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Preparation method of spherical cobaltosic oxide with high battery security

A high-safety cobalt tetroxide technology, which is applied in cobalt oxide/cobalt hydroxide, electrode manufacturing, battery electrodes, etc., can solve problems such as difficult solid-liquid separation, large metal loss, and poor particle morphology. The effect of uniform distribution and easy control, low content of magnetic foreign matter, and high reactivity

Active Publication Date: 2009-11-25
NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Famous scholars such as Li Yadong reported that Na 2 CO 3 Preparation of Co for precipitant 3 o 4 , the precipitate is difficult to achieve solid-liquid separation, and the impurity Na adsorbed on the colloidal particles + Difficult to wash off; NH 4 HCO 3 As a precipitating agent, the resulting precipitate is basic cobalt carbonate. Although it is easy to separate solid-liquid and wash, it can only be obtained by high-temperature heat treatment. 3 o 4 , high energy consumption and poor particle morphology
Some use NH 4 HCO 3 Prepare basic cobalt carbonate or cobalt carbonate as a precipitant, and then thermally decompose to obtain Co 3 o 4 , the existing problems are that incomplete precipitation causes a large amount of metal loss, a large amount of ammonia-containing wastewater needs to be treated, and the environmental protection issues involved are expected to be resolved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] On the large-scale test line, a 2mol / L cobalt sulfate solution is prepared, a certain amount of disodium edetate is added to the feed liquid, and the cobalt liquid and lye are simultaneously flowed into the reactor to control the intermediate reaction. The pH value is 11, the reaction temperature is 60°C, the total amount of feed liquid is controlled at 500 liters / hour, the stirring speed of the reactor is 180 rpm, and the constant temperature aging is continued for 10 hours after the reaction is completed, then washed, dried and dried. Strong magnetic vibration filter removes magnetic foreign matter. Other processes are carried out as required, continuous production lasts for 10 days, and the bulk density of the obtained spherical cobalt tetraoxide precursor of lithium cobaltate is 1.75g / cm 3 , tap density 2.53g / cm 3 , particle size: D10 = 2.23 microns, D50 = 4.15 microns, D90 = 6.56 microns, magnetic foreign matter content 0.036PPM.

Embodiment 2

[0031] On the large-scale test line, prepare 2mol / L cobalt chloride solution, add a certain amount of disodium ethylenediamine tetraacetate into the feed liquid, and flow cobalt liquid and lye into the reaction kettle at the same time to control the intermediate reaction The PH value is 11, the reaction temperature is 60°C, the total amount of feed liquid is controlled at 350 liters / hour, and the stirring speed of the reactor is 180 rpm. After the reaction, continue to age at a constant temperature for 10 hours, then wash, dry and dry. The magnetic foreign matter is removed by the strong magnetic vibration filter. Other processes are carried out as required, and the continuous production lasts for 10 days. The bulk density of the obtained spherical cobalt trioxide precursor of lithium cobalt oxide is 1.68g / cm 3 , tap density 2.48g / cm 3 , particle size: D10 = 2.42 microns, D50 = 4.35 microns, D90 = 7.02 microns, magnetic foreign matter content 0.028PPM.

Embodiment 3

[0033] On the large-scale test line, prepare a 1.5mol / L cobalt chloride solution, add a certain amount of aminoacetic acid to the feed liquid, and simultaneously flow the cobalt liquid and lye into the reactor, and control the pH value of the intermediate reaction 11.5, the reaction temperature is 50°C, the total amount of feed liquid is controlled at 500 liters / hour, the stirring speed of the reactor is 150 rpm, and after the reaction is completed, continue to age at a constant temperature for 10 hours, then wash, dry and dry, and undergo strong magnetic vibration The filter removes magnetic foreign matter. Other processes are carried out as required, continuous production lasts for 10 days, and the bulk density of the obtained spherical cobalt trioxide precursor of lithium cobalt oxide is 1.25g / cm 3 , tap density 2.52g / cm 3 , particle size: D10 = 2.47 microns, D50 = 4.15 microns, D90 = 6.81 microns, magnetic foreign matter content 0.038PPM.

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Abstract

The invention relates to a preparation method of spherical cobaltosic oxide with high battery security. The point of the method lies in that the spherical cobaltosic oxide powder is obtained by direct oxidization. This powder uses a deironing device to reduce the content of the magnetic foreign substance. The specific steps are as follows: preparing the cobalt salt into the solution with concentration of 1 to 2 mol / L; then adding quantitative complexing agent A; the hydroxide solution being the first and second mixed solutions; simultaneously leading the first and second mixed solutions to a reaction container by means of parallel flow; making the first and second mixed solutions react with each other by strong stirring; strictly controlling pH value, flow, stirring speed and reaction temperature during the reaction process; continuously leading the oxidizing agent with certain flow to the reaction system during the reaction process; after the reaction is finished, aging for 3 to 24 hours in a constant temperature; filter pressing the material by a filter press and the washing the material; then washing the material by the washing kettle and filter pressing, washing it; drying it; filtering the powder by a ferromagnetic filtering device to reduce the content of the magnetic foreign substance; the spherical cobaltosic oxide with high battery security belongs to the battery anode material.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a preparation method of a battery-grade high-safety spherical cobalt trioxide precursor, which is a positive electrode material precursor of lithium ion batteries. Background technique [0002] With the successful development of lithium cobalt oxide, the cathode material of lithium-ion batteries, and the rapid development of its industrialization, and its wide application in various fields such as mobile phones, cameras, notebook computers, and portable appliances, accidents of lithium battery explosions have also occurred frequently. Therefore, higher requirements are put forward for the safety performance of lithium-ion batteries, and battery-grade spherical cobalt tetroxide is used as the main raw material of lithium cobalt oxide, the positive electrode material of lithium-ion batteries, and its physical properties (such as density, particle size, spec...

Claims

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Application Information

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IPC IPC(8): C01G51/04H01M4/04H01M4/58
CPCY02E60/12Y02E60/10
Inventor 沈恒冠袁巧平韩道洋
Owner NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD
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