A kind of molybdenum removal method of ammonium tungstate liquid

Abstract

The invention provides a method for removing molybdenum from ammonium tungstate feed liquid, comprising: a vulcanization step, adding a vulcanizing agent to the ammonium tungstate feed liquid to obtain a vulcanized feed liquid; a step adsorption step, passing the vulcanized feed liquid through WDA918 resin Carry out one adsorption to saturation to obtain the liquid after the first adsorption, and carry out the second adsorption to saturation through the 201×7 resin to obtain the ammonium tungstate feed liquid for molybdenum removal, and use the two resins in combination to make Both resins achieved high adsorption capacity and had good adsorption effect.

Description

technical field

[0001] The invention relates to the field of utilization of rare metal resources, in particular to a method for removing molybdenum from ammonium tungstate liquid. Background technique

[0002] Due to the influence of the contraction of lanthanides, molybdenum and tungsten, the congener elements of the fifth period and sixth period (VIB), have similar properties, and are often symbiotic and associated in the same mineral, making separation difficult. Therefore, the separation of tungsten and molybdenum has always been a key and difficult issue in the tungsten smelting industry. At present, in the classic process of tungsten smelting in my country, the method of removing molybdenum from the ammonium tungstate solution is the combination of selective precipitation and ion exchange. In this method, the ammonium tungstate solution is pre-sulfurized, and the Mo and S 2- Thiomolybdate is formed, and then copper salt is added to remove it by coprecipitation, and th...

Examples

Embodiment 1

[0029] This embodiment provides a method for removing molybdenum from ammonium tungstate feed liquid, comprising:

[0030] In the vulcanization step, ammonium sulfide is added to the ammonium tungstate feed liquid as a vulcanizing agent, and stirred for 4 hours. After the stirring is completed, the concentration of molybdenum is 1.15g / L, S 2- The ion concentration is 3.06g / L, let it stand for 72 hours, and use a precision filter to remove particles and suspended solids in the feed liquid to make a vulcanized feed liquid.

[0031] In the cascade adsorption step, the vulcanization material liquid is adsorbed once through WDA918 resin. The mass of WDA918 resin is 467g, and the flow rate of the vulcanization material liquid is controlled at 15ml / min to obtain the liquid after the first adsorption. The concentration of molybdenum in the liquid after the first adsorption is controlled to be ≤0.1g / L, when it reaches 0.1g / L, it is the primary adsorption saturation, and the adsorption...

Embodiment 2

[0034] This embodiment provides a method for removing molybdenum from ammonium tungstate feed liquid, comprising:

[0035] In the vulcanization step, add ammonium sulfide as a vulcanizing agent to the ammonium tungstate feed liquid, stir for 8 hours, and after the stirring is completed, the molybdenum concentration is 1.15g / L, S 2- The ion concentration is 3.06g / L, stand still for 36 hours, and use a precision filter to remove particles and suspended solids in the feed liquid to make a vulcanized feed liquid;

[0036] In the cascade adsorption step, the simulated exchange column I (model φ5cm×70cm) was loaded with 467g of WDA918 resin, and the simulated exchange column II (model φ5cm×70cm) was loaded with 467g of 201×7 resin. Put the vulcanized feed liquid into the simulated exchange column I, and carry out primary adsorption by WDA918 resin. The flow rate of the vulcanized feed liquid is controlled at 20ml / min to obtain the liquid after the primary adsorption. When it reache...

Embodiment 3

[0041] This embodiment provides a method for removing molybdenum from ammonium tungstate feed liquid, comprising:

[0042] In the vulcanization step, ammonium sulfide is added to the ammonium tungstate feed solution as a vulcanizing agent, and stirred for 6 hours. After the stirring is completed, the molybdenum concentration is 2.5g / L, S 2- The ion concentration is 4.56g / L, let it stand for 54 hours, and use a precision filter to remove particles and suspended solids in the feed liquid to make a vulcanized feed liquid;

[0043] In the cascade adsorption step, the simulated exchange column I (model φ5cm×70cm) was loaded with 467g of WDA918 resin, and the simulated exchange column II (model φ5cm×70cm) was loaded with 467g of 201×7 resin. Put the vulcanized feed liquid into the simulated exchange column I, and carry out primary adsorption by WDA918 resin. The flow rate of the vulcanized feed liquid is controlled to be 25ml / min to obtain the liquid after the primary adsorption. W...

technical field

[0001] The invention relates to the field of utilization of rare metal resources, in particular to a method for removing molybdenum from ammonium tungstate liquid. Background technique

[0002] Due to the influence of the contraction of lanthanides, molybdenum and tungsten, the congener elements of the fifth period and sixth period (VIB), have similar properties, and are often symbiotic and associated in the same mineral, making separation difficult. Therefore, the separation of tungsten and molybdenum has always been a key and difficult issue in the tungsten smelting industry. At present, in the classic process of tungsten smelting in my country, the method of removing molybdenum from the ammonium tungstate solution is the combination of selective precipitation and ion exchange. In this method, the ammonium tungstate solution is pre-sulfurized, and the Mo and S 2- Thiomolybdate is formed, and then copper salt is added to remove it by coprecipitation, and th...

Examples

Embodiment 1

[0029] This embodiment provides a method for removing molybdenum from ammonium tungstate feed liquid, comprising:

[0030] In the vulcanization step, ammonium sulfide is added to the ammonium tungstate feed liquid as a vulcanizing agent, and stirred for 4 hours. After the stirring is completed, the concentration of molybdenum is 1.15g / L, S 2- The ion concentration is 3.06g / L, let it stand for 72 hours, and use a precision filter to remove particles and suspended solids in the feed liquid to make a vulcanized feed liquid.

[0031] In the cascade adsorption step, the vulcanization material liquid is adsorbed once through WDA918 resin. The mass of WDA918 resin is 467g, and the flow rate of the vulcanization material liquid is controlled at 15ml / min to obtain the liquid after the first adsorption. The concentration of molybdenum in the liquid after the first adsorption is controlled to be ≤0.1g / L, when it reaches 0.1g / L, it is the primary adsorption saturation, and the adsorption...

Embodiment 2

[0034] This embodiment provides a method for removing molybdenum from ammonium tungstate feed liquid, comprising:

[0035] In the vulcanization step, add ammonium sulfide as a vulcanizing agent to the ammonium tungstate feed liquid, stir for 8 hours, and after the stirring is completed, the molybdenum concentration is 1.15g / L, S 2- The ion concentration is 3.06g / L, stand still for 36 hours, and use a precision filter to remove particles and suspended solids in the feed liquid to make a vulcanized feed liquid;

[0036] In the cascade adsorption step, the simulated exchange column I (model φ5cm×70cm) was loaded with 467g of WDA918 resin, and the simulated exchange column II (model φ5cm×70cm) was loaded with 467g of 201×7 resin. Put the vulcanized feed liquid into the simulated exchange column I, and carry out primary adsorption by WDA918 resin. The flow rate of the vulcanized feed liquid is controlled at 20ml / min to obtain the liquid after the primary adsorption. When it reache...

Embodiment 3

[0041] This embodiment provides a method for removing molybdenum from ammonium tungstate feed liquid, comprising:

[0042] In the vulcanization step, ammonium sulfide is added to the ammonium tungstate feed solution as a vulcanizing agent, and stirred for 6 hours. After the stirring is completed, the molybdenum concentration is 2.5g / L, S 2- The ion concentration is 4.56g / L, let it stand for 54 hours, and use a precision filter to remove particles and suspended solids in the feed liquid to make a vulcanized feed liquid;

[0043] In the cascade adsorption step, the simulated exchange column I (model φ5cm×70cm) was loaded with 467g of WDA918 resin, and the simulated exchange column II (model φ5cm×70cm) was loaded with 467g of 201×7 resin. Put the vulcanized feed liquid into the simulated exchange column I, and carry out primary adsorption by WDA918 resin. The flow rate of the vulcanized feed liquid is controlled to be 25ml / min to obtain the liquid after the primary adsorption. W...

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