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Preparation method of spherical alpha-cobalt hydroxide and spherical alpha-cobalt hydroxide

A cobalt hydroxide, spherical technology, applied in the direction of cobalt oxide/cobalt hydroxide, electrochemical generators, structural parts, etc., can solve the problems of complex preparation process, increased cobalt loss, increased cost, etc., to avoid excessive OH- , Low Co loss effect

Pending Publication Date: 2021-04-09
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the mother liquor is red after the reaction, indicating that some cobalt salts have not reacted, which increases the loss of cobalt; in order to prepare a relatively stable α-Co(OH) 2 Scholars at home and abroad have also adopted the doping method, which replaces the cobalt in the cobalt hydroxide lattice with other metals. The essence is to use some metals with stable properties to strengthen the crystal form of cobalt, but the preparation process Relatively complicated and will further increase the cost
Therefore, there is a lack of simple, efficient and low-cost preparation of stable α-Co(OH) in the prior art 2 Methods

Method used

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  • Preparation method of spherical alpha-cobalt hydroxide and spherical alpha-cobalt hydroxide
  • Preparation method of spherical alpha-cobalt hydroxide and spherical alpha-cobalt hydroxide
  • Preparation method of spherical alpha-cobalt hydroxide and spherical alpha-cobalt hydroxide

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Embodiment 1

[0039] The present invention provides α-Co(OH) 2 The preparation method comprises the following steps:

[0040] (1) Take soluble cobalt chloride and dissolve in water to obtain soluble cobalt chloride solution.

[0041](2) Add a mixed solution of triethylamine and tripropylamine to the clarified solution of soluble cobalt salt, the molar ratio of triethylamine and tripropylamine in the mixed solution is 40:60, control the reaction temperature to 65°C, and the stirring rate to 480r / min, after the reaction is over, the solid-liquid separation will give blue-cyan α-Co(OH) 2 Solid and organic amine salt solutions;

[0042] 3) Add quicklime to the organic amine salt solution, react to generate calcium chloride and organic amine liquid, and finally obtain a mixed solution containing calcium chloride and organic amine, and then separate and recover the organic amine in the mixed solution for step 2).

Embodiment 2

[0044] (1) Weigh soluble cobalt nitrate and dissolve in water to obtain soluble cobalt nitrate solution.

[0045] (2) Add the mixed solution of tripropylamine and tributylamine in the cobalt nitrate solution, the molar ratio of triethylamine and tripropylamine in the mixed solution is 20:80, control the reaction temperature to be 55°C, and the stirring rate to be 560r / min, After the reaction is completed, the solid-liquid separation will give blue-cyan α-Co(OH) 2 Solid and organic amine salt solutions;

[0046] 3) adding calcium hydroxide to the organic amine salt solution to react to obtain a mixed solution containing calcium nitrate and organic amine, and then separating and recovering the organic amine in the mixed solution for step 2).

Embodiment 3

[0048] (1) Weigh soluble cobalt nitrate and dissolve in water to obtain soluble cobalt nitrate solution.

[0049] (2) Add tributylamine solution to the cobalt nitrate solution, control the reaction temperature to 60°C, and the stirring rate to 550r / min. After the reaction is completed, the solid-liquid separation will give blue cyan α-Co(OH) 2 Solid and organic amine salt solutions;

[0050] 3) adding calcium hydroxide to the organic amine salt solution to react to obtain a mixed solution containing calcium nitrate and organic amine, and then separating and recovering the organic amine in the mixed solution for step 2).

[0051] To the α-Co(OH) that embodiment 1 prepares 2 Solid carries out XRD and analysis, the result is as follows figure 1 as shown, figure 1 There are obvious diffraction peaks in , and each diffraction peak is related to α-Co(OH) 2 Consistent with standard cards, no β-Co(OH) 2 Miscellaneous peak; Prepare α-Co(OH) to embodiment 1, embodiment 2, embodimen...

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Abstract

The invention relates to a preparation method of spherical alpha-cobalt hydroxide and spherical alpha-cobalt hydroxide. The preparation method comprises the following steps: adding organic amine into a cobalt salt solution, conducting stirring for reaction at the temperature of 50-70 DEG C, and carrying out solid-liquid separation to obtain a spherical alpha-Co(OH)2 solid and an organic amine salt solution after the reaction is finished, wherein the organic amine is selected from one or a combination of more of liquid organic amines slightly soluble in water; and adding inorganic base into the organic amine salt solution, conducting reacting to obtain a mixed solution containing the inorganic salt and organic amine, separating liquid to recover the organic amine in the mixed solution, and applying the organic amine to the step 1). Based on the method provided by the invention, not only can relatively stable spherical alpha-Co(OH)2 be prepared, but also the organic amine is used as a precipitator in the preparation process, additional metal ions or complexing agents are not required to be added, the raw material components are simple, the cost is low, the organic amine can be recycled, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of cobalt hydroxide, and in particular relates to a preparation method of spherical α-cobalt hydroxide and spherical α-cobalt hydroxide. Background technique [0002] Lithium cobaltate is currently one of the cathode materials for large-scale industrialization. Although the technology is very mature and stable, there is still a lot of room for improvement in its comprehensive performance. One of the directions is the research on high tap density spherical cathode materials. As we all know, the spherical positive electrode material not only has a high tap density, but also is very conducive to the coating of the electrode sheet due to its excellent fluidity and processing properties, so it has become an improvement direction for lithium cobalt oxide positive electrode materials. Lithium cobaltate on the market is prepared by solid-state sintering method, which uses lithium salt and cobalt oxide to calcinate. ...

Claims

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Application Information

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IPC IPC(8): C01G51/04H01M4/525H01M10/0525
CPCC01G51/04H01M4/525H01M10/0525C01P2002/72C01P2004/03C01P2004/61C01P2004/32Y02E60/10
Inventor 张勇罗喆韩培林桑子容陈喆
Owner WUHAN INSTITUTE OF TECHNOLOGY
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