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Method for preparing high-purity vanadium pentoxide from sodium vanadium solution through two-step method

A technology of vanadium pentoxide and vanadium liquid, applied in the direction of vanadium oxide, etc., can solve the problems of complex process flow, introduction of impurity ions, and low product purity, and achieve the effects of simple process, high vanadium yield, and high product purity

Pending Publication Date: 2022-05-06
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to overcome the defects of poor impurity removal effect, low product purity, complex process flow or introduction of impurity ions in the existing process for preparing vanadium pentoxide using sodium vanadium liquid as raw material, and to provide a sodium vanadium pentoxide The method for preparing high-purity vanadium pentoxide by vanadium liquid two-step method has low operating cost, simple and convenient operation, short technological process, little environmental pollution, and high purity of the prepared vanadium pentoxide product, which has broad application prospects and Economic Value

Method used

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  • Method for preparing high-purity vanadium pentoxide from sodium vanadium solution through two-step method

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Embodiment 1

[0046] This embodiment is used to illustrate the method that sodium vanadium solution two-step method of the present invention prepares high-purity vanadium pentoxide.

[0047] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 30ml of vanadyl sulfate solution with a concentration of 2.85mol / L, then add sulfuric acid dropwise to control the pH to 4.0, then add 26.23g of sulfuric acid Ammonium, stirred and reacted at 100°C for 0.5h. After the reaction is finished, filter to obtain the vanadium-precipitated product, wash the vanadium-precipitated product twice with deionized water, filter and dry to obtain SAV.

[0048] (2) Dissolve the dried SAV in sodium hydroxide solution, control the end point pH value to 10.5, stir and react at 90°C for 12 hours, filter to obtain dark green filter cake and 515ml colorless vanadium solution, TV is 41.2g / L.

[0049] (3) Add 53.26g ammonium sulfate in described colorless vanadium solutio...

Embodiment 2

[0052] This embodiment is used to illustrate the method that sodium vanadium solution two-step method of the present invention prepares high-purity vanadium pentoxide.

[0053] (1) Measure 500ml of sodium vanadium solution, first drop sulfuric acid to adjust the pH to neutral, add 23g dihydrate oxalic acid, then add dropwise sulfuric acid to control the pH to 5.0, then add 34.93g ammonium bicarbonate (NH 3 content of about 21wt%), stirred and reacted at 50°C for 3h. After the reaction is finished, filter to obtain the vanadium-precipitated product, wash the vanadium-precipitated product twice with deionized water, filter and dry to obtain SAV.

[0054] (2) Dissolve the dried SAV in sodium hydroxide solution, control the end point pH value to 11, stir and react at 95°C for 9h, filter to obtain dark green filter cake and 490ml colorless vanadium solution, TV is 39.4g / L.

[0055] (3) Add 71g ammonium bicarbonate in described colorless vanadium solution, stir reaction 1h, filter ...

Embodiment 3

[0058] This embodiment is used to illustrate the method that sodium vanadium solution two-step method of the present invention prepares high-purity vanadium pentoxide.

[0059] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 10.7g sodium sulfite, then add sulfuric acid dropwise to control the pH to 5.5, then add 25.17g ammonium chloride, and stir the reaction at 85°C 1h. After the reaction is finished, the vanadium precipitation product is obtained by filtration, and the vanadium precipitation product is beaten and washed twice with deionized water, filtered and dried to obtain SAV.

[0060] (2) Dissolve the dried SAV in sodium hydroxide solution, control the end point pH to 11.5, stir and react at 98°C for 3h, filter to obtain dark green filter cake and 490ml colorless vanadium solution, TV is 41.5g / L.

[0061] (3) Add 57.6g ammonium chloride in described colorless vanadium solution, stir reaction 2h, filter after re...

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Abstract

The invention relates to the technical field of vanadium chemical industry and high-purity vanadium pentoxide preparation, in particular to a method for preparing high-purity vanadium pentoxide from a sodium vanadium solution through a two-step method. The method comprises the following steps: providing a sodium vanadium solution, adding an acid and a reducing agent, adjusting the pH value to 4-6, then adding a first ammonium salt, carrying out a reaction, after the reaction is finished, filtering to obtain a vanadium precipitation filter cake, pulping and washing the filter cake with deionized water, and then drying; dissolving the dried product in a sodium hydroxide solution, controlling the final pH value to be 10.5-12, stirring for reaction, filtering to obtain a grey green filter cake and a colorless vanadium solution, adding a second ammonium salt into the colorless vanadium solution, filtering, washing and drying after the reaction is finished to obtain a white solid, and roasting the white solid to obtain vanadium pentoxide. According to the method for preparing the high-purity vanadium pentoxide from the sodium vanadium solution through the two-step method, the high-purity vanadium pentoxide with the purity being 99.99 wt% or above can be prepared.

Description

technical field [0001] The invention relates to the technical field of vanadium chemical industry and the preparation of high-purity vanadium pentoxide, in particular to a method for preparing high-purity vanadium pentoxide by a two-step method of sodium vanadium pentoxide. Background technique [0002] At present, the methods for preparing high-purity vanadium pentoxide from sodium vanadium solution mainly include redissolution method, chemical impurity removal method, extraction method, ion exchange method and chlorination method. [0003] To prepare high-purity vanadium pentoxide with sodium vanadium liquid as raw material, the most widely used method in industry is the re-dissolution method. The basic principle is that vanadium ions have different precipitation characteristics in different pH environments. Using this precipitation characteristic, The vanadium raw material can achieve the purpose of separating impurities after repeated precipitation-dissolution-reprecipit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCC01G31/02C01P2006/80Y02P10/20
Inventor 彭穗刘波姚洁文俊维
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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