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

A technology of vanadium pentoxide and sodiumization, which is applied in the field of preparation of high-purity vanadium pentoxide by reduction hydrolysis of sodium vanadium solution, can solve the problems of poor impurity removal effect, low operating cost, and small environmental pollution, and meet the requirements of the equipment environment Friendly, strong adaptability of raw materials, improve the effect of comprehensive utilization

Pending Publication Date: 2022-04-12
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

[0008] 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 hydrolyzing 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 hydrolyzing sodium vanadium solution

Examples

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Effect test

Embodiment 1

[0045] This example is used to illustrate the method for preparing high-purity vanadium pentoxide by reduction hydrolysis of sodium vanadium solution according to the present invention.

[0046] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 5.85g oxalic acid dihydrate, then add sulfuric acid dropwise to control the pH to 1.5, and stir at 100°C for 0.5h. After the reaction is finished, filter, beat and wash the filter cake with deionized water twice, filter and dry to obtain a hydrolyzate.

[0047] (2) Dissolve the dried hydrolyzate in sodium hydroxide solution, control the end point pH value to 10.5, stir and react at 100°C for 3h, filter to obtain dark green filter cake and 485ml colorless vanadium solution, TV is 42.06g / L .

[0048] (3) Add 51.2 g of ammonium sulfate to the colorless vanadium solution, stir and react for 0.5 h, filter, wash and dry after the reaction to obtain a white solid.

[0049] (4) Roast th...

Embodiment 2

[0051] This example is used to illustrate the method for preparing high-purity vanadium pentoxide by reduction hydrolysis of sodium vanadium solution according to the present invention.

[0052] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 81ml of vanadyl sulfate solution with a concentration of 2.85mol / L, then add sulfuric acid dropwise to control the pH to 2.0, and stir at 95°C Reaction 2h. After the reaction is finished, filter, beat and wash the filter cake with deionized water twice, filter and dry to obtain a hydrolyzate.

[0053] (2) Dissolve the dried hydrolyzate in sodium hydroxide solution, control the end point pH value to 11.5, stir and react at 95°C for 9h, filter to obtain dark green filter cake and 565ml colorless vanadium solution, TV is 37.54g / L .

[0054] (3) Add 40.83 g of ammonium carbonate to the colorless vanadium solution, stir and react for 1 h, filter, wash and dry after the reaction to ob...

Embodiment 3

[0057] This example is used to illustrate the method for preparing high-purity vanadium pentoxide by reduction hydrolysis of sodium vanadium solution according to the present invention.

[0058] (1) Measure 500ml of sodium vanadium solution, add sulfuric acid dropwise to adjust the pH to neutral, add 12.9g of sodium metabisulfite, then add sulfuric acid dropwise to control the pH to 2.5, and stir at 98°C for 1 hour. After the reaction is finished, filter, beat and wash the filter cake with deionized water twice, filter and dry to obtain a hydrolyzate.

[0059] (2) Dissolve the dried hydrolyzate in sodium hydroxide solution, control the end point pH value to 11, stir and react at 98°C for 6 hours, filter to obtain dark green filter cake and 487ml colorless vanadium solution, TV is 43.86g / L .

[0060] (3) Add 60.49 g of ammonium chloride to the colorless vanadium solution, stir and react for 2 hours, filter, wash and dry after the reaction to obtain a white solid.

[0061] (4)...

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Abstract

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 reducing and hydrolyzing 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 1.5-3, carrying out a reduction reaction, after the reaction is finished, filtering to obtain a hydrolysate, and pulping and washing the hydrolysate with deionized water; dissolving the hydrolysate in a sodium hydroxide solution, controlling the final pH value to be 10.5-12, reacting for 3-12 hours, filtering to obtain a filter cake and a colorless vanadium solution, adding 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 at the temperature of 450-600 DEG C. According to the method for preparing the high-purity vanadium pentoxide through reductive hydrolysis of 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 reducing and hydrolyzing sodium vanadium solution. Background technique [0002] At present, the methods for preparing high-purity vanadium pentoxide from sodium vanadium solution mainly include extraction method, ion exchange method, chlorination method, chemical impurity removal method, redissolution method, etc. [0003] The process route of the extraction method is similar, mainly using the difference in solubility of substances in different organic solvents to selectively extract the vanadium or impurities in the vanadium solution to the organic phase, so that the vanadium and impurities are separated, so the extraction method can be divided into extraction Vanadium and extraction of impurities in two ways. Extracting vanadium is to use an organic ex...

Claims

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Application Information

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IPC IPC(8): C01G31/02
CPCY02P10/20
Inventor 刘波彭穗辛亚男杨亚东
Owner CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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