Process for removing molybdenum from tungstate solution through ion exchange method

A technology of ion exchange and tungstate, which is applied in the field of solution purification and impurity removal, can solve the problems of resin exchange capacity attenuation, severe heat release of oxidation reaction, etc., and achieve the effect of shortening the vulcanization time

Active Publication Date: 2018-10-12
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the higher the content of negative divalent sulfur in the resin column, the more intense the heat release of the oxidation reaction, and the resin functional groups are easily degraded, resulting in the decline of resin exchange capacity.

Method used

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  • Process for removing molybdenum from tungstate solution through ion exchange method

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Experimental program
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Effect test

Embodiment 1

[0022] 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 and molybdenum to 3, then add ammonium chloride to adjust the pH value to 9.5, and vulcanize at 70°C React for 0.5 hours, then mix with new resin, stir and react at 40°C for 1 hour to obtain a section of molybdenum-loaded resin and a section of molybdenum-removed liquid. The molybdenum content in the first-stage molybdenum-removed liquid is 0.91g / L. A section of molybdenum-removed solution was added to sodium hydrosulfide solution according to the ratio of sulfur and molybdenum substances to 6, and the vulcanization reaction was carried out at 70°C for 2 hours, and then the solution was volatilized and desulfurized at 90°C and vacuum degree -20kPa for 2 hours, and used The crude sodium tungstate solution containing 249g / L tungsten trioxide and 3g / L molybdenum that has not been added with a vulcanizing agent ab...

Embodiment 2

[0025] 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 2.5, vulcanize at 10°C for 2 hours, and then mix with new resin, Stir and react at 10°C for 5 hours to obtain a section of molybdenum-loaded resin and a section of molybdenum-removed liquid, the molybdenum content of the first-stage molybdenum-removed liquid is 1.39g / L. Add ammonium sulfide solution to a section of molybdenum-removed solution according to the ratio of sulfur and molybdenum to 9, and react for 8 hours at 10°C for sulfidation, then place the solution at 40°C and vacuum degree of -95kPa for 2 hours for volatilization and desulfurization, and use untreated The crude ammonium tungstate solution containing 193g / L tungsten trioxide and 15.6g / L molybdenum added with vulcanizing agent absorbs the volatilized vulcanizing agent, and it can be observed that the color of the soluti...

Embodiment 3

[0028] For the crude sodium tungstate solution containing 181g / L tungsten trioxide and 28.9g / L molybdenum, add sodium sulfide solution according to the molar ratio of sulfur and molybdenum to 3, and then add ammonium chloride to adjust the pH to 9.5. Vulcanize for 1 hour, then mix with new resin, stir and react at 40°C for 4 hours to obtain a section of molybdenum-loaded resin and a section of molybdenum-removed liquid. The molybdenum content in the first-stage molybdenum-removed liquid is 2.52g / L. Add ammonium sulfide solution to a section of molybdenum-removed liquid according to the molar ratio of sulfur and molybdenum to 12, vulcanize and react at 70°C for 2 hours, then place the solution at 90°C and vacuum degree of -75kPa for 2 hours for volatilization and desulfurization, and use untreated The crude sodium tungstate solution containing 181g / L tungsten trioxide and 28.9g / L molybdenum added with vulcanizing agent absorbs the volatilized vulcanizing agent, and it can be obs...

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Abstract

The invention discloses a process for removing molybdenum from a tungstate solution through an ion exchange method. According to the process, deep purification of high content of molybdenum is achieved with adoption of a two-section sulfuration-resin adsorption molybdenum removal method. Through first-section sulfidizing, most molybdenum in the solution is converted into dithio-molybdate and trithio-molybdate under the condition of low quantity of sulfurizing agent, and most molybdenum is adsorbed to resin in a first-section adsorption molybdenum removal mode; through second-section deep sulfidizing, the small amount of molybdenum left in the solution is converted into tetrathiomolybdate having higher affinity with strong base anion exchange resin under the condition of excessively-high quantity of the sulfurizing agent, and then the redundant sulfurizing agent is removed from the sulfurized solution and recovered in a vacuum volatilization mode; and the solution is subjected to second-section adsorption molybdenum removal after vacuum sulfurizing, so that a purified solution is obtained, and deep removal of molybdenum is achieved.

Description

technical field [0001] The invention relates to a solution purification and impurity removal process, in particular to a process for removing molybdenum from a tungstate solution by ion exchange. Background technique [0002] The separation of tungsten and molybdenum has always been a technical problem that plagues tungsten smelting. With the gradual reduction of high-quality tungsten mineral resources, the molybdenum content in the tungsten smelting system continues to increase, which has caused greater pressure on the existing molybdenum removal process based on sulfidation reactions. On the one hand, the time required for complete conversion of molybdenum to tetrathiomolybdate is further extended; on the other hand, the consumption of vulcanizing agent is significantly increased, and the oxidant required for subsequent conversion of thiomolybdate to molybdate also increases accordingly. [0003] Due to the increase of molybdenum content, in order to completely vulcanize ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B34/36C22B3/42C22B34/34
CPCC22B3/42C22B34/34C22B34/36Y02P10/20
Inventor 曹才放李昱芃聂华平李小文邱晓辰王刚董宏伟张柏朝
Owner JIANGXI UNIV OF SCI & TECH
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