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Method for preparing high-purity vanadium pentoxide by reducing and precipitating sodium vanadium solution

A technology of vanadium pentoxide and sodium pentoxide is applied in the field of preparing high-purity vanadium pentoxide by reduction and precipitation of sodium vanadium solution, which can solve the problems of complex process flow, introduction of impurity ions, poor impurity removal effect, etc. The effect of high vanadium yield and high production efficiency

Pending Publication Date: 2022-04-05
CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 A method for preparing high-purity vanadium pentoxide by reducing and precipitating vanadium liquid. The method has low operating cost, simple operation, short process flow, low environmental pollution, and high purity of the prepared vanadium pentoxide product, which has broad application prospects and economical value

Method used

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  • Method for preparing high-purity vanadium pentoxide by reducing and precipitating sodium vanadium solution

Examples

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Embodiment 1

[0046] This example is used to illustrate the method for preparing high-purity vanadium pentoxide by the two-step method of sodium vanadium solution according to the present invention.

[0047] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 3.54g sodium metabisulfite, then add sulfuric acid dropwise to control the pH to 2.0, then add 30.6g ammonium chloride, and stir at 75°C Reaction 3h. After the reaction is finished, the vanadium-precipitated product is obtained by filtration, the vanadium-precipitated product is beaten and washed twice with deionized water, filtered and dried to obtain APV.

[0048] (2) Dissolve the dried APV in sodium hydroxide solution, control the final pH value to 10.5, stir and react at 90°C for 12 hours, filter to obtain dark green filter cake and 490ml colorless vanadium solution, TV is 42.67g / L.

[0049] (3) Add 42.76 g of ammonium chloride to the colorless vanadium solution, stir and reac...

Embodiment 2

[0052] This example is used to illustrate the method for preparing high-purity vanadium pentoxide by the two-step method of sodium vanadium solution according to the present invention.

[0053] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 65ml of vanadyl sulfate solution with a concentration of 2.85mol / L, then add sulfuric acid dropwise to control the pH to 2.2, then add 51.53g of carbonic acid Ammonium Hydrogen (NH 3 content of about 21wt%), stirred and reacted at 85°C for 2h. After the reaction is finished, the vanadium-precipitated product is obtained by filtration, the vanadium-precipitated product is beaten and washed twice with deionized water, filtered and dried to obtain APV.

[0054] (2) Dissolve the dried APV in sodium hydroxide solution, control the end point pH value to 11, stir and react at 95°C for 9 hours, filter to obtain dark green filter cake and 540ml colorless vanadium solution, TV is 38.17g / L. ...

Embodiment 3

[0058] This example is used to illustrate the method for preparing high-purity vanadium pentoxide by the two-step method of sodium vanadium solution according to the present invention.

[0059] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 17.6g sodium sulfite, then add sulfuric acid dropwise to control the pH to 2.5, then add 48.62g ammonium sulfate, and stir at 95°C for 1h . After the reaction is finished, the vanadium-precipitated product is obtained by filtration, the vanadium-precipitated product is beaten and washed twice with deionized water, filtered and dried to obtain APV.

[0060] (2) Dissolve the dried APV in sodium hydroxide solution, control the end point pH value to 11.5, stir and react at 98°C for 6 hours, filter to obtain dark green filter cake and 485ml colorless vanadium solution, TV is 42.14g / L.

[0061] (3) Add 71.53 g of ammonium sulfate to the colorless vanadium solution, stir and react for 2 ...

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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 through reduction precipitation of a sodium vanadium solution. The method comprises the following steps: providing a sodium vanadium solution, adding an acid and a reducing agent, adjusting the pH value to 2-3, 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 by reducing and precipitating the sodium vanadium solution, the high-purity vanadium pentoxide with the purity of 99.99 wt% or above can be prepared.

Description

technical field [0001] The invention relates to the technical field of vanadium chemical industry and preparation of high-purity vanadium pentoxide, in particular to a method for preparing high-purity vanadium pentoxide by reduction precipitation of sodium vanadium solution. 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-reprecipi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/02
CPCY02P10/20
Inventor 彭穗刘波辛亚男姚洁
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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