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Method for preparing cobaltic-cobaltous oxide powder with octahedron shape

A technology of tricobalt tetroxide powder and octahedron, which is applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of wide particle size distribution and the inability to meet the production of high-quality lithium cobaltate products, and achieve complete crystallization, improved washing efficiency, and prevention of hydrolysis. Effect

Active Publication Date: 2008-10-29
GRIPM ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most cobalt tetroxide powders produced by this process are irregular in shape or other spherical or quasi-spherical, and the particle size distribution is wide, which cannot meet the production of high-quality lithium cobalt oxide products.

Method used

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  • Method for preparing cobaltic-cobaltous oxide powder with octahedron shape
  • Method for preparing cobaltic-cobaltous oxide powder with octahedron shape
  • Method for preparing cobaltic-cobaltous oxide powder with octahedron shape

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preparation example Construction

[0026] The preparation method of the present invention is to add soluble cobalt salt solutions such as cobalt chloride, cobalt acetate or cobalt nitrate and ammonium bicarbonate or ammonium carbonate solution into the reactor at a certain speed, stir vigorously at the same time, and strictly control the reaction temperature and The pH value is within a certain range to control the crystallization process. The obtained cobalt carbonate precursor is washed, filtered, dried at a certain temperature, and then calcined at a certain temperature to obtain the final octahedral cobalt tetroxide powder. The process flow diagram of the present invention is as figure 1 As shown, the specific steps are:

[0027] Preparation of solution

[0028] a preparation of soluble cobalt salt solution

[0029] Soluble cobalt salts such as cobalt chloride, cobalt acetate or cobalt nitrate are used as raw materials, dissolved in deionized water to form an aqueous solution with a cobalt ion concentrat...

Embodiment 1

[0039]Prepare 10L of cobalt chloride solution with a cobalt ion concentration of 2mol / L, and 20L of ammonium bicarbonate solution with a concentration of 2mol / L. First add 2L of deionized water to a reactor with a volume of 50L, heat it to 40°C, and add the above solution into the reactor at the same time under the stirring condition of 200-2000r / min, and the cobalt salt solution is added at a speed of 20L / h 1. The ammonium bicarbonate solution was added at a rate of 40L / h, the reaction temperature was 40°C, and the pH value was controlled at 6.7. After the addition was completed, the reaction was continued for 30 minutes, aged at 40°C for 4 hours, and the cobalt carbonate precursor was suction filtered or pressed. filter, and wash the precipitate by suction filtration or pressure filtration, spin dry after washing, dry at 100°C for 8 hours, and finally calcinate at 600°C for 2 hours. The finally obtained cobalt tetroxide powder has a median diameter (D50) of 2.2 μm and a bulk...

Embodiment 2

[0041] Prepare 20 L of cobalt chloride solution with a cobalt ion concentration of 0.5 mol / L, and 20 L of ammonium bicarbonate solution with a concentration of 1 mol / L. First add 2L of deionized water to a reactor with a volume of 50L, heat it to 80°C, and add the above solution into the reactor at the same time under the stirring condition of 200-2000r / min, and the cobalt salt solution is added at a rate of 100L / h 1. The ammonium bicarbonate solution was added at a rate of 100L / h, the reaction temperature was 80°C, and the pH value was controlled at 6.5. After the addition was completed, the reaction was continued for 60 minutes, aged at 60°C for 4 hours, and the cobalt carbonate precursor was suction filtered or pressed. filter, and wash the precipitate by suction filtration or pressure filtration, spin dry after washing, dry at 110°C for 10 hours, and finally calcinate at 500°C for 2 hours. The finally obtained cobalt tetroxide powder, under the S4800 type field emission sc...

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Abstract

The invention provides a preparation method of an electronic grade cobaltosic oxide powder which is shaped like an octahedron.The cobaltosic oxide powder has the complete appearance of the octahedron, the middle diameter (D50) of the powder is 0.5 to 5 Mum (the value can be adjusted by changing process parameters), the apparent density is more than 0.7g / cm<3>, and the tap density is more than 2.0g / cm<3>. The technological process is characterized in that the soluble cobalt salt solution, such as cobalt chloride and cobalt acetate, and ammonium bicarbonate solution are strongly stirred when being added to a reactor in the form of cocurrent flow at a definite speed, and the reaction temperature and PH value are strictly controlled, so the crystallization process is controlled. The obtained cobalt carbonate sediment is dried at a certain temperature after washing and filtration, and finally calcined at a certain temperature to get the ultimate cobaltosic oxide powder in the shape of an octahedron. The preparation method has the advantages that the cobaltosic oxide powder with the complete crystal form and in the form of the octahedron is prepared at atmospheric pressure, the specific surface area is high and the activity is high, etc., and besides the technique is simple, reliable and easy to industrialize.

Description

technical field [0001] The invention relates to a method for preparing cobalt trioxide powder with an octahedral shape, which is a key raw material of lithium cobalt oxide, a positive electrode material of a lithium ion secondary battery, and is also used in catalysts, magnetic materials, and the like. The invention belongs to the field of chemical industry and material preparation. Background technique [0002] The appearance of cobalt tetroxide is gray black or black powder, the theoretical cobalt content is 73.43%, the oxygen content is 26.57%, and the crystals are cubic crystals with normal spinel structure. of which CO 3+ Occupying the octahedral position, it has high crystal field stabilization energy. The lattice constant is 8.1A, and the specific gravity is 6.0-6.2g / cm 3 . [0003] Cobalt tetroxide is mainly used in the fields of catalyst, electrochemistry, high temperature resistance and corrosion resistance, and magnetic materials. Cobalt tetroxide is an effic...

Claims

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Application Information

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IPC IPC(8): C01G51/04
Inventor 刘宇慧汪礼敏张景怀申思闫世凯庞鹏沙
Owner GRIPM ADVANCED MATERIALS CO LTD
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