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Battery-grade cobaltosic oxide preparation method

A technology of tricobalt tetroxide and battery level, which is applied in the direction of cobalt oxide/cobalt hydroxide, etc., which can solve the problems of complex process, uneven particle size range of powder, large battery volume, etc., and achieve optimized preparation process, narrow particle size distribution and chemical purity high effect

Inactive Publication Date: 2010-12-15
JIANGSU DONGXIN ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Cobalt tetroxide produced by the traditional method is amorphous, and the particle size range of the powder is wide and uneven, so that the tap density of the positive electrode material produced by it is low, resulting in a large battery volume, so it cannot meet the current development of the lithium-ion battery industry. Require
Although, by improving the existing precipitation-thermal decomposition process, researchers can obtain tricobalt tetroxide powder with regular shape. The preparation method of tricobalt tetroxide powder, the method reacts soluble cobalt salt solutions such as cobalt chloride and cobalt acetate with ammonium bicarbonate solution in a reaction kettle to obtain a cobalt carbonate precipitate, and the cobalt carbonate precipitate is washed and filtered at a certain temperature Drying, and finally calcining to obtain the final octahedral cobalt tetroxide powder, but the cobalt tetroxide produced by this method has a high impurity content, which cannot effectively control the content of magnetic metal foreign matter (such as Fe, Ni, Cr, Zn, etc.), resulting in poor consistency of the battery , poor electrochemical performance, poor safety performance and other defects
[0004] Because the particle size distribution, density, and microscopic morphology of cobalt tetroxide products have a great influence on the particle size and particle crystallinity of its precursor, it is also very important to control various operating conditions in the process of preparing its precursor cobalt salt. Patent application The Chinese invention patent application No. 200710156482.X discloses a preparation of precursor by complexation-homogeneous precipitation method, that is, the cobalt liquid is prepared into a complexed cobalt salt solution, and then the synthesis of the precursor is controlled by adding a precipitant solution Obtain a monodisperse precipitate precursor, separate the generation and growth of crystal nuclei, and obtain cobalt tetroxide with high purity, uniform particle size, and high tap density. However, this method is complicated in process and cannot effectively control the content of magnetic metal foreign matter. Cause defects such as poor battery consistency, poor electrochemical performance, and poor safety performance

Method used

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  • Battery-grade cobaltosic oxide preparation method
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  • Battery-grade cobaltosic oxide preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Use deionized water to make industrial-grade cobalt sulfate into a solution with a cobalt concentration of 60g / L, use deionized water to make ammonium bicarbonate into a precipitant solution with a concentration of 100g / L, and massage the cobalt solution and the precipitant solution Il ratio, cobalt: precipitating agent=1.0: 2.1, add reaction container with co-current feeding method, the adding speed of described cobalt solution and the adding speed of described precipitating agent solution are determined according to container size, control the reaction that precursor is synthesized The temperature is 60°C, the reaction pH value is 7.0, the stirring speed is 300rpm, and the reaction time is . The precursor is prepared by the homogeneous crystallization precipitation method. The precursor is washed with 80°C deionized water for 3 times and then dehydrated. The water content of the filter cake is 25%, put it directly into a bowl, put it into a roasting furnace and bake it...

Embodiment 2

[0042] With deionized water, industrial-grade cobalt nitrate is prepared into a solution with a cobalt concentration of 80g / L, and with deionized water, ammonium carbonate is made into a precipitant solution with a concentration of 80g / L, and the cobalt solution and the precipitant solution are molarally Ratio, cobalt: precipitating agent=1.0: 3.0, add reaction container with co-current feeding method, control the reaction temperature of precursor synthesis to be 80 ℃, reaction pH value is 8.5, stirring speed is 500rpm, and reaction time is 15 hours, with average The precursor was prepared by phase crystallization and precipitation method. The precursor was washed with deionized water at 90°C for 5 times and then dehydrated. The water content of the filter cake was 24%. , naturally cooled to below 400°C and released from the furnace, lowered to room temperature, after crushing and grading, metal foreign matter was removed by iron remover to obtain spherical cobalt trioxide powd...

Embodiment 3

[0044] Use deionized water to make industrial-grade cobalt chloride into a solution with a cobalt concentration of 70g / L, use deionized water to make sodium carbonate into a precipitant solution with a concentration of 100g / L, and massage the cobalt solution and the precipitant solution Il ratio, cobalt: precipitating agent=1.0: 3.8, add reaction vessel with co-current feeding method, control the reaction temperature of precursor synthesis to be 100 ℃, the reaction pH value is 9.0, stirring speed is 500rpm, and the reaction time is 8 hours, with The precursor was prepared by homogeneous crystallization precipitation method. The precursor was washed with deionized water at 100°C for 5 times and then dehydrated. The water content of the filter cake was 24%. Hours, naturally cooled to below 400°C and released from the furnace, lowered to room temperature, after crushing and grading, metal foreign matter was removed by iron remover to obtain spherical cobalt trioxide powder, D 10 ...

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Abstract

The invention relates to a battery-grade cobaltosic oxide preparation method, which comprises the following steps of: preparing solution of cobalt and solution of precipitator from a cobalt raw material and a precipitator by using de-ionized water respectively; preparing a precursor by using a homogeneous crystallization precipitation method, wherein the precipitate precursor is synthesized by adding the prepared solution of cobalt at a certain concentration and the solution of precipitator at a certain concentration into a reactor according to a certain molar ratio by using a cocurrent-flow feeding method, and effectively controlling chemical impurities, crystallinity of crystals, granularity, density and the like of the precursor by controlling parameters such as reaction temperature, feeding speed, pH value and stirring speed; directly filling a water-containing filter cake into a pot after washing and dewatering, and controlling grain size and crystal shape by using low-temperature dehydration phase-change calcination and high-temperature nodulizing sintering; crushing by using a machine and performing classified activation treatment; and finally, removing magnetic metal foreign bodies to obtain the battery-grade cobaltosic oxide similar to spheres. The battery-grade cobaltosic oxide has high density and high chemical purity, the grain size is easy to control, grain composition is uniform and narrow in distribution, and the magnetic metal foreign body content is low.

Description

technical field [0001] The invention relates to a method for producing cobaltous oxide, in particular to a method for preparing cobaltous oxide used as a raw material for a positive electrode material of a lithium ion battery. Background technique [0002] Lithium-ion batteries are favored because of their high voltage, high energy density, long cycle life, and low environmental pollution. In recent years, with the further increase in demand for small portable power sources, good opportunities have been created for the development of the lithium-ion battery industry. The rapid development of the lithium-ion battery industry has driven the development of cobalt-based cathode materials such as lithium cobaltate, lithium nickel-cobaltate, and lithium-nickel-cobalt-manganate. Therefore, the demand for cobalt-based cathode materials for lithium-ion batteries has also increased significantly. increase. Cobalt tetroxide is the raw material of lithium ion battery cathode materials...

Claims

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Application Information

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IPC IPC(8): C01G51/04
Inventor 戴振华柏瑞芳丁一东
Owner JIANGSU DONGXIN ENERGY TECH
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