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Vanadium electrolytic solution and preparation method thereof

A technology of electrolyte and vanadium solution, which is applied in the field of energy chemistry, can solve the problems of low vanadium utilization rate, large loss, difficulty in removing aluminum and silicon elements to less than 0.02%, and achieve the effect of reducing vanadium loss

Active Publication Date: 2017-07-11
HEBEI IRON AND STEEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The vanadium utilization rate of this method is low, and the electrolyte purity also depends on the raw material V 2 o 5 the purity of
In the prior art, part of the impurities in vanadium pentoxide can be reduced by increasing the reaction steps and carrying out multiple acidic and alkaline dissolution and precipitation reactions alternately, but the loss of vanadium in this process is large, and aluminum and silicon elements are due to encapsulation and inclusion. and other reasons are difficult to remove to below 0.02%, and the content of aluminum and silicon elements in the prepared vanadium electrolyte is difficult to be lower than 30ppm after the vanadium concentration is 2mol / L

Method used

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  • Vanadium electrolytic solution and preparation method thereof
  • Vanadium electrolytic solution and preparation method thereof
  • Vanadium electrolytic solution and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0042] 1) Weigh 99.5g of ammonium metavanadate with a purity of 99.5% and a water content of about 10%, put it into 3L of water, slowly add sulfuric acid to pH 5, react at a constant temperature at 50°C for 50 minutes, and filter to obtain a vanadium concentration of 13g / L The purified vanadium solution; in the purified vanadium solution, sulfuric acid was added dropwise to adjust the pH to 3, and heated and stirred until boiling. After 180 minutes of reaction, the solid-liquid separation was completed to obtain the vanadium precipitation mother liquor and the ammonium polyvanadate solid phase. The solid material was washed with water Times

[0043] 2) The ammonium polyvanadate is calcined at 850°C for 3 hours under a reducing gas atmosphere to obtain a mixture containing vanadium tetroxide and vanadium trioxide, wherein the molar ratio of vanadium tetraoxide to vanadium trioxide is 1.01:1;

[0044] 3) Take the mixture obtained in step 2) and dissolve it with an aqueous sulfuric ac...

Embodiment 2

[0052] 1) Weigh 191g of ammonium metavanadate with a purity of 99.5% and a water content of about 10%, put it into 3L of water, slowly add sulfuric acid to a pH of 3, and react at a constant temperature at 99°C for 10 minutes to obtain a purification with a vanadium concentration of 25g / L Vanadium solution: Add sulfuric acid dropwise to the purified vanadium solution to adjust the pH to 1.5, heat and stir until boiling, and complete the solid-liquid separation after 40 minutes of reaction to obtain the vanadium precipitation mother liquor and the solid phase of ammonium polyvanadate;

[0053] 2) The ammonium polyvanadate is calcined at 980°C for 1 hour under a reducing gas atmosphere to obtain a mixture containing vanadium tetroxide and vanadium trioxide, wherein the molar ratio of vanadium tetraoxide to vanadium trioxide is 1.02:1;

[0054] 3) Take the mixture obtained in step 2) and dissolve it with an aqueous sulfuric acid solution to obtain a vanadium electrolyte with a vanadium...

Embodiment 3

[0056] 1) Weigh 160g of ammonium metavanadate with a purity of 99.5% and a water content of about 10%, put it into 3L of water, slowly add sulfuric acid to a pH of 4.8, and react at a constant temperature of 75°C for 30 minutes to obtain a purification with a vanadium concentration of 21g / L Vanadium solution: Add sulfuric acid dropwise to the purified vanadium solution to adjust the pH to 2.5, and heat and stir until boiling. After 130 minutes of reaction, the solid-liquid separation is completed to obtain the vanadium precipitation mother liquor and ammonium polyvanadate solid phase;

[0057] 2) The ammonium polyvanadate is calcined at 930°C for 2 hours under a reducing gas atmosphere to obtain a mixture containing vanadium tetroxide and vanadium trioxide, wherein the molar ratio of vanadium tetraoxide to vanadium trioxide is 0.95:1;

[0058] 3) Take the mixture obtained in step 2) and dissolve it with an aqueous sulfuric acid solution to obtain a vanadium electrolyte with a vanadi...

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Abstract

The invention relates to a vanadium electrolytic solution preparation method, which comprises: (1) using ammonium metavanadate with a purity of 99.0-99.5 wt% as a raw material, dissolving, filtering to obtain a purified vanadium dissolving solution, and carrying out acid ammonia precipitation to obtain an ammonium polyvanadate solid phase; (2) calcining the ammonium polyvanadate solid phase in a reducing atmosphere to obtain the mixture containing vanadium tetraoxide and vanadium trioxide, wherein a molar ratio of vanadium tetraoxide to vanadium trioxide is (0.95-1.05):1; and (3) carrying out acid dissolving on the mixture to obtain the vanadium electrolytic solution. According to the present invention, when the vanadium concentration of the vanadium electrolytic solution is 2 mol / L, the contents of impurities such as silicon, calcium and aluminum can be respectively reduced to less than 7 ppm, less than 10 ppm and less than 10 ppm, the total impurity content is less than 65 ppm, and the requirement of the vanadium battery vanadium electrolytic solution can be met; and compared to the acid and alkaline alternating impurity removing method, the method of the present invention has the following advantages that the vanadium loss can be significantly reduced, the vanadium recovery rate is more than 96.6%, the vanadium valence in the obtained vanadium electrolytic solution is +3.5, and the obtained vanadium electrolytic solution can be used directly as the vanadium battery electrolytic solution without activation.

Description

Technical field [0001] The invention relates to the technical field of energy chemistry, in particular to a vanadium electrolyte and a preparation method thereof. Background technique [0002] All vanadium redox flow battery (VRB) is an excellent energy storage device. The battery capacity depends on the amount of electrolyte and the concentration of vanadium ions. The electrolyte can be placed separately from the battery, with long battery life, high reliability, and fast charging and discharging. There are great development prospects in photovoltaic power generation, wind power generation, peak cutting and valley filling. The VRB battery has no solid state reaction, no change in the structure of the electrode material, and is cheap, safe and environmentally friendly, and low in operation and maintenance costs. [0003] As the active material of the vanadium battery electrode, the concentration and volume of the electrolyte determine the size of the battery capacity, and the sta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M8/18H01M10/0563
CPCH01M8/188H01M10/0563Y02E60/10Y02E60/50
Inventor 李兰杰闫浩徐从美祁健姜建海王海旭
Owner HEBEI IRON AND STEEL
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