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A method for extracting and removing molybdenum from tungstate solution

A tungstate and solution technology, applied in the field of solution purification and impurity removal, can solve the problems of volatilization of diluent kerosene, unfavorable industrial application, accelerated extraction agent degradation, etc. Effect

Active Publication Date: 2019-08-20
JIANGXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The higher the negative divalent sulfur content in the organic phase, the more intense the heat release of the oxidation reaction, and the reaction temperature can reach above 90°C, which not only causes the significant volatilization of the diluent kerosene, but also accelerates the degradation of the extractant, which is not conducive to industrial applications

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  • A method for extracting and removing molybdenum from tungstate solution

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Embodiment 1

[0023] For the crude sodium tungstate solution containing 249g / L tungsten trioxide and 3g / L molybdenum, add sodium sulfide solution according to the molar ratio of sulfur molybdenum to 3, slowly add ammonium chloride under vigorous stirring to adjust the pH value to 9.5, Sulfurize at 70°C for 0.5 hours, then mix with new organic phase, extract at 25°C for 15 minutes to obtain an extracted organic phase and raffinate, the molybdenum content in the raffinate is 0.52g / L. Add sodium hydrosulfide solution to the above raffinate according to the molar ratio of sulfur and molybdenum to 6, sulfide and react at 70°C for 2 hours, then place the solution at 90°C and vacuum degree of -20kPa for 0.5 hours to volatilize and desulfurize, and use untreated The crude sodium tungstate solution containing 249g / L tungsten trioxide and 3g / L molybdenum added with vulcanizing agent absorbs volatilized volatilizing agent, and it can be observed that the color of the solution turns yellow and gradually...

Embodiment 2

[0026]For the crude ammonium tungstate solution containing 193g / L tungsten trioxide and 15.6g / L molybdenum, add ammonium sulfide solution according to the molar ratio of sulfur and molybdenum to 2, react for 2 hours at 10°C, and then mix with new organic phase , extracted at 10° C. for 30 minutes to obtain an extracted organic phase and a raffinate, and the molybdenum content in the raffinate was 1.52 g / L. Add the above raffinate to the ammonium sulfide solution according to the molar ratio of sulfur and molybdenum to 9, sulfide and react at 10°C for 8 hours, then place the solution at 40°C and vacuum degree of -95kPa for 2 hours to volatilize and desulfurize, and use The crude ammonium tungstate solution containing tungsten trioxide of 193g / L and molybdenum of 15.6g / L absorbs the volatilized vulcanizing agent, and it can be observed that the color of the solution turns yellow and gradually transitions to orange, indicating that volatilized volatilization agent involved in the...

Embodiment 3

[0029] For the crude ammonium tungstate solution containing 171g / L tungsten trioxide and 29.6g / L molybdenum, add ammonium sulfide solution according to the molar ratio of sulfur and molybdenum to 3, vulcanize at 45°C for 2 hours, and then mix with new organic phase , extracted at 40° C. for 15 minutes to obtain an extracted organic phase and a raffinate, and the molybdenum content in the raffinate was 2.18 g / L. The above new organic phase contains 5 wt.% methyltrialkylammonium chloride, 5 wt.% isooctyl alcohol, and 90 wt.% kerosene. Add the above raffinate to the ammonium sulfide solution according to the molar ratio of sulfur and molybdenum to 12, and react for 4 hours at 55°C for sulfidation, then divide the above-mentioned two-stage sulfided liquid into four parts, and one part of the solution is not subjected to vacuum desulfurization treatment. Directly carry out the second-stage extraction molybdenum removal operation; the other three solutions are vacuum desulfurized un...

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Abstract

The invention discloses a method for extracting and removing molybdenum from a tungstate solution. The method adopts two-stage sulfuration-solvent extraction to achieve deep purification of high-content molybdenum. Through the first stage of sulfidation treatment, most of the molybdenum in the solution is quickly converted into dithiomolybdate and trithiomolybdate, and then most of the molybdenum in the solution is extracted to the organic phase through a stage of extraction; the remaining small amount of molybdenum in the solution is passed through In the second stage of deep vulcanization, the molybdenum is further transformed into tetrathiomolybdate with stronger affinity with the extractant, and then the excess vulcanizing agent after vulcanization is removed and recycled by vacuum volatilization; after vacuum desulfurization treatment Solution, the molybdenum is deeply removed by two-stage extraction to obtain a purified solution. The invention has high utilization rate of the vulcanizing agent, low total consumption, less consumption of oxidant in the process of organic phase extraction, remarkably alleviates oxidation exothermic phenomenon, and is beneficial to prolonging the service life of the organic phase. There is no waste residue in the whole process of molybdenum removal, which can realize the deep molybdenum removal of high molybdenum solution.

Description

technical field [0001] The invention relates to a method for purifying and removing impurities from a solution, in particular to a method for extracting and removing molybdenum from a tungstate solution. Background technique [0002] The separation of tungsten and molybdenum has always been a technical problem that plagues tungsten smelting. Based on the subtle differences in certain properties of tungsten and molybdenum, different forms of separation methods such as precipitation, resin adsorption, and solvent extraction have been developed. Among them, the properties of tungsten oxophilic and molybdenum thiophilic are quite different, and most studies on the removal of molybdenum from tungstate solutions are based on this principle, and most of the molybdenum removal methods that have been industrially applied are also based on this principle. With the gradual reduction of high-quality tungsten mineral resources, the molybdenum content in the tungsten smelting system cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/44C22B3/26C22B34/36
CPCC22B3/44C22B34/36C22B3/26Y02P10/20
Inventor 曹才放董宏伟李小文王刚邱晓辰李昱芃聂华平徐志峰
Owner JIANGXI UNIV OF SCI & TECH
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