Preparation method of high-purity vanadium powder

A technology based on high-purity vanadium powder and vanadium pentoxide, which is applied in the field of preparation of high-purity vanadium powder, can solve the problems of harsh reaction conditions, expensive equipment, and high cost, and achieve low cost, easy operation, and low comprehensive energy consumption. Effect

Inactive Publication Date: 2019-02-01
CHONGQING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Aiming at the above-mentioned deficiencies in the prior art, the present invention provides a method for preparing high-purity vanadium powder, aiming at solving the technical problems of the prior art such as high cost, high energy consumption, expensive equipment, harsh reaction conditions, etc.

Method used

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  • Preparation method of high-purity vanadium powder

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Effect test

Embodiment 1

[0032] Take 100g of vanadium pentoxide (99.5%) powder and 350g of calcium chloride and sodium chloride (99%) eutectic molten salt, put into a high-energy ball mill and mill for 2 hours, then add 170g of calcium hydride powder (99%) and mix for 0.5h , put it into a vacuum tube furnace for thermal reduction, control the temperature in the furnace to 600°C, and after reduction in an argon atmosphere for 12 hours, perform vacuum thermal reduction to control the vacuum degree to be less than 5 Pa, and the reduction time is 16 hours. The reduced product is in the washing tank Wash with 1mol / L ammonium chloride solution, the temperature of the washing solution is 70°C, and the washing time is 7h. The washed product continues to be washed in the washing tank with 1mol / L sodium hydroxide solution and 1mol / L hydrochloric acid solution for 3 hours, and finally the product is dehydrogenated. The dehydrogenation temperature is 400°C, and then high Pure vanadium powder, its purity is 99.95%...

Embodiment 2

[0034] Take 110g of metavanadic acid (98%) powder and 350g of calcium chloride and sodium chloride (99%) eutectic molten salt, add high-energy ball mill for ball milling for 2h, then add 170g of calcium hydride powder (99%) and mix for 0.5h, Put it into a vacuum tube furnace for thermal reduction, control the temperature in the furnace to 600°C, and after reduction in an argon atmosphere for 12 hours, perform vacuum thermal reduction to control the vacuum degree to be less than 5Pa, and the reduction time is 16 hours. The reduced product is used in the washing tank. Wash in 1mol / L ammonium chloride solution, the temperature of the washing solution is 70°C, and the washing time is 7h. The washed product continues to be washed in the washing tank with 1mol / L sodium hydroxide solution and 1mol / L hydrochloric acid solution for 3 hours, and finally the product is dehydrogenated. The dehydrogenation temperature is 400°C, and then high Pure vanadium powder, its purity is 99.9%. Proc...

Embodiment 3

[0036] Take 100g of vanadium pentoxide (99.5%) powder and 350g of calcium chloride and sodium chloride (99%) eutectic molten salt, put into a high-energy ball mill and mill for 2 hours, then add 170g of calcium hydride powder (99%) and mix for 0.5h , put it into a vacuum tube furnace for thermal reduction, control the temperature in the furnace to 750°C, and after reduction in an argon atmosphere for 12 hours, perform vacuum thermal reduction to control the vacuum degree to be less than 5 Pa, and the reduction time is 16 hours. The reduced product is in the washing tank Wash with 1mol / L ammonium chloride solution, the temperature of the washing solution is 70°C, and the washing time is 7h. The washed product continues to be washed in the washing tank with 1mol / L sodium hydroxide solution and 1mol / L hydrochloric acid solution for 3 hours, and finally the product is dehydrogenated. The dehydrogenation temperature is 400°C, and then high Pure vanadium powder, its purity is 99.99%...

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Abstract

The invention discloses a preparation method of high-purity vanadium powder. The preparation method comprises the following steps: mixing vanadium-containing material with alkali metal or alkaline-earth metal chloride salt and then mixing with calcium hydride; then, carrying out vacuum thermal reduction to obtain a reduction product; washing the reduction product with ammonium chloride solution, alkaline liquor and acid liquor sequentially; and finally, carrying out dehydrogenation treatment to obtain high-purity vanadium powder. The preparation method has the advantages of being low in cost and energy consumption, moderate in reaction condition and safe in operation.

Description

technical field [0001] The invention belongs to the technical field of rare metal refining, and in particular relates to a preparation method of high-purity vanadium powder. Background technique [0002] With the development and progress of powder metallurgy technology, the application field of its main raw material, metal powder, has been continuously expanded, and the market demand has also increased sharply, and it is developing towards high purity and ultrafine. At present, the relatively mature metal powder preparation methods mainly include solid Phase method and gas phase method, and both methods have certain shortcomings and deficiencies. [0003] Although the solid-phase method (mechanical method) has a large amount of powder preparation, its energy utilization rate is low, and impurities are easily introduced during the preparation process. The prepared powder has a large particle size, wide distribution, and difficult to control the shape. Handling is difficult. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/20C22B34/22
CPCC22B34/22B22F9/20
Inventor 胡丽文扈玫珑徐建吕学伟党杰
Owner CHONGQING UNIV
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