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Method for preparing spherical cobalt hydroxide in the absence of complexing agent

A cobalt hydroxide and complexing agent technology, applied in the direction of cobalt oxide/cobalt hydroxide, etc., can solve the problems of long process, harsh drying conditions, increased consumption of carbonate or bicarbonate, etc., and achieve strong oxidation resistance, The reaction conditions are simple and easy to control, and the effect of easy filtration and washing

Active Publication Date: 2010-04-21
ZHEJIANG HUAYOU COBALT
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

This method has a long process and needs to increase the consumption of carbonate or bicarbonate, and the drying conditions are harsh, which is not conducive to industrial production.
[0007] Although the morphology of cobalt hydroxide can be improved to a certain extent by controlling crystallization through complexation, most of them are flake or irregular block particles, and spherical cobalt hydroxide is rarely reported.
And the addition of complexing agents will also bring some negative effects, such as ammonia water or ammonium salt complexing agents will introduce ammonia nitrogen wastewater problems, which will increase the cost of wastewater treatment; other complexing agents sodium tartrate, disodium edetate, citric acid etc. Due to the strong complexation, the precipitation of some metal cobalt complex ions is not complete, resulting in the loss of cobalt

Method used

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  • Method for preparing spherical cobalt hydroxide in the absence of complexing agent
  • Method for preparing spherical cobalt hydroxide in the absence of complexing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Prepare 10L of cobalt sulfate solution (metal content) with a concentration of 30g / l and 4L of sodium hydroxide solution with a concentration of 120g / l, add 2L of pure water to a reaction kettle with a volume of 20L, heat up to 60°C, and then Add cobalt liquid and sodium hydroxide solution in parallel, maintain the pH value of 6-7 during the feeding process, and obtain a uniformly dispersed blue precipitate; continue to add sodium hydroxide solution until the final pH value is 13.5, add 4g of butyl hydroxy anise Ether solid is used as a protective agent, the reaction time is about 3 hours, after aging for half an hour, it is filtered and washed, and then the filter cake is dried in a flash dryer at 150°C to obtain the product β-Co(OH) 2 .

[0022] The pink cobalt hydroxide that obtains, cobalt content is 62.21% (mass), bulk density is 0.43g / cm 3 . From the SEM image (see figure 1 ) It can be seen that the product is a spherical particle with an average particle diame...

Embodiment 2

[0024] Prepare 2L of cobalt sulfate solution (metal content) with a concentration of 160g / l and 12L of sodium hydroxide solution with a concentration of 40g / l, add 2L of pure water to a reaction kettle with a volume of 20L, heat up to 60°C, and then Add cobalt liquid and sodium hydroxide solution in parallel, maintain the pH value of the feeding process at 5-6, and obtain a uniformly dispersed blue precipitate; continue to add sodium hydroxide solution to the final pH value of 10.5, add 4g of tert-butyl to Hydroquinone solid is used as protective agent, after aging for half an hour, it is filtered and washed, and then the filter cake is dried in a flash dryer at 240°C to obtain the product.

[0025] The obtained pink cobalt hydroxide has a cobalt content of 62.43% and a bulk density of 0.34g / cm 3 . The product is spherical particles with an average particle size of 30 μm.

Embodiment 3

[0027] Prepare 4L of cobalt sulfate solution (metal content) with a concentration of 90g / l and 8L of sodium hydroxide solution with a concentration of 90g / l, add 2L of pure water to a reaction kettle with a volume of 20L, heat up to 60°C, and then Add cobalt liquid and sodium hydroxide solution in parallel flow, maintain the pH value of the feeding process at 5-6, and obtain a uniformly dispersed blue precipitate; continue to add sodium hydroxide solution to the final pH value of 12.6, add 4g of dibutyl hydroxyl The toluene solid is used as a protective agent, after aging, it is filtered and washed, and then the filter cake is adjusted to a slurry with a certain fluidity by adding an appropriate amount of water, and dried at 300°C in a spray dryer to obtain the product.

[0028] The pink cobalt hydroxide has a cobalt content of 62.32% and a bulk density of 0.65g / cm 3 . From the SEM image (see figure 2 ) It can be seen that the product is a spherical particle with an average...

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Abstract

The invention relates to a method for preparing a spherical cobalt hydroxide in the absence of a complexing agent. Though the shape of the cobalt hydroxide can be improved to a certain degree by complexing to control crystallization, the cobalt hydroxide is mostly particles in sheet shape or irregular block shape, and the addition of a complexing agent can cause negative effects. The technical scheme adopted by the invention comprises the following steps of: taking pure water as a base solution; adding a cobalt solution and a sodium hydroxide solution into the base solution with stirring at the same time to cause a precipitation reaction, wherein the pH value of the solution is kept between 5 and 7 in the process of adding the cobalt solution and the sodium hydroxide and is kept between 10.5 and 13.5 in the end of the process; adding an antioxidant into the solution to prevent the solution from being oxidized; and obtaining the cobalt hydroxide product after washing and drying the cobalt hydroxide slurry. The method adopts a forward feeding mode in the absence of complexing agent to form pink spherical cobalt hydroxide powder with very good crystallinity. The spherical cobalt hydroxide powder is easily filtered and washed, and the reaction condition is simple and easy to control. Therefore, the method is suitable for industrial mass production.

Description

technical field [0001] The invention relates to a preparation method of spherical cobalt hydroxide. Background technique [0002] Due to the excellent fluidity of spherical cobalt hydroxide particles and high bulk density, at the same time, because spherical particles have the lowest porosity and relatively small sliding friction coefficient, they have excellent expansion and ductility. When mixed with other materials, the performance Good miscibility, with good processability. [0003] Spherical Co(OH) 2 It is mainly used in the field of lithium-ion batteries (including polymer lithium-ion batteries), and is one of the important raw materials for the preparation of lithium cobalt oxide, a positive electrode material that has been widely used in the production of lithium-ion batteries. It is also used in magnetic materials and electronics industry, and is one of the new cobalt materials. [0004] Cobalt hydroxide is easy to form colloids or flocs during synthesis, which i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
Inventor 刘人生刘秀庆杨仁武向波卿波秦鸣飞田礼平徐伟
Owner ZHEJIANG HUAYOU COBALT
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