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A method for selective extraction and separation of molybdenum from high-phosphorus tungsten-molybdenum mixed solution

A mixed solution and selective technology, applied in the field of tungsten and molybdenum metallurgy, can solve the problem of inability to directly handle and separate molybdenum, and achieve the effect of simple method

Active Publication Date: 2017-02-01
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the first time, the method adopts the method of controlling the acid concentration and adding hydrogen peroxide to treat the mixed solution containing high phosphorus tungsten and molybdenum, and then extracts, so that the molybdenum in the mixed solution containing high phosphorus tungsten and molybdenum can be effectively separated. The problem of extraction and separation of molybdenum by tungsten-molybdenum mixed solution also provides a new idea for the extraction and separation of molybdenum by high-phosphorus tungsten-molybdenum mixed solution

Method used

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  • A method for selective extraction and separation of molybdenum from high-phosphorus tungsten-molybdenum mixed solution
  • A method for selective extraction and separation of molybdenum from high-phosphorus tungsten-molybdenum mixed solution

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Experimental program
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Effect test

Embodiment 1

[0030] Organic phase composition (volume percentage): 90% TBP+10% sulfonated kerosene.

[0031] Raw material liquid: a company uses sulfur-phosphorus mixed acid to treat the leaching liquid obtained from high-molybdenum scheelite, containing WO 3 120.5g / L, Mo 12.05g / L, phosphoric acid concentration 1.3mol / L, sulfuric acid concentration 1.1mol / L.

[0032] Feed liquid adjustment: add H at a concentration of 30% to it 2 o 2 solution, H 2 o 2 The added amount is 1.4 times of the total amount of moles of tungsten and molybdenum. get containing WO 3 114.1g / L, Mo 11.41g / L, WO 3 / Mo=10 / 1, a hydrogen peroxide-containing feed solution with a phosphoric acid concentration of 1.2 mol / L and a sulfuric acid concentration of 1 mol / L.

[0033] Extraction and separation: the above-mentioned organic phase and aqueous phase feed liquid are subjected to 5-stage countercurrent extraction under the condition of 1 / 1 ratio, and the loaded organic phase is back-extracted with 4mol / L ammonia aqu...

Embodiment 2

[0036] Organic phase composition (volume percentage): 80% TBP+20% sulfonated kerosene.

[0037] Raw material liquid: a company uses phosphate to decompose high-molybdenum scheelite under alkaline conditions. The leaching liquid contains WO 3 105.3g / L, Mo 5.27g / L, phosphorus concentration 0.82mol / L, sodium hydroxide concentration 0.4mol / L.

[0038] Feed liquid adjustment: add sulfuric acid thereinto, the final feed liquid containing sulfuric acid concentration is 1.4mol / L; And add concentration is 30% H 2 o 2 solution, H 2 o 2 The added amount is 0.8 times of the total amount of moles of tungsten and molybdenum. The final result contains WO 3 90.5g / L, Mo 4.53g / L, WO 3 / Mo=20 / 1, a hydrogen peroxide-containing feed solution with a phosphorus concentration of 0.7mol / L and a sulfuric acid concentration of 1.4mol / L.

[0039] Extraction and separation: the organic phase and the aqueous phase feed liquid are subjected to 5-stage countercurrent extraction under the condition of ...

Embodiment 3

[0042] Organic phase composition (volume percent): 70% TBP+30% benzene.

[0043] Raw feed liquid: feed liquid contains WO 3 10.2g / L, Mo 102.9g / L, phosphorus concentration 4.5mol / L, nitric acid concentration 2.6mol / L, hydrochloric acid concentration 1.9mol / L.

[0044] Feed liquid adjustment: add H at a concentration of 30% to it 2 o 2 solution, H 2 o 2 The added amount is 1.2 times of the total amount of moles of tungsten and molybdenum. get containing WO 3 9g / L, Mo 90.8g / L, WO 3 / Mo=1 / 10, a hydrogen peroxide-containing feed solution with a phosphorus concentration of 4mol / L, a nitric acid concentration of 2.3mol / L, and a hydrochloric acid concentration of 1.7mol / L.

[0045] Extraction and separation: the above-mentioned organic phase and aqueous phase feed liquid are subjected to 7-stage countercurrent extraction under the condition of ratio 2 / 1, and the loaded organic phase is back-extracted with 1mol / L ammonium carbonate aqueous solution under the condition of ratio 2...

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Abstract

The invention relates to a method of selectively extracting and separating molybdenum from a high-phosphorus tungsten- and molybdenum-containing mixed solution. In the prior art, according to the process of extraction and separation of tungsten and molybdenum through complexation of hydrogen peroxide, when the content of phosphorus in the solution is higher than 0.005 mol / L, the extraction efficiency of the tungsten and the molybdenum is greatly reduced, so that the conventional process of extraction and separation of the tungsten and the molybdenum through complexation of the hydrogen peroxide cannot be used for directly treating the tungsten- and molybdenum-containing mixed solution being higher than 0.005 mol / L in the content of the phosphorus. According to the invention, by means of adjustment and control of the content of acid in the high-phosprous mixed solution, the tungsten and the molybdenum in the mixed solution can be reacted with the phosphorus completely to form tungstomolybdophosphate acid. By means of addition of a proper amount of the hydrogen peroxide, the phosphor-tungstic heteropoly acid and phospho-molybdic heteropoly acid are depolymerized to generate peroxy phosphotungstic acid and peroxy phospho-molybdic acid. By means of TBP as an extraction agent, the peroxy phospho-molybdic acid is extracted into an organic phase and then the loaded organic phase is subjected to reverse-extraction by an alkaline reverse-extraction agent. The method can treat the high-phosphorus tungsten- and molybdenum-containing mixed solution, is low in co-extraction of tungsten, can reach 70% in molybdenum extraction rate in a single stage, is low in the cost of the employed extraction agent and is easy to industrialize.

Description

technical field [0001] The invention belongs to the field of tungsten-molybdenum metallurgy, in particular to a method for selectively extracting and separating molybdenum from a high-phosphorus tungsten-molybdenum mixed solution. Background technique [0002] Tungsten is an indispensable strategic metal in the field of national defense and occupies an important position in the national military strategic reserve. In view of the current situation of resources, it is an inevitable trend to replace black tungsten with scheelite, and it is a strategic choice for the sustainable development of my country's tungsten industry. However, my country's scheelite resource endowment is relatively poor, and there are many impurities such as molybdenum and phosphorus. Tungsten and molybdenum belong to the VIB group in the periodic table of elements. Due to the influence of lanthanide shrinkage, the properties of tungsten and molybdenum are very similar. The separation of molybdenum has b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/38C22B34/34C22B34/36
CPCY02P10/20
Inventor 赵中伟李永立李江涛王文强
Owner CENT SOUTH UNIV
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