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Vanadium pentoxide purification method

A technology of vanadium pentoxide and vanadium oxychloride, applied in the field of purifying vanadium pentoxide and preparing high-purity vanadium pentoxide, can solve the problems of insufficient purity of vanadium pentoxide, strong corrosiveness of chlorine gas, difficulty in regeneration, etc. problem, to achieve the effect of less environmental pollution, high purity, and reducing the generation of three wastes

Active Publication Date: 2017-07-14
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the purity of the vanadium pentoxide obtained by this method is not high enough
[0005] In addition, there are also patent documents that use chlorine gas as a chlorination agent to extract vanadium, and the prepared vanadium pentoxide product has high purity, but chlorine gas is very corrosive, and requires high equipment and operation, which greatly increases the cost, and serious pollution is difficult to regenerate

Method used

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Embodiment 1

[0063] A method for purifying vanadium pentoxide, comprising the steps of:

[0064] (1) Chlorination: Mix 17.2 g of industrial-grade vanadium pentoxide with a raw material purity of 96.5% and anhydrous aluminum trichloride in a molar ratio of 1:4, and the reaction temperature is 170°C for 3.5 hours to obtain oxytrichloride Vanadium gas and alumina residue, the vanadyl chloride gas is condensed, and 24.12g of vanadyl chloride liquid is collected;

[0065] (2) Hydrolysis: Hydrolyze 5 mL of vanadium oxychloride in 110 mL of dilute ammonia water (1+2), filter to obtain 5.99 g of ammonium metavanadate and the filtrate, the filtrate is weakly alkaline with a pH of about 8;

[0066] (3) Pyrolysis: calcining ammonium metavanadate at 500°C for 3 hours in a pure air atmosphere to obtain 4.35 g of an orange-yellow solid product and ammonia gas;

[0067] (4) recovery of by-products: the aluminum oxide residue obtained in step (1) is reacted with hydrochloric acid to reclaim aluminum tric...

Embodiment 2

[0071] A method for purifying vanadium pentoxide, comprising the steps of:

[0072] (1) Chlorination: Mix 17.1 g of industrial-grade vanadium pentoxide with a raw material purity of 97.2% and anhydrous aluminum trichloride at a molar ratio of 1:1, react at a temperature of 160°C, and react for 2 hours to obtain vanadium oxychloride Gas and alumina residue, the vanadyl chloride gas is condensed, and 12.79g of vanadyl chloride liquid is collected;

[0073] (2) Hydrolysis: 5mL of vanadyl trichloride was hydrolyzed in 50mL of high-purity water, and liquid-solid separation obtained 0.17g of polyvanadic acid and filtrate, and the filtrate was strongly acidic with a pH less than 1;

[0074] (3) Pyrolysis: Calcining polyvanadic acid at 500°C for 3 hours in a pure oxygen atmosphere to obtain 0.15 g of orange-yellow vanadium pentoxide product and ammonia gas;

[0075] (4) By-product recovery: the aluminum oxide residue obtained in step (1) is reacted with hydrochloric acid to reclaim a...

Embodiment 3

[0078] A method for purifying vanadium pentoxide, comprising the steps of:

[0079] (1) Chlorination: Mix 18.7g of industrial-grade vanadium pentoxide with a raw material purity of 88.5% and anhydrous aluminum trichloride in a molar ratio of 1:2, and the reaction temperature is 170°C for 3.5 hours to obtain oxytrichloride Vanadium gas and alumina residue, the vanadyl chloride gas is condensed, and 15.45g of vanadyl chloride liquid is collected;

[0080] (2) Hydrolysis: 5mL of vanadyl trichloride is hydrolyzed in 100mL of ammonium chloride (pH is 9) aqueous solution, filters, obtains ammonium polyvanadate 1.04g and filtrate, and filtrate is strongly acidic pH and is 1;

[0081] (3) Pyrolysis: calcining ammonium polyvanadate at 500°C for 3 hours in a pure air atmosphere to obtain 0.92 g of orange-yellow vanadium pentoxide product and ammonia gas;

[0082] (4) By-product recovery: the aluminum oxide residue obtained in step (1) is reacted with hydrochloric acid to reclaim alumin...

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Abstract

The present invention provides a vanadium pentoxide purification method, which comprises: carrying out a reaction on vanadium pentoxide to be purified and anhydrous aluminum trichloride at a temperature of 150-200 DEG C in an inert atmosphere to obtain vanadium oxytrichloride gas and residue, and carrying out post-treatment on the vanadium oxytrichloride gas to obtain the high purity vanadium pentoxide, wherein the post-treatment comprises: condensing the vanadium oxytrichloride gas, carrying out hydrolysis, carrying out liquid-solid separation on the hydrolysis product to obtain a solid product and a liquid product, and carrying out pyrolysis on the slid product, wherein the residue and the liquid product can be recovered. According to the present invention, the method has characteristics of short process, effective production cost reducing, three-waste generation reducing, and low environmental pollution; the prepared vanadium pentoxide has the high purity (the purity of more than or equal to 99.99%) and can meet the requirements of vanadium aluminum alloys and all-vanadium batteries for aerospace and other fields; and the method provides the basis for the small batch or large-scale production of the high purity vanadium pentoxide.

Description

technical field [0001] The invention belongs to the technical field of purification of inorganic materials, and in particular relates to a method for purifying vanadium pentoxide, in particular to a new method for preparing high-purity vanadium pentoxide from industrial-grade vanadium pentoxide through a chlorination hydrolysis method. Background technique [0002] Vanadium is an important strategic resource, with many excellent physical and chemical properties, known as the metal "vitamin". Therefore, vanadium is widely used in many fields such as iron and steel, metallurgy and chemical industry. Among many vanadium products, vanadium pentoxide is the most stable and widely used. However, in recent years, ordinary vanadium pentoxide is facing the current situation of overproduction, sluggish sales market, and continuously falling prices. However, high-tech fields such as all-vanadium batteries, vanadium-aluminum master alloys, electrode materials, and catalysts have highe...

Claims

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Application Information

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IPC IPC(8): C01G31/02
CPCC01G31/02C01P2002/72C01P2006/80
Inventor 张红玲姜单单董玉明朱光锦徐红彬张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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