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Preparation method of large-particle-size and high-density spherical cobalt oxide

A technology of cobalt tetroxide and high density, applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of cracking, breaking and slowing of growth rate of product particles, and achieve the effect of uniform particle size distribution and preventing particle cracking or breaking.

Active Publication Date: 2016-03-16
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To meet the above requirements, there are the following difficulties: first, when the crystal particles grow to a certain particle size, especially above 15 μm, it is difficult to continue to grow. increase and instantaneously burst into nucleation, producing a large number of small particles; secondly, to obtain high-density cobalt tetroxide, it is necessary to prepare a denser cobalt carbonate precursor in the wet synthesis stage, but this large particle size cobalt carbonate occurs in the thermal decomposition stage Intense chemical reaction will release a large amount of CO 2 Gas, easy to cause cracking or breaking of product particles

Method used

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  • Preparation method of large-particle-size and high-density spherical cobalt oxide
  • Preparation method of large-particle-size and high-density spherical cobalt oxide
  • Preparation method of large-particle-size and high-density spherical cobalt oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] ①Inject a certain amount of ammonium bicarbonate solution into the reaction kettle as the bottom liquid and submerge the stirring paddle;

[0025] ②Raise the temperature to 50°C, add cobalt chloride solution with a concentration of 80g / L and ammonium bicarbonate solution with a concentration of 180g / L into the reaction kettle at the same time under stirring, and a precipitation reaction occurs. The pH value of the reaction solution is controlled during the feeding process to be 7.0, Until the material is filled to the top of the reactor; after the feeding is completed, stop stirring, and after the solid-liquid layer is separated, the supernatant is pumped away to make room for further feeding, so that the crystals continue to grow;

[0026] ③ Repeat the cycle process of feeding, standing for stratification, pumping supernatant, and continuing feeding for 9 times. At this time, the crystal grows until the seed crystal particle size reaches 9.4 μm;

[0027] ④Separate the ...

Embodiment 2

[0032] ①Inject a certain amount of ammonium carbonate solution into the reaction kettle as the bottom liquid and submerge the stirring paddle;

[0033] ②Raise the temperature to 70°C, add the cobalt sulfate solution with a concentration of 125g / L and the ammonium carbonate solution with a concentration of 210g / L into the reaction kettle at the same time under stirring, and a precipitation reaction occurs. During the feeding process, the pH of the reaction solution is controlled to be 8.2 until the material Fill up the reactor; after feeding, stop stirring, and after the solid-liquid layer is separated, remove the supernatant to make room for further feeding, so that the crystals continue to grow;

[0034] ③ Repeat the cycle process of feeding, standing for stratification, pumping supernatant, and continuing feeding for 12 times. At this time, the crystal grows until the seed crystal particle size reaches 11.8 μm;

[0035] ④Separate the reactor materials for the first time, tha...

Embodiment 3

[0040] ①Inject a certain amount of ammonium bicarbonate solution into the reaction kettle as the bottom liquid and submerge the stirring paddle;

[0041] ②Raise the temperature to 80°C, add cobalt nitrate solution with a concentration of 160g / L and ammonium carbonate solution with a concentration of 230g / L into the reaction kettle at the same time under stirring, and a precipitation reaction occurs. The pH of the reaction solution is controlled to be 6.7 during the feeding process until the material Fill up the reactor; after feeding, stop stirring, and after the solid-liquid layer is separated, remove the supernatant to make room for further feeding, so that the crystals continue to grow;

[0042] ③ Repeat the cycle process of feeding, standing for stratification, pumping supernatant, and continuing feeding for 10 times. At this time, the crystal grows until the seed crystal particle size reaches 10.3 μm;

[0043] ④Separate the reactor materials for the first time, that is, t...

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Abstract

The invention discloses a preparation method of large-particle-size and high-density spherical cobalt oxide. The preparation method aims at achieving the purposes that the median particle size D50 of the cobalt oxide is larger than or equal to 15 microns, particle size distribution is uniform, compacting density (TD) is larger than or equal to 2.2 g / cm<3>, and the large-particle-size and high-density spherical cobalt oxide can meet the development requirement of high-voltage lithium cobaltate. The preparation method of the cobalt oxide includes the cobalt carbonate synthesis stage and the spherical cobalt carbonate thermal decomposition stage. In the cobalt carbonate synthesis stage, a cobalt carbonate precursor prepared through many times of cyclic crystallization is compact and uniform in particle size distribution; due to the segmented thermal decomposition, cobalt carbonate is locally decomposed in the low-temperature pre-decomposing stage, a micro hole channel is formed, release of CO2 gas during subsequent decomposition is facilitated, and particles are prevented from crazing or being broken; in the high-temperature thermal decomposition stage, the particle surface is compact, and therefore the large-particle-size and high-density spherical cobalt oxide is prepared.

Description

technical field [0001] The invention relates to a preparation method of tricobalt tetroxide, in particular to a preparation method of spherical cobalt trioxide with large particle size and high density. Background technique [0002] 3C electronic products require lightness and compactness, and the corresponding batteries need to have high energy density. Small lithium-ion batteries with lithium cobalt oxide as the preferred cathode material are currently widely used in 3C electronic products. The compaction density of spherical lithium cobalt oxide can reach 4.1g / cm 3 , not only has a high tap density, but also because of its excellent fluidity and processing performance, it is very conducive to the coating of electrode sheets, and has become an important direction for the improvement of lithium cobalt oxide materials. Another way to increase the energy density of lithium-ion battery cathode materials is to increase the operating voltage of the material. At present, the ch...

Claims

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Application Information

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IPC IPC(8): C01G51/04
Inventor 徐伟刘人生金力田礼平熊铜兴曾凡志黄亚东黄超秦才胜
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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