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A kind of liquid phase synthesis prepares the production method of pure phase cobalt tetroxide

A technology of cobalt tetroxide and liquid phase synthesis, which is applied in chemical methods, chemical instruments and methods, cobalt oxide/cobalt hydroxide and other directions for reacting liquid and gas medium, and can solve the problem of long process flow, reduced product activity and high energy consumption. problems, to achieve the effect of simple process flow and reduced energy consumption

Active Publication Date: 2017-03-15
GEM JIANGSU COBALT IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High vibration, high activity, and pure phase cobalt tetroxide are necessary conditions for the production of high-quality lithium cobalt oxide; currently, cobalt tetroxide on the market is mainly produced by cobalt salt and ammonium carbonate or lye liquid-phase synthesis to produce intermediate products, and then prepared by high-temperature sintering and crushing Cobalt tetroxide has disadvantages such as long process flow, high energy consumption, and high temperature sintering to reduce product activity.
The existing patent No. 200910099751.2 is a battery-grade high-safety spherical cobalt tetroxide preparation method. Cobalt salt solution and sodium hydroxide are used to flow through the reactor, and the oxidant is oxidized to prepare cobalt tetroxide. The cobalt salt solution and sodium hydroxide are first reacted to form hydroxide Cobalt will form a precipitate before the oxidant is passed through. Even if the oxidant passed through can oxidize part of the precipitated surface layer, most of the reaction product is still cobalt hydroxide, which cannot directly prepare cobalt tetroxide, which does not meet the production requirements.

Method used

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  • A kind of liquid phase synthesis prepares the production method of pure phase cobalt tetroxide

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Effect test

Embodiment 1

[0016] The method for preparing pure phase cobalt tetroxide by liquid phase synthesis of the present invention comprises the following steps:

[0017] a. Deep degreasing treatment of cobalt chloride solution, adding ethylenediaminetetraacetic acid in proportion to prepare cobalt solution, the cobalt content of cobalt solution is 130g / L, and ethylenediaminetetraacetic acid is added according to 3% of the weight of cobalt metal;

[0018] b. Cobalt solution, lye and air are passed through the cobalt liquid feed pipe, lye feed pipe and air feed pipe respectively to react in the reactor, the concentration of lye is 10mol / L, and the temperature is controlled at 70°C during the reaction , the pH value is between 10, the cobalt chloride flow rate is 280L / h, the lye flow rate is adjusted according to the pH value, and the air flow rate is 18m 3 / h, continuous reaction;

[0019] c. Monitor the oxidation of cobalt chloride in real time. When the oxidation is insufficient, shorten the si...

Embodiment 2

[0022] The method for preparing pure phase cobalt tetroxide by liquid phase synthesis of the present invention comprises the following steps:

[0023] a. Deep degreasing treatment of cobalt chloride solution, adding ethylenediaminetetraacetic acid in proportion to prepare cobalt solution, the cobalt content of cobalt solution is 135g / L, and ethylenediaminetetraacetic acid is added according to 4.0% of the weight of cobalt metal;

[0024] b. Cobalt solution, lye and air are passed through the cobalt liquid feed pipe, lye feed pipe and air feed pipe respectively to react in the reactor, the concentration of lye is 11mol / L, and the temperature is controlled at 80°C during the reaction , the pH value is between 10.4, the cobalt chloride flow rate is 300L / h, the lye flow rate is adjusted according to the pH value, and the air flow rate is 21m 3 / h, continuous reaction;

[0025] c. Monitor the oxidation of cobalt chloride in real time. When the oxidation is insufficient, shorten th...

Embodiment 3

[0028] The method for preparing pure phase cobalt tetroxide by liquid phase synthesis of the present invention comprises the following steps:

[0029] a. Deep degreasing treatment of cobalt chloride solution, adding ethylenediaminetetraacetic acid in proportion to prepare cobalt solution, the cobalt content of cobalt solution is 125g / L, and ethylenediaminetetraacetic acid is added according to 1.0% of the weight of cobalt metal;

[0030] b. Cobalt solution, lye and air are passed through the cobalt liquid feed pipe, lye feed pipe and air feed pipe respectively to react in the reactor, the concentration of lye is 9mol / L, and the temperature is controlled at 60°C during the reaction , the pH value is between 9.7, the cobalt chloride flow rate is 220L / h, the lye flow rate is adjusted according to the pH value, and the air flow rate is 15m 3 / h, continuous reaction;

[0031] c. Monitor the oxidation of cobalt chloride in real time. When the oxidation is insufficient, shorten the ...

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Abstract

The present invention relates to a production method for liquid-phase synthesis preparation of pure-phase tricobalt tetraoxide. According to the production method, a reaction kettle is used, an oxidant feeding pipe, a cobalt liquid feeding pipe and an alkali liquid feeding pipe are parallel to the axis line of the reaction kettle body, have the adjustable height in a vertical direction, extend into the reaction kettle body, and are 5-50 cm far away from the inner wall of the reaction kettle body, the lower pipe opening of the cobalt liquid feeding pipe and the lower pipe opening of the alkali liquid feeding pipe are higher than the lower pipe opening of the oxidant feeding pipe, the plane formed by the lower pipe openings of the oxidant feeding pipe, the cobalt liquid feeding pipe and the alkali liquid feeding pipe and the horizontal plane form an included angle of 0-60 DEG, and the height of a stirring paddle is positioned between the horizontal plane of the highest pipe opening and the horizontal plane of the lowest pipe opening of the oxidant feeding pipe, the cobalt liquid feeding pipe and the alkali liquid feeding pipe. According to the present invention, the process is simple, the operation is convenient, and the generated product is changed along with the change of the reaction rate during the tricobalt tetraoxide production process so as to obtain the pure-phase tricobalt tetraoxide.

Description

technical field [0001] The invention relates to a production method applied to tricobalt tetroxide, in particular to a method for liquid-phase preparation of pure-phase cobalt tetraoxide. Background technique [0002] As a first-generation battery system, lithium-ion batteries have the characteristics of high specific energy, high specific power, no memory, and low self-discharge rate. They are ideal power sources for high-tech applications such as mobile electronic devices, electric vehicles, and national defense industries. In recent years, with the rapid development of communications and transportation, the market demand for lithium cobaltate, which is the cathode material for lithium batteries, is increasing, and the market demand for cobalt tetroxide, as the key raw material for lithium cobaltate, is also increasing rapidly. High vibration, high activity, and pure phase cobalt tetroxide are necessary conditions for the production of high-quality lithium cobalt oxide; cu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/18B01J10/00C01G51/04
Inventor 袁国和袁邦耀叶圣毅王琴
Owner GEM JIANGSU COBALT IND CO LTD
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