten from the high-tungsten-content molybdate solution is good, the process is short, and the method is prone to realizing industrialization.

Description

technical field [0001] The invention belongs to the field of extraction and separation of rare metals, in particular to a method for extracting and separating tungsten from a molybdate solution. Background technique [0002] As important strategic metals of the country, tungsten and molybdenum are widely used in industrial production, national defense construction and other fields. Tungsten and molybdenum are strictly controlled impurity metals in molybdenum and tungsten metallurgical products respectively. The national standard GB10116-2007 stipulates that the molybdenum content in grade 0 APT (ammonium paratungstate) is not more than 20ppm, and the national standard GB / T3460-2007 stipulates that the tungsten content in MSA-0 grade ammonium molybdate products is not more than 150ppm. However, tungsten and molybdenum often coexist in their mineral resources, secondary resources and metallurgical intermediate materials, and their properties are very similar. It is very diffi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/28C22B34/36C22B34/34
CPCY02P10/20
Inventor 曾理王应松张贵清曹佐英李青刚关文娟肖连生
Owner CENT SOUTH UNIV
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