Method for preparing large-particle high-purity vanadium pentoxide

A technology of vanadium pentoxide and large particles, which is applied in the field of vanadium chemical industry, can solve the problems of high production cost, long process flow, and insufficient purity of vanadium pentoxide products, and achieve easy realization, simple process operation and good application foreground effect

Active Publication Date: 2018-12-11
HEBEI IRON AND STEEL
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned method has a long process flow, a lot of labor, and high production costs, and the purity of most vanadium pentoxide products cannot meet the requirements of vanadium for some high-end products.
[0005] In addition to the requirements on purity, some customers need larger particles and specific particle size range of vanadium pentoxide products in the application process, which poses new challenges for the preparation of vanadium pentoxide products

Method used

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  • Method for preparing large-particle high-purity vanadium pentoxide

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Experimental program
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Effect test

Embodiment 1

[0041] Such as figure 1 Shown, the present invention prepares large particle high-purity vanadium pentoxide according to the following steps.

[0042] (1) Weigh 300g of ammonium metavanadate with a water content of about 10%, put it into 5L of water, heat to 98°C to dissolve, add ammonia water until the pH value is 7.0, and after 10min, filter to obtain a vanadium-containing vanadium with a vanadium concentration of 23g / L purification fluid;

[0043] (2) Heat the vanadium-dissolved purification solution obtained in step (1) to boiling, gradient acid precipitation, add sulfuric acid dropwise to the vanadium-containing purification solution to adjust the pH, and stop at the pH values ​​of 5.8, 5.6, and 4.4 for 10 minutes to precipitate vanadium , continue to drop sulfuric acid to adjust the pH to 2.1, and precipitate vanadium for 60 minutes. During the entire process of vanadium precipitation, the temperature is controlled at 95-100°C. After the reaction is completed, filter to...

Embodiment 2

[0047] (1) Weigh 150g of ammonium metavanadate with a water content of about 10%, put it into 5L of water, heat to 95°C to dissolve, add ammonia water until the pH value is 7.5, and after 20min, filter to obtain a vanadium concentration of 11.5g / L. Vanadium purification solution;

[0048] (2) Heat the vanadium-dissolved purification solution obtained in step (1) to boiling, gradient acid precipitation, add sulfuric acid dropwise to the vanadium-containing purification solution to adjust the pH, and stop at the pH values ​​of 5.9, 5.5, and 4.7 for 15 minutes to deposit vanadium , continue to drop sulfuric acid to adjust the pH to 2.0, react for 50 minutes, and control the temperature at 90-100°C during the whole process of vanadium precipitation, filter after the reaction, and obtain the mother liquor of vanadium precipitation and high-purity large-particle solid-phase ammonium polyvanadate;

[0049] (3) Washing the high-purity large-particle solid-phase ammonium polyvanadate o...

Embodiment 3

[0052] (1) Weigh 300g of ammonium metavanadate with a water content of about 10%, put it into 5L of water, heat to 98°C to dissolve, add ammonia water until the pH value is 6.5, and after 30min, filter to obtain vanadium with a vanadium concentration of 23g / L purification fluid;

[0053] (2) Heat the vanadium-dissolved purification solution obtained in step (1) to boiling, gradient acid precipitation, add sulfuric acid to the vanadium-containing purification solution to adjust the pH, and stop at the pH values ​​of 6, 5.7, and 4.8 for 20 minutes to precipitate vanadium , continue to add sulfuric acid dropwise to adjust the pH to 2.4, react for 80 minutes, and control the temperature at 90-100°C during the whole process of vanadium precipitation, filter after the reaction, and obtain the mother liquor of vanadium precipitation and high-purity large-particle solid-phase ammonium polyvanadate;

[0054] (3) Washing the high-purity large-particle solid-phase ammonium polyvanadate o...

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Abstract

The invention relates to a method for preparing large-particle high-purity vanadium pentoxide. The method comprises the following steps: after dissolving ammonium metavanadate, adding an impurity removing agent; regulating the pH (Potential of Hydrogen) of a solution to 6.5 to 8.2 and carrying out vanadium dissolving; after the vanadium dissolving is finished, carrying out solid-liquid separationto obtain a vanadium-contained purification solution; heating the vanadium-contained purification solution; then regulating the pH to 6 to 5.8, 5.7 to 5.4, 4.8 to 4.0 and 2.4 to 1.9 in sequence at four phases and carrying out gradient vanadium deposition; after vanadium deposition is finished, carrying out the solid-liquid separation to obtain a vanadium deposition mother solution and solid-phaseammonium polyorthovanadate; carrying out calcination and deamination on the ammonium polyorthovanadate to obtain a vanadium pentoxide product with the purity of greater than or equal to 99.95 weight percent and the granularity of greater than or equal to 150mum. According to the method provided by the invention, a vanadium dissolving and gradient vanadium deposition method is adopted and impurityelements are greatly removed; meanwhile, the granularity of the vanadium pentoxide is accurately controlled, so that the content of particles with the size in a range of 180 to 230mum is greater thanor equal to 60 percent; the requirements of customers are met and the method has a good application prospect.

Description

technical field [0001] The invention relates to the field of vanadium chemical industry, in particular to a method for preparing large-particle high-purity vanadium pentoxide. Background technique [0002] Vanadium is a polyvalent element, its valence is V 2+ to V 5+ Transform between. High-efficiency, green, and emerging energy storage devices, all-vanadium redox flow batteries use this characteristic of vanadium, and use all-vanadium ion solution as the positive and negative electrolytes of the vanadium battery. 4+ / V 5+ , at the negative pole of the battery V 2+ / V 3+ Charge and discharge are mutually converted; the performance of the vanadium ion electrolyte directly affects the performance of the vanadium battery. In order to achieve its high quality, long life, high energy efficiency, and stable working conditions, vanadium pentoxide with a purity of more than 99.9% is generally used to produce its electrolyte. [0003] In the chemical synthesis industry, this c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2004/60C01P2006/80
Inventor 李兰杰闫浩祁健赵备备柳朝阳张振全
Owner HEBEI IRON AND STEEL
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