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Method and apparatus for preparing large particle size spherical tricobalt tetreoxide

A technology of cobalt tetroxide and large particle size, applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problem of inability to prepare cobalt tetroxide particles

Active Publication Date: 2014-05-07
NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD
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  • Abstract
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Problems solved by technology

[0005] However, since this method is to directly feed the reaction raw materials into the bottom of the reactor, and then continuously stir through the stirring device to generate cobalt tetroxide particles, and the generated cobalt tetroxide particles will rise with the stirring of the stirring tank and finally flow from the discharge port together with the liquid. Outflow, the newly formed cobalt tetroxide at the bottom tends to continue to form smaller cobalt tetroxide particles because there is no attachment body, so this method and device cannot prepare cobalt tetroxide particles above 14 microns

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  • Method and apparatus for preparing large particle size spherical tricobalt tetreoxide

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[0032] The main purpose of the method for preparing large-diameter spherical cobalt tetroxide provided by the embodiment of the present invention is to solve the problem that cobalt trioxide particles with a diameter of 14 microns or more cannot be grown in the current reactor. The method includes:

[0033] Step S1: Prepare mixed solution:

[0034] First, configure the selected cobalt salt into a 60-120g / L cobalt salt solution, and then add a complexing agent to the cobalt salt solution to prepare a mixed solution for use;

[0035] Step S2: Configure the hydroxide solution:

[0036] Configure the selected hydroxide to be a hydroxide solution with a concentration of 8-11mol / L for use;

[0037] Step S3: Feeding:

[0038] The feeding method of the present invention adopts the method of feeding in parallel. Specifically, the above-mentioned configured mixed solution and hydroxide solution and an appropriate amount of air are simultaneously and concurrently flowed into the reacti...

Embodiment 1

[0047] First prepare 60g / L of cobalt chloride solution, add an appropriate amount of glycine to the feed liquid, configure it as a mixed solution, configure sodium hydroxide into an 8mol / L sodium hydroxide solution, mix the mixed solution, sodium hydroxide solution and an appropriate amount of The air flows into the reactor in parallel, and the total flow rate is controlled to be 100L / h, the pH is 10.5, the reaction temperature is 65°C, the stirring speed is 180rpm, and the bulk density of tricobalt tetroxide at the outlet of the reactor is 1.42g / cm 3 , D50=6.77 microns, the three cobalt tetroxide solution at the outlet of the reactor is re-introduced into the reactor with the mixed solution, sodium hydroxide solution and an appropriate amount of air to react, and after a period of time, the particle size of the outlet of the reactor is tested again to be D50 =14.05 microns.

Embodiment 2

[0049] Prepare the cobalt chloride solution of 120g / L, add an appropriate amount of disodium ethylenediaminetetraacetate in the feed liquid, configure it as a mixed solution, configure potassium hydroxide into a potassium hydroxide solution of 11mol / L, mix the solution, hydrogen Potassium oxide solution and an appropriate amount of air flowed into the reactor in parallel, and the total flow rate was controlled to 800L / h, the pH was 8, the reaction temperature was 80°C, and the stirring speed was 100rpm. Sampling and testing of loose cobalt tetroxide at the outlet of the reactor The density is 1.45g / cm 3 , D50=6.83 microns, the three cobalt tetroxide solution at the outlet of the reactor is re-introduced into the reactor with the mixed solution, potassium hydroxide solution and an appropriate amount of air to react, and after a period of time, the particle size of the outlet of the reactor is tested again to be D50 =14.16 microns.

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Abstract

The present invention discloses a method for preparing large particle size spherical tricobalt tetreoxide. The method comprises: preparing a mixed solution, preparing a hydroxide solution, feeding, and preparing tricobalt tetreoxide with a predetermined particle size, wherein the particle size of the tricobalt tetreoxide particles on the material outlet is measured during preparation of the tricobalt tetreoxide with the predetermined particle size, the suspension in the material outlet is re-introduced into the reaction apparatus when the particle size is less than the predetermined production particle size of the tricobalt tetreoxide so as to continuously carry out a reaction until the particle size of the tricobalt tetreoxide particles on the material outlet of the reaction apparatus is not less than the predetermined production particle size, and then the suspension is introduced into the press filter to filter to obtain the spherical tricobalt tetreoxide. With the method, the large particle size battery-grade spherical tricobalt tetreoxide with the diameter of 14 mum and above can be prepared. The present invention further discloses an apparatus for preparing the large particle size spherical tricobalt tetreoxide.

Description

technical field [0001] The invention relates to the technical field of battery material preparation, in particular to a method and a device for preparing large-sized battery-grade spherical cobalt tetroxide. Background technique [0002] Lithium-ion batteries are favored due to their advantages of high voltage, high energy density, long cycle life, and less environmental pollution. opportunity. [0003] The rapid development of the lithium-ion battery industry has driven the development of its cathode materials such as lithium cobaltate and other cobalt-based cathode materials, so the demand for cobalt-based cathode materials for lithium-ion batteries has also increased significantly. Cobalt tetroxide is the raw material of lithium cobalt oxide, the positive electrode material of lithium-ion batteries. Generally speaking, the larger the particle size of lithium cobalt oxide, the higher the voltage of the battery made. Precursors are inherited, so the production of high-vol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
Inventor 戚洪亮沈恒冠陆益展蔡运和
Owner NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD
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