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Method for preparing high-sphericity-degree and large-particle cobaltosic oxide

A technology with high sphericity of cobalt trioxide, which is applied in the direction of cobalt oxide/cobalt hydroxide, electrical components, battery electrodes, etc., can solve the problem of rapid capacity cycle decay of lithium cobalt oxide batteries, battery energy density has not been improved, particle sphericity and serious problems. Density difference and other problems, to achieve the effect of strengthening natural ecological protection, high voltage, and less environmental pollution

Inactive Publication Date: 2016-07-27
HUNAN HINA NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Cobalt tetroxide D50 currently on the market is generally 5-8um, the particle size is too small, and the sphericity and density of the particles are poor. The main problems of the prepared lithium cobalt oxide battery are fast capacity cycle decay, low charge cut-off voltage, and the energy density of the battery has not been improved. , can no longer meet the requirements of high energy density 3C lithium batteries that people are increasingly pursuing, and the flow rate in the synthesis reaction process of the prior art is generally greater than 1200L / h, the flow rate is too large, and there are too many crystal nuclei, resulting in too small crystal nuclei particle size

Method used

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  • Method for preparing high-sphericity-degree and large-particle cobaltosic oxide
  • Method for preparing high-sphericity-degree and large-particle cobaltosic oxide
  • Method for preparing high-sphericity-degree and large-particle cobaltosic oxide

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Experimental program
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Effect test

Embodiment 1

[0041] Embodiment one: the cobalt salt raw material is made into the cobalt salt solution that cobalt salt content is 90g / L with deionized water; Precipitant is dissolved in deionized water, is mixed with the precipitant solution of 220g / L; Cobalt salt solution and The precipitant solution is injected into the reactor in a parallel flow mode, and stirred and heated for reaction. The injection rate of the cobalt salt solution is 800L / h, the injection rate of the precipitant solution is 900L / h, and the temperature in the reactor is controlled at 55 ℃, the rotation speed is 60r / min, and the particle size of the cobalt carbonate synthesized for the first time is controlled at about 8.0um; the cobalt carbonate synthesis process adopts a separate kettle process. After a period of reaction, when the number of crystallization reaches 6 times, the reaction kettle Transfer 1 / 2 of the slurry to other empty tanks to continue the reaction. After the reaction is complete, the product is wash...

Embodiment 2

[0043] Embodiment two: the cobalt salt raw material is made into the cobalt salt solution that cobalt content is 120g / L with deionized water; Precipitant is dissolved in deionized water, is filtered and is mixed with the precipitant solution of 250g / L; Cobalt salt solution and The precipitant solution is injected into the reaction kettle in parallel flow, and stirred and heated for reaction. The injection rate of the cobalt salt solution is 1200L / h, the injection rate of the precipitant solution is 1200L / h, and the temperature in the reaction kettle is controlled at 45 ℃, the rotation speed is 90r / min, and the particle size of cobalt carbonate synthesized for the first time is controlled at about 6.0um; the cobalt carbonate synthesis process adopts a separate kettle process. After a period of reaction, when the number of crystallization reaches 8 times, the reaction kettle Transfer 1 / 2 of the slurry to other empty tanks to continue the reaction. After the reaction is complete, ...

Embodiment 3

[0045] Embodiment three: the cobalt salt raw material is made into the cobalt salt solution that cobalt content is 110g / L with deionized water; Precipitant is dissolved in deionized water, is filtered and is mixed with the precipitant solution of 240g / L; Cobalt salt solution and The precipitant solution is injected into the reactor in parallel flow for synthesis reaction, the injection rate of the cobalt salt solution is 1200L / h, the injection rate of the precipitant solution is 1120L / h, the temperature in the reactor is 52°C, and the rotation speed is 80r / min, the particle size of the cobalt carbonate synthesized for the first time is controlled at about 7.0um; the cobalt carbonate synthesis process adopts a separate kettle process, and after a period of reaction, when the number of crystallization reaches 7 times, the slurry in the reactor is transferred 1 / 2 to other empty kettles. After the reaction is complete, the product is washed and centrifuged to finally obtain large-p...

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Abstract

The invention relates to a method for preparing high-sphericity-degree and large-particle cobaltosic oxide. The method includes the steps that at least one of cobalt chloride, cobaltous sulfate and cobalt nitrate serves as a raw cobalt salt material, and is purified and prepared to obtain a cobalt salt solution; at least one of ammonium carbonate, ammonium bicarbonate, sodium carbonate and sodium bicarbonate serves as a precipitant; a precursor is prepared with the solution direct precipitation method, and added into a reaction vessel with the concurrent adding method, the parameters of the injecting speed, the reaction temperature, the stirring speed, the PH value and the like of the solution are controlled, the batch-type crystallization technology and the kettle dividing technology are adopted, the chemical impurities of the precursor and the crystallinity degree, the granularity, the density and the like of crystals are effectively controlled, a precipitate precursor is synthesized, washing and centrifuging are carried out, then sintering is carried out twice, and the high-sphericity-degree and large-particle cobaltosic oxide is finally obtained. The method is simple in technology and low in cost, and the prepared cobaltosic oxide is high in cut-off voltage, tap density and stability.

Description

technical field [0001] The invention relates to a preparation method of tricobalt tetroxide, in particular to a preparation method of cobalt trioxide with high sphericity and large particles, belonging to the technical field of secondary rechargeable battery materials. Background technique [0002] With the continuous development of my country's economy and technology, the use of energy has also increased, especially the rapid development of industry, which consumes a lot of battery energy, and the harmful substances produced are likely to cause damage to the ecological environment. Therefore, the country puts forward higher requirements on the use of energy, not only to improve the efficiency of energy use, but also to achieve energy conservation and emission reduction, and to strengthen the purpose of natural ecological protection. Therefore, it is extremely important to improve the structure of battery energy devices, especially the preparation of high-purity battery ener...

Claims

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Application Information

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IPC IPC(8): C01G51/04H01M4/525
CPCC01G51/04C01P2004/03C01P2004/32C01P2004/61C01P2006/40H01M4/525Y02E60/10
Inventor 涂勇訚硕尹桂珍刘兴国
Owner HUNAN HINA NEW MATERIALS
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