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Preparation method of vanadium trioxide

A technology of vanadium trioxide and ammonium vanadate, which is applied to vanadium oxide, electrochemical generators, fuel cells, etc., can solve the problems of complicated operation and high production process cost, and achieve simple production process operation, reduced production cost, and Coulomb Efficiency and energy efficiency without attenuation effect

Active Publication Date: 2018-02-06
PANZHIHUA UNIV
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of vanadium trioxide, to overcome the defects of high cost and complicated operation of the existing production process

Method used

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  • Preparation method of vanadium trioxide
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  • Preparation method of vanadium trioxide

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preparation example Construction

[0040] The invention provides a preparation method of vanadium trioxide, comprising the following steps (see the production process schematic diagram figure 1 ):

[0041] 1) Mix ammonium metavanadate or ammonium polyvanadate with oxalic acid (the mixing ratio is, the molar amount of vanadium: the molar amount of oxalic acid = 1:1.5~1:2.5), and add it to the deionized In water (the molar amount of vanadium: the volume of water is 8.5-10mol / L), carry out liquid phase reduction;

[0042] 2) After ammonium metavanadate or ammonium polyvanadate is completely dissolved, heat to boiling, concentrate the solution and evaporate to dryness to obtain a precursor;

[0043] 3) Calcining the obtained precursor for 2-4 hours under the protection of nitrogen at a temperature of 700-900° C., and cooling to room temperature under the protection of nitrogen to obtain vanadium trioxide.

[0044] In this production process, the main component obtained is (NH 4 ) 2 (VO) 2 (C 2 o 4 ) 3 The p...

Embodiment 1

[0047] Embodiment 1 adopts technique of the present invention to prepare vanadium trioxide

[0048]1) Mix analytically pure ammonium metavanadate with analytically pure oxalic acid dihydrate (mixing ratio: molar mass of vanadium: molar mass of oxalic acid = 1:1.5), and add in batches to deionized water at a temperature of 80°C (vanadium The molar weight: the volume of water=10mol / L), carry out liquid phase reduction;

[0049] 2) After the ammonium metavanadate is completely dissolved, heat to boiling, concentrate the solution and evaporate to dryness to obtain the precursor;

[0050] 3) After the obtained precursor was dried at 160°C, it was calcined for 2.5h under the protection of nitrogen at a temperature of 700°C, and cooled to room temperature under the protection of nitrogen. Finally, the purity of the obtained vanadium trioxide is 98.8%.

Embodiment 2

[0051] Embodiment 2 adopts technique of the present invention to prepare vanadium trioxide

[0052] 1) Mix analytically pure ammonium metavanadate with analytically pure oxalic acid dihydrate (mixing ratio: molar mass of vanadium: molar mass of oxalic acid = 1:2), and add in batches to deionized water at a temperature of 95°C (vanadium The molar weight: the volume of water=9mol / L), carry out liquid phase reduction;

[0053] 2) After the ammonium metavanadate is completely dissolved, heat to boiling, concentrate the solution and evaporate to dryness to obtain the precursor;

[0054] 3) The obtained precursor was dried at 100° C., calcined for 3 h under the protection of nitrogen at a temperature of 750° C., and cooled to room temperature under the protection of nitrogen. Finally, the purity of the obtained vanadium trioxide is 99.2%.

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Abstract

The invention discloses a preparation method of vanadium trioxide suitable for a vanadium battery. The preparation method comprises the following steps: enabling ammonium vanadate with a vanadium valence state of +5 valence and oxalic acid or solvent complex of the oxalic acid to have liquid-phase reduction in a reaction solvent, drying by distillation a reaction solution, and calcining, thus obtaining the vanadium trioxide. According to the preparation method, the +5-valence ammonium vanadate which is relatively low in price and available is adopted as a raw material to be reduced by the oxalic acid and to be calcined, thus obtaining the vanadium trioxide with purity reaching up to 99 percent, and except for the transfer loss in the production process, the yield of vanadium has no other loss. The production process is simple in operation, low in energy consumption, safe, low in requirement on equipment, suitable for industrialized mass production and capable of significantly decreasing the production cost of the vanadium trioxide.

Description

technical field [0001] The invention relates to a preparation method of vanadium trioxide and belongs to the field of chemical material synthesis. Background technique [0002] Vanadium trioxide is an important vanadium oxide, which is widely used in the production of high-vanadium iron and vanadium-nitrogen alloys, sensors, new electronic components, and battery production. Among them, vanadium trioxide has a good application prospect in the production process of the electrolyte of the all-vanadium redox flow battery. The process is simple, the reduction effect is good, and no other impurities are brought in. It has the advantages of both chemical reduction and electrolysis, which reduces the production cost of vanadium electrolyte. Therefore, once this method is proposed, it has attracted extensive attention from related industries. However, due to the high cost of preparing vanadium trioxide and the low purity of the product, this method for producing vanadium electrolyt...

Claims

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Application Information

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IPC IPC(8): C01G31/02H01M8/18
CPCC01G31/02C01P2006/40C01P2006/80H01M8/188Y02E60/50
Inventor 崔旭梅陈孝娥张贵刚蓝德均刘甜甜左承阳丁虎标候冰雪
Owner PANZHIHUA UNIV
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