Preparation method of small-particle-size uniform-aluminum-doped spherical tricobalt tetraoxide

A technology with small particle size of cobalt tetroxide, which is applied in cobalt oxide/cobalt hydroxide, electrochemical generators, structural parts, etc., and can solve the problems of poor sphericity, small tap density, and low tap density of doped cobalt tetroxide, etc. Achieve the effects of narrow laser particle size distribution, guaranteed response time, and high tap density

Active Publication Date: 2019-02-19
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of using cobalt hydroxide system for wet doping is that the particle sphericity is poor, the tap density is too small, and it is difficult to reach 2.0g / cm 3
[0005] At present, the outstanding problems of doping with small particle size cobalt tetroxide are: 1. Doping elements are easy to separate out compounds, especially Al element, resulting in uneven doping; Loose, severe particle adhesion, large agglomerate particles, and low tap density

Method used

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  • Preparation method of small-particle-size uniform-aluminum-doped spherical tricobalt tetraoxide

Examples

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Embodiment 1

[0023] 1. To 15M 3 Pour high-concentration cobalt sulfate into the preparation tank, add water to prepare a cobalt salt solution with a metal ion concentration of 80g / L, weigh 20.4kg aluminum sulfate octadecanoate and 12kg complexing agent disodium EDTA and add it to the cobalt sulfate solution. The mass ratio of ions, EDTA and cobalt ions is 0.0014:0.01:1 to obtain a cobalt-aluminum mixed salt complex solution.

[0024] 2. Inject 2.5M into the reactor 3 Use pure water as the bottom liquid, turn on the stirring, raise the temperature to 75°C, blow in air, and the air flow rate is 30m 3 / h, adding a small amount of sodium hydroxide solution with a concentration of 160g / L to adjust the pH to 10.9;

[0025] 3. Add the cobalt-aluminum mixed salt complex solution configured in step 1 and the sodium hydroxide solution with a concentration of 160g / L into the reaction kettle at the same time under stirring, and the flow rate of the cobalt-aluminum mixed salt complex solution is 150L...

Embodiment 2

[0030] 1. To 15M 3 Pour high-concentration cobalt chloride into the preparation tank, add water to prepare a cobalt salt solution with a metal ion concentration of 100g / L, weigh 92.5kg of aluminum chloride hexahydrate and 18kg of complexing agent disodium EDTA and add them to the cobalt chloride solution , the mass ratio of aluminum ions, EDTA and cobalt ions is 0.007:0.012:1 to obtain a cobalt-aluminum mixed salt complex solution.

[0031] 2. Inject 2.5M into the reactor 3 Pure water is used as the bottom liquid, start stirring, heat up to 80°C, blow in air, the air flow rate is 38m 3 / h, adding a small amount of sodium hydroxide solution with a concentration of 280g / L to adjust the pH to 10.6;

[0032] 3. Under stirring, add the cobalt-aluminum mixed salt complex solution configured in step 1 and the sodium hydroxide solution with a concentration of 280g / L into the reaction kettle at the same time for precipitation reaction, and the flow rate of the cobalt-aluminum mixed s...

Embodiment 3

[0037] 1. To 15M 3 Pour high-concentration cobalt nitrate into the preparation tank, add water to prepare a cobalt salt solution with a metal ion concentration of 120g / L, weigh 350.1kg of aluminum sulfate nonahydrate and 12kg of complexing agent disodium EDTA and add them to the cobalt nitrate solution, and the aluminum ions , The mass ratio of EDTA to cobalt ions is 0.014:0.015:1 to obtain a cobalt-aluminum mixed salt complex solution.

[0038] 2. Inject 2.5M into the reactor 3 Use pure water as the bottom liquid, turn on the stirring, raise the temperature to 85°C, blow in air, and the air flow rate is 42m 3 / h, adding a small amount of sodium hydroxide solution with a concentration of 400g / L to adjust the pH to 10.3;

[0039] 3. Under stirring, add the cobalt-aluminum mixed salt complex solution configured in step 1 and the sodium hydroxide solution with a concentration of 400g / L into the reaction kettle at the same time for precipitation reaction, and the flow rate of th...

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Abstract

The invention relates to a preparation method of a lithium ion battery positive electrode material precursor, in particular to a preparation method of small-particle-size uniform-aluminum-doped spherical tricobalt tetraoxide. The preparation method includes following steps: 1, adding soluble aluminum salt and EDTA disodium into a cobalt salt solution to prepare a cobalt-aluminum mixed salt complexsolution; 2, injecting pure water into a reaction kettle to serve as base liquid, blowing in air, adding a small amount of sodium hydroxide solution to adjust pH, and rising temperature; 3, adding the cobalt-aluminum mixed salt complex solution and the sodium hydroxide solution into the reaction kettle for settling reaction while stirring; 4, sampling every 2h to measure granularity till reaching2-5um after more than 40h of reaction, and filtering and washing a material after the granularity reaches a target value; 5, thermally decomposing aluminum-doped hydroxyl cobalt after being washed sectionally to finally obtain small-particle-size uniform-aluminum-doped spherical tricobalt tetraoxide with uniform distribution of aluminum from inside to outside, tricobalt tetraoxide is compact andadhesion-free spherical particles in morphology, tap density is 2.0-2.7g / cm3, and laser granularity distribution is narrow.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion battery cathode material precursor, in particular to a preparation method of a high voltage lithium ion battery precursor tricobalt tetroxide. Background technique [0002] Cobalt tetroxide is the precursor of lithium cobalt oxide (LCO) cathode materials, and its terminal applications are batteries for 3C electronic products such as large-capacity mobile phones, notebook computers, and digital cameras. 3C batteries require high energy density and have high requirements for LCO cathode materials. The energy density of the battery can be increased by increasing the charging cut-off voltage and compaction density of LCO. The corresponding precursor cobalt tetroxide has two development trends: ① one is the change of particle size, which develops towards both ends of large particle size and small particle size, Large and small particles are mixed in a certain proportion to increase the compacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04H01M4/525H01M10/0525
CPCC01G51/04C01P2004/03C01P2004/32C01P2004/61C01P2006/11H01M4/525H01M10/0525Y02E60/10
Inventor 刘人生田礼平张荣洲熊铜兴夏勇秦才胜
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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