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A method for preparing battery-grade sodium vanadyl fluorophosphate cathode material by using industrial waste vanadium and the prepared cathode material

A technology of sodium vanadyl fluorophosphate and positive electrode materials, which is applied in battery electrodes, secondary batteries, battery recycling, etc., and can solve problems such as poor carbon wrapping effect, material shape, easy agglomeration of particle size, and large drying shrinkage. Achieve the effect of improving commercial value, improving electrical performance, and reducing synthesis cost

Active Publication Date: 2022-07-12
湖南钠邦新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sol-gel method has a complicated process, large drying shrinkage, and the obtained material has irregular appearance and is easy to agglomerate; the product obtained by the hydrothermal method is small, the purity is not high, and the particle distribution is uneven. Carry out solid-phase carbon encapsulation treatment on the obtained precipitate, the operation process is cumbersome, and the carbon encapsulation effect is not good
The solid-phase method is simple to operate, but the prepared material has large particles, uneven distribution, poor cycle stability and rate performance
Secondly, the preparation method of sodium vanadyl fluorophosphate is obtained by one-step synthesis, and there are problems such as the morphology of the material, the control of particle size, and the ease of agglomeration in the one-step synthesis.
[0006] In summary, there are still many deficiencies in the preparation methods of sodium vanadyl fluorophosphate reported at present, and there is still a lot of room for improvement in the electrical properties of the prepared sodium vanadyl fluorophosphate
[0007] In addition, vanadium is an important strategic resource, which can only be obtained by smelting natural minerals. The smelting process will produce more vanadium-containing slag, and the main treatment methods for these slag are to recycle vanadium or discard them; there is no one in the industry. An effective method for directly preparing high-performance sodium-ion battery materials from vanadium-containing minerals or slag

Method used

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  • A method for preparing battery-grade sodium vanadyl fluorophosphate cathode material by using industrial waste vanadium and the prepared cathode material
  • A method for preparing battery-grade sodium vanadyl fluorophosphate cathode material by using industrial waste vanadium and the prepared cathode material
  • A method for preparing battery-grade sodium vanadyl fluorophosphate cathode material by using industrial waste vanadium and the prepared cathode material

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Experimental program
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Effect test

Embodiment 1

[0090] Take 90g of industrial waste vanadium, add 110ml of sodium hydroxide (pH=7.1), heat and stir for 3h, filter and wash 5 times, add 100ml of sulfuric acid (pH=4.5) to the filter residue, and react at 30°C for 2h , then, filter the above solution 3 times to obtain a dark green solution, add 20 g of sodium chlorate (1.05-1.1 of theoretical molar amount) under stirring at room temperature for 5 h to obtain a yellow solution; add phosphoric acid (concentration is 80%) Stir well to obtain a mixed solution (the V / P molar ratio is 1:6 to 8), and the solution is sprayed and pyrolyzed at 500° C. under an argon atmosphere (the injection rate is 100 ml / h, and the air inlet volume is 5 L / min), The collected vanadyl phosphate powder (XRD showed δ-VOPO 4 ); The collected vanadyl phosphate, sodium fluoride, sodium acetate and citric acid are 2: 1: 2: 3 (Na, V, P, F are in stoichiometric ratio according to mol ratio, and citric acid / vanadyl phosphate are 3 : 2) After mixing and manual g...

Embodiment 2

[0092] Take 90g of industrial waste vanadium, add 110ml of sodium hydroxide (PH=10), heat and stir for 3h, filter and wash 5 times, add 100ml of sulfuric acid (pH=4.5) to the filter residue, and react at 30°C for 2h , then, the above solution was filtered 3 times to obtain a dark green solution, and 20 g of sodium chlorate (1.05-1.1 of theoretical molar amount) was added under stirring at room temperature to react for 5 h to obtain a yellow solution; add phosphoric acid (concentration is 80%; The V / P molar ratio is 1:6 to 8) and stir to obtain a mixed solution. The solution is sprayed and pyrolyzed at 500 °C under an argon atmosphere (the injection rate is 100 ml / h, and the air inlet volume is 5 L / min), and the solution is collected. Vanadyl phosphate powder was obtained (XRD showed δ-VOPO 4 ); The collected vanadyl phosphate, sodium fluoride, sodium acetate and citric acid are 2: 1: 2: 3 (Na, V, P, F are in stoichiometric ratio according to mol ratio, and citric acid / vanadyl ...

Embodiment 3

[0094] Take 90g of industrial waste vanadium, add 110ml of sodium hydroxide (PH=8), heat and stir for 3 hours, filter and wash 5 times, add 100ml of sulfuric acid (pH=4) to the filter residue, and react at 30°C for 2 hours , then, the above solution was filtered 3 times to obtain a dark green solution, and 20 g of sodium chlorate (1.05-1.1 of theoretical molar amount) was added under stirring at room temperature to react for 5 h to obtain a yellow solution; add phosphoric acid (concentration is 80%; The V / P molar ratio is 1:6 to 8) and stir to obtain a mixed solution. The solution is sprayed and pyrolyzed at 500 °C under an argon atmosphere (the injection rate is 100 ml / h, and the air inlet volume is 5 L / min), and the solution is collected. Vanadyl phosphate powder was obtained (XRD showed δ-VOPO 4); The collected vanadyl phosphate, sodium fluoride, sodium acetate and citric acid are 2: 1: 2: 3 (Na, V, P, F are in stoichiometric ratio according to mol ratio, and citric acid / va...

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Abstract

The invention belongs to the field of sodium ion battery electrode materials, and specifically discloses a method for preparing a sodium ion battery sodium vanadyl fluorophosphate positive electrode material by using industrial waste vanadium. slag; carry out oxidative acid leaching of the alkali leaching slag, or carry out oxidation treatment after acid leaching in advance to obtain a vanadium-rich solution; add a phosphorus source to the vanadium-rich solution, and pre-convert it into vanadyl phosphate; fluorine source, sodium source, The vanadyl phosphate is mixed to obtain a mixture, which is then sintered in a protective atmosphere at 650-900° C. to obtain a sodium-vanadyl fluorophosphate cathode material for a sodium ion battery. The present invention innovatively obtains the vanadium source through the alkali leaching-oxidative acid leaching (or acid leaching+oxidation), and innovatively pre-reacts (transforms) the phosphorus source and the vanadium source into a vanadyl phosphate intermediate, and then pre-reaction Mixing reaction with fluorine source and sodium source can unexpectedly significantly improve the electrical properties of the prepared material, especially the initial capacity performance and cycle stability of the material.

Description

technical field [0001] The invention relates to the field of preparation of positive electrode materials for sodium ion batteries, in particular to a method for preparing battery-grade sodium vanadyl fluorophosphate positive electrode materials by using industrial waste vanadium. Background technique [0002] As a socially dominant electrochemical energy storage device, lithium-ion batteries have achieved good results in portable electronics (laptops, smart mobile devices, tablet computers, etc.), electric vehicles, and plug-in hybrid electric vehicles. application. At the same time, sodium-ion batteries have also received extensive attention due to their abundant reserves of sodium resources and their environmental friendliness. The research and development of sodium-ion batteries can alleviate the problem of limited battery development caused by the shortage of lithium resources to a certain extent, and is considered to be the next generation of electric batteries. It is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/455H01M4/485H01M4/58H01M10/054
CPCC01B25/455H01M4/582H01M4/5825H01M4/485H01M10/054C01P2002/72C01P2004/03C01P2006/40Y02W30/84
Inventor 张治安王涛胜孙学文赖延清张凯洪波李劼
Owner 湖南钠邦新能源有限公司