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Preparation method of compact crystal form small-particle-size spherical cobalt carbonate

A cobalt carbonate, small particle size technology, applied in the direction of cobalt carbonate, positive electrode, active material electrode, etc., can solve the problems of unsatisfactory sphericity and tap density of cobalt trioxide, serious agglomeration, etc.

Active Publication Date: 2020-04-24
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cobalt carbonate system is the main production method in the battery-grade cobalt tetroxide industry. There are few studies on the small particle size part, especially the part less than 3 μm, and the sphericity and tap density of the cobalt trioxide prepared by the cobalt carbonate system cannot meet the needs of the next generation. product requirement
For example, "Small Particle Spherical Cobalt Tetroxide Doped with Aluminum and Its Preparation Method" CN 201811275016 .8 published by Zhongwei New Materials Co., Ltd. prepared cobalt tetraoxide with a D50 of 3.5 μm and a tap density of about 2.0 g / cm3; Li Yongguang et al. Phase preparation of small particle size spherical cobalt carbonate with high tap density" prepared 6μm cobalt carbonate with a tap density of 1.8 g / cm 3 ; Jingmen GEM New Material Co., Ltd. published "A Method for Preparation of Small-Size Spherical Cobalt Carbonate" CN201611066226.7, prepared particles of 3-5 microns shown by the electron microscope, but the agglomeration was serious, and the D5 detected by the laser particle size analyzer was greater than 19 μm

Method used

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  • Preparation method of compact crystal form small-particle-size spherical cobalt carbonate
  • Preparation method of compact crystal form small-particle-size spherical cobalt carbonate
  • Preparation method of compact crystal form small-particle-size spherical cobalt carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step 1. Preparation of solution: Weigh soluble aluminum salt and cobalt salt and add them into pure water to prepare a mixed salt solution containing aluminum as a raw material. The concentration of cobalt salt is 2 mol / L, and the mass ratio of aluminum to cobalt is 0.0063; The concentration is 2.9 mol / L ammonium bicarbonate solution;

[0030] Step 2, cobalt carbonate synthesis:

[0031] (1) Inject pure water and ammonium bicarbonate solution into the reactor as the bottom liquid, the ammonium bicarbonate concentration of the bottom liquid is 1.5 mol / L, the total bottom liquid volume accounts for 30% of the reactor volume, and sodium hexametaphosphate is added as a dispersant , the concentration is 3 g / L, and the pH value of the bottom solution is controlled at 8.5;

[0032] (2) In the first stage of liquid phase precipitation, firstly pump the mixed salt solution configured in step 1 into the second stage of liquid phase precipitation at a stirring speed of 280rpm for...

Embodiment 2

[0037] Step 1. Preparation of solution: Weigh soluble aluminum salt and cobalt salt and add them into pure water to prepare a mixed salt solution containing aluminum as a raw material. The concentration of cobalt salt is 1.7 mol / L, and the mass ratio of aluminum to cobalt is 0.013; The concentration is 2.2 mol / L ammonium bicarbonate solution;

[0038] Step 2, cobalt carbonate synthesis:

[0039] (1) Inject pure water and ammonium bicarbonate solution into the reactor as the bottom liquid, the concentration of the bottom liquid ammonium bicarbonate is 0.5 mol / L, the total bottom liquid volume accounts for 40% of the reactor volume, and add sodium hexametaphosphate as a dispersant , the concentration is 7 g / L, and the pH value of the bottom solution is controlled at 8.2;

[0040](2) In the first stage of liquid phase precipitation, firstly pump the mixed salt solution configured in step 1 separately for 2 hours at a stirring speed of 300 rpm, the reaction temperature is 45°C, a...

Embodiment 3

[0045] Step 1. Preparation of solution: Weigh soluble aluminum salt and cobalt salt and add them into pure water to prepare a mixed salt solution containing aluminum as a raw material. The concentration of cobalt salt is 2mol / L, and the mass ratio of aluminum to cobalt is 0.0067; 2.5mol / L ammonium bicarbonate solution;

[0046] Step 2, cobalt carbonate synthesis:

[0047] (1) Inject pure water and ammonium bicarbonate solution into the reactor as the bottom liquid, the concentration of the bottom liquid ammonium bicarbonate is 1.0 mol / L, the total bottom liquid volume accounts for 50% of the reactor volume, and add sodium hexametaphosphate as a dispersant , the concentration is 10 g / L, and the pH value of the bottom solution is controlled at 8.2;

[0048] (2) In the first stage of liquid phase precipitation, first pump the mixed salt solution prepared in step 1 separately for 1.5 hours at a stirring speed of 320rpm, and the reaction temperature is 30°C. After feeding until th...

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Abstract

The invention relates to the technical field of battery material preparation, in particular to a preparation method of cobalt carbonate. The invention provides a preparation method of compact crystalform small-particle-size spherical cobalt carbonate, which comprises the following steps of: by using cobalt salt as a raw material and ammonium bicarbonate as a precipitant, injecting pure water andammonium bicarbonate solution into a reaction kettle as a base solution, and adding sodium hexametaphosphate as a dispersing agent, then entering a first stage of liquid phase precipitation, independently pumping a mixed salt solution under a high-intensity stirring condition, feeding until the pH value is reduced to 7.4-7.8, then entering a second stage of liquid phase precipitation, and simultaneously pumping mixed salt and a precipitant solution to synthesize cobalt carbonate, after the volume of the materials reaches the upper limit of the reaction kettle, stopping feeding and stirring, pumping away the supernatant after solid-liquid layering, and then continuing feeding, and repeating the above steps so that the particles grow to 2-3 mum. The prepared spherical cobalt carbonate is small in particle size, uniform and non-sticky in particles and compact in crystal form.

Description

technical field [0001] The invention relates to the technical field of battery material preparation, in particular to a method for preparing cobalt carbonate. Background technique [0002] With the upgrading of products in the 3C field and the rapid development of various high-end smart devices, the requirements for thinner, lighter and higher capacity batteries are getting higher and higher. Cobalt tetroxide is an important raw material for the preparation of lithium cobalt oxide, a cathode material for lithium batteries, and its various properties determine the performance of lithium cobalt oxide cathode materials and downstream lithium-ion batteries. At present, in order to prepare high-energy and high-voltage battery products, it has become a common method for positive electrode manufacturers to increase the compaction density of positive electrode materials by blending cobalt tetraoxide with large and small particle sizes. A research hotspot. Lithium cobalt oxide cath...

Claims

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Application Information

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IPC IPC(8): C01G51/06H01M4/58H01M10/0525
CPCC01G51/06H01M4/5825H01M10/0525H01M2004/028C01P2004/03C01P2004/61Y02E60/10
Inventor 夏勇田礼平刘人生胡招文祝婷
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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