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Method for preparing cobaltosic oxide with large grain size and high safety

A technology of cobalt tetroxide and large grain size, applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of poor electrochemical performance of the battery, difficult to obtain industrial application, complicated process, etc., and achieves low cost and large grain size. , the effect of simple process

Inactive Publication Date: 2011-03-02
JIANGSU DONGXIN ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some of the methods that have been reported are complex in process, or consume a lot of energy, and are difficult to be applied industrially; or have the disadvantages of poor electrochemical performance of the battery.

Method used

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  • Method for preparing cobaltosic oxide with large grain size and high safety
  • Method for preparing cobaltosic oxide with large grain size and high safety
  • Method for preparing cobaltosic oxide with large grain size and high safety

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] With deionized water, industrial-grade cobalt sulfate is prepared into a solution with a cobalt concentration of 70g / L, ammonium bicarbonate is made into a precipitant solution with a concentration of 120g / L, and the cobalt solution and the precipitant solution are in molar ratio, cobalt : precipitating agent=1.0: 3.0, add reaction vessel with co-current feeding method, control feeding speed is 15ml / min, the synthetic reaction temperature is 60 ℃, and reaction pH value is 7.3, and stirring speed is 400rpm, makes precursor, will The precursor was washed with deionized water at 80°C and then dehydrated. The water content of the filter cake was 25%. At room temperature, after crushing and grading, metal foreign matter is removed by an iron remover to obtain a spherical cobalt tetraoxide powder, D 10 : 2.26 μm, D 50 : 8.16 μm, D 97 : 12.45μm, TD: 2.98g / cm 3 , and its SEM image is figure 1 shown.

Embodiment 2

[0035]With deionized water, the cobalt nitrate of technical grade is mixed with the solution that cobalt concentration is 80g / L, and sodium carbonate is made into the precipitant solution that concentration is 100g / L, with cobalt solution and precipitant solution in molar ratio, cobalt: Precipitating agent=1.0:3.1, add the reaction vessel with co-current feeding method, control the feeding speed to be 12ml / min, the synthetic reaction temperature is 80°C, the reaction pH value is 8.5, and the stirring speed is 500rpm to prepare the precursor. The body is washed with deionized water at 90°C and then dehydrated. The water content of the filter cake is 24%. It is directly loaded into a bowl, sent to a roasting furnace for 9 hours at 300°C to 950°C, cooled naturally to below 400°C, and then cooled to room temperature. After pulverization and classification, metal foreign matter is removed by iron remover to obtain spherical cobalt tetraoxide powder, D 10 : 3.55 μm, D 50 : 10.90 μm...

Embodiment 3

[0037] With deionized water, industrial-grade cobalt chloride is formulated into a solution with a cobalt concentration of 90g / L, ammonium carbonate is made into a precipitant solution with a concentration of 100g / L, and the cobalt solution and the precipitant solution are in molar ratio, cobalt : precipitating agent=1.0: 3.8, add reaction vessel with co-current feeding method, control feeding speed is 8ml / min, the synthetic reaction temperature is 100 ℃, and reaction pH value is 9.0, and stirring speed is 800rpm, makes precursor, will The precursor is washed with deionized water at 100°C and then dehydrated. The water content of the filter cake is 24%. Put it in a bowl directly, send it to a roasting furnace for 10 hours at 300°C to 1000°C, cool it naturally to below 400°C, and then cool it down to room temperature. , after crushing and grading, metal foreign matter is removed by iron remover to obtain spherical cobalt tetraoxide powder, D 10 : 3.16 μm, D 50 : 13.59 μm, D 9...

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Abstract

The invention provides a method for preparing cobaltosic oxide with large grain size and high safety, comprising the following steps: preparing the raw material cobalt and a precipitant into cobalt solution and precipitant solution with deionized water, adding the cobalt solution and the precipitant solution which are prepared to certain concentration to a reaction vessel by the charging methods including cocurrent charging according to certain molar ratio, preparing the cobalt salt precursor by controlling the reaction temperature, charging speed, PH value and stirring speed, washing and dehydrating the precursor, directly putting the water-containing filter cake into a pot, spheroidizing and calcining the pot at high temperature, carrying out mechanical grinding, grading and activating, controlling the grain size and the crystal morphology and finally removing the magnetic metal foreign bodies, thus finally obtaining the high quality battery grade cobaltosic oxide. The method is simple in process, easy to operate, low in cost, energy-saving, environment-friendly and suitable for industrial production. The prepared cobaltosic oxide looks like spheroid and has large grain size, good powder flowability and uniform granularity.

Description

technical field [0001] The invention relates to a preparation method of tricobalt tetroxide, in particular to a preparation method of tricobalt tetroxide for lithium ion batteries. The invention belongs to the technical field of inorganic chemical industry and secondary rechargeable battery material. 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 growth of demand for small portable power sources, good opportunities have been created for the development of the lithium-ion battery industry. With the development of cobalt-based cathode materials, the demand for cobalt-based cathode materials for lithium-ion batteries has also increased significantly. Among them, the consumption form of cobalt is to prepare cobalt-based cathode materials based on tricobalt tetroxide. The microstructural factors such as grain size, particle siz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
Inventor 戴振华柏瑞芳丁一东
Owner JIANGSU DONGXIN ENERGY TECH
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