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Spherical cobaltosic oxide and preparation method thereof

A technology of cobalt tetroxide and spherical shape, applied in the field of spherical cobalt tetroxide and its preparation, can solve the problems of difficult removal of cobalt hydroxide impurity content, small particles, poor particle size distribution, etc., and achieves low alkaline impurity content, uniform particle size distribution, and acceptable particle size. control effect

Active Publication Date: 2013-10-23
BEIJING EASPRING MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The cobalt oxide wet synthesis process mainly includes cobalt carbonate process and cobalt hydroxide process: according to the cobalt carbonate process disclosed in the patent application publication CN1376638A, cobalt carbonate is synthesized in liquid phase, and cobalt oxide is obtained by high-temperature calcination, and then reacted with lithium source. Low yield, difficult crushing, poor particle size distribution, small particles and difficult to enlarge, low density, cannot meet the requirements of high-end lithium cobalt oxide
According to the patent application publication documents CN101857277A, CN101434416A, and CN101279771A, the cobalt hydroxide process is a liquid phase synthesis of cobalt hydroxide, which directly reacts with the lithium source. The particle size and particle size distribution of this process are controllable, the density is high, and the calcination temperature is low , without strong crushing, but this process needs to add a complexing agent, usually an ammonia system, the discharge of waste water and gas is a serious problem, causing pollution to the environment, and the impurity content in cobalt hydroxide is difficult to remove

Method used

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  • Spherical cobaltosic oxide and preparation method thereof
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Experimental program
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Effect test

Embodiment 1

[0022] Prepare 4 mol / L cobalt sulfate solution, 8 mol / L sodium hydroxide solution and 8 mol / L hydrogen peroxide solution, and put the three solutions into the stirred reactor at the same time, and control the moles of salt: hydrogen peroxide: sodium hydroxide The ratio is 1:1:2, the liquid addition speed is controlled so that the pH value of the reaction is 8, the reaction temperature is controlled at 60°C, and the reacted slurry naturally overflows into another kettle for aging, centrifuged, washed and filtered, and then placed in Calcined at 500°C for 8h to obtain the diameter D 50 =15.51um, bulk density 1.64g / cm 3 of cobalt tetroxide.

Embodiment 2

[0024] Prepare 5mol / L cobalt chloride salt solution, 6mol / L sodium hydroxide solution and 7mol / L hydrogen peroxide solution, and add the three solutions into the stirred reactor at the same time, and control the salt: hydrogen peroxide: sodium hydroxide The molar ratio is 1:1:2, the liquid addition speed is controlled so that the pH value of the reaction is 9.5, the reaction temperature is controlled at 50°C, the reacted slurry naturally overflows into another kettle for aging, centrifuged, washed and filtered, and then Calcined at 600°C for 6h to obtain the diameter D 50 =12.50um, bulk density 1.57g / cm 3 of cobalt tetroxide.

Embodiment 3

[0026] Prepare 2mol / L cobalt sulfate solution, 5mol / L sodium hydroxide solution and 6mol / L sodium hypochlorite solution, and add the three solutions into the stirred reactor at the same time, and control the salt: hydrogen peroxide: the mole of sodium hydroxide The ratio is 1:1:2, the liquid addition speed is controlled so that the pH value of the reaction is 10.1, the reaction temperature is controlled at 65°C, the reacted slurry naturally overflows into another kettle for aging, centrifuged, washed and filtered, and then in Calcined at 500°C for 8h to obtain the diameter D 50 =10.89um, bulk density 1.57g / cm 3 of cobalt tetroxide.

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Abstract

The invention discloses spherical cobaltosic oxide and a preparation method thereof. Salt, a precipitator and an oxidant are adopted in a liquid-phase synthesis process; the salt, the precipitator and the oxidant simultaneously flow inside a reaction kettle to react; and the spherical cobaltosic oxide is continuously prepared by adopting the methods of ageing, centrifuging, washing, secondary centrifuging and burning. The particle size is controllable; D50 is 2-20 microns; the spherical cobaltosic oxide is even in distribution of particle size, high in compactness, high in product consistency, and simple in preparation method; a complexing agent does not need to be added; and no harmful substance is discharged in the process, so that the preparation method is safe and friendly.

Description

technical field [0001] The invention belongs to the technical field of positive electrode materials of lithium ion batteries, and in particular relates to a spherical tricobalt tetroxide and a preparation method thereof. Background technique [0002] With the rapid development of high-end electronic products such as smartphones and tablet computers, the requirements for lithium batteries will become higher and higher. Larger capacity and longer standby time are the inevitable development direction. In this broad high-end market field, High-density lithium cobalt oxide accounts for more than 90% of the share. [0003] High-density lithium cobalt oxide is prepared from cobalt oxide. Since the performance of the raw material cobalt oxide has a great influence on the lithium cobalt oxide material, there are strict physical and chemical index requirements for the preparation of cobalt oxide. At present, the common preparation methods of cobalt oxide include wet method and dry m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
Inventor 宋顺林王汝娜刘亚飞陈彦彬汤贺军
Owner BEIJING EASPRING MATERIAL TECH CO LTD
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