Preparation method of regular octahedron-type cobaltosic oxide

A technology of tricobalt tetroxide and regular octahedron, which is applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of high energy consumption, volatile, safety hazards, etc., and achieve low energy consumption, smooth reaction, and small safety hazards.

Inactive Publication Date: 2014-08-06
NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD
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Problems solved by technology

[0004] At present, the high-performance cobalt tetroxide produced by foreign advanced technology has the shape of octahedron or polyhedron, but not the spherical cobalt tetroxide prepared by many domestic manufacturers. The preparation process generally adopted abroad is the spray pyrolysis method, but the required The equipment investment is very large, and at the same time, the energy consumption caused by roasting is also very large, which is still difficult to achieve in China at present
[0005] The Chinese patent whose publication number is CN102134104A discloses a method of "preparing ultrafine octahedron tricobalt tetroxide by cobalt salt precipitation microwave-induced pyrolysis", and the Chinese patent whose publication number is CN102491431A discloses a method of "preparing cobalt trioxide octahedron by microwave one-step method". method", but it is difficult to realize industrial production by microwave induction method, and it consumes a lot of energy and has radiation pollution, and the base liquid currently used is ethanol, volatile or flammable organic matter, and microwave induction method is also used to prepare octahedral cobalt trioxide. There is a great security risk

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preparation example Construction

[0026] The preparation method of octahedral cobalt tetroxide provided by the present invention mainly solves the disadvantages that the current preparation cost of regular octahedral cobalt tetroxide is relatively high, and the safety hazards in the preparation process are relatively large. For this reason, the preparation method provided by the present invention includes the following steps:

[0027] S1) Prepare the mixed solution:

[0028] The cobalt salt is prepared into a uniform cobalt salt solution, and the concentration of cobalt ions in the cobalt salt solution is maintained within the range of 1.0-2.0mol / L, and then a complexing agent is added to the prepared cobalt salt solution to prepare a mixed solution to be prepared. use;

[0029] S2) Preparation of hydroxide solution:

[0030] The prepared hydroxide is prepared as a hydroxide solution for use, and the concentration of hydroxide in the hydroxide solution is preferably 5.0-10.0mol / L;

[0031] The solvent in ste...

Embodiment 1

[0047] Cobalt chloride is formulated as a cobalt salt solution, and the molar concentration of cobalt ions in the solution is 1.5mol / L, and glycine is added as a complexing agent, and the molar concentration of glycine is 0.003mol / L (that is, 0.2% of the concentration of cobalt ions). %), at this time the preparation of the mixed solution is completed; the sodium hydroxide is prepared into a 9.0mol / L lye, and then the mixed solution and the lye are mixed and flowed into the reactor at a flow rate of 200L / h, and the The pH in the reaction kettle is controlled at 10.0, the reaction temperature is controlled at 65°C, and the stirring speed is controlled at 300rpm. After 8 hours of stirring reaction, the suspension is passed into an aging kettle with a temperature of 50°C for 3 hours of aging , and then press-filter the aged suspension to obtain cobaltous hydroxide, wash the cobaltous hydroxide three times with deionized water, and then enter the drying furnace to dry to obtain dry...

Embodiment 2

[0049] Cobalt sulfate is formulated as a cobalt salt solution with a cobalt ion molar concentration of 1.0mol / L, and histidine is added as a complexing agent, and the molar concentration of histidine is 0.005mol / L (that is, 0.5% of the cobalt ion concentration ), the preparation of the mixed solution is completed at this time; the potassium hydroxide is prepared into a lye with a concentration of 7.0mol / L, and the mixed solution and lye are passed into the reactor at a flow rate of 300L / h in parallel, and the reaction The pH in the kettle is controlled at 9.0, the reaction temperature is controlled at 45°C, and the stirring speed is controlled at 380rpm. After 16 hours of stirring reaction, the suspension in the reaction kettle is passed into an aging kettle at 70°C for 3 hours of aging. and then press-filter the aged suspension to obtain cobaltous hydroxide, wash the cobaltous hydroxide with deionized water for four times, and then dry it in a drying furnace to obtain dry coba...

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Abstract

The invention discloses a preparation method of regular octahedron-type cobaltosic oxide. The preparation method comprises the following steps of 1, mixing a cobalt salt solution having a cobalt ion concentration of 1.0-2.0mol/L and a complexing agent to obtain a mixed solution, 2, preparing a hydroxide solution having a hydroxyl concentration of 5.0-10.0mol/L from a hydroxide, 3, merging the mixed solution and the hydroxide solution, feeding the mixture into a reactor and preparing a cobalt hydroxide suspension liquid, 4, filtering the cobalt hydroxide suspension liquid, washing the filter residue and carrying out drying, and 5, calcining the dried hydroxide solids in a calcining furnace to obtain the regular octahedron-type cobaltosic oxide. The preparation method avoids microwave radiation pollution, comprises a mild liquid phase reaction in a preparation early stage and a calcining oxidation reaction in a preparation later stage, has high safety in the whole preparation process, has low energy consumption, and realizes easy enlargement of the reactor. Therefore, the preparation method easily realizes industrialization.

Description

technical field [0001] The invention relates to the technical field of chemical industry and material preparation, in particular to a preparation method of regular octahedron tricobalt tetroxide. Background technique [0002] The appearance of tricobalt tetroxide is black or black powder. It is mainly used in the fields of catalysts, electrochemistry, high temperature and corrosion resistance, and magnetic materials. In the field of catalysts, tricobalt tetroxide is mainly used in oxidation reactions. In the field of solid-liquid electrochemistry, it is mainly used in Activate metal electrodes. [0003] With the rapid development of the lithium-ion battery industry, it has driven the rapid development of its positive electrode material, lithium cobalt oxide, and the main raw material for the preparation of lithium cobalt oxide is tricobalt tetroxide. have an important impact. [0004] At present, the high-performance cobalt tetroxide produced by foreign advanced technology...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
Inventor 朱珠沈恒冠蔡运和陆益展
Owner NINGBO RONBAY LITHIUM BATTERY MATERIAL CO LTD
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