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Preparation method of aluminum-doped cobaltosic oxide particles

A technology of cobalt tetroxide particles and aluminum doping, which is applied in the direction of cobalt oxide/cobalt hydroxide, etc., which can solve the problems of poor distribution uniformity of aluminum elements, poor aluminum uniformity, and strict requirements on process parameters, so as to achieve high uniformity and reduce losses , good effect of size controllability

Pending Publication Date: 2022-04-19
JINGMEN GEM NEW MATERIAL
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  • Description
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  • Application Information

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Problems solved by technology

[0003] However, the wet doping method is mainly fed in the form of cobalt and aluminum mixed salt solution, the aluminum element enters the reaction in the form of trivalent cations, and the cobalt element enters the reaction in the form of divalent cations, due to the presence of trivalent aluminum The precipitation rate is higher than that of divalent cobalt. Therefore, the aluminum-doped cobalt carbonate obtained by this process has poor distribution uniformity of aluminum elements, and the requirements for process parameters are strict. Especially when the amount of aluminum is high, the uniformity of aluminum is even worse. The prepared The quality of the obtained aluminum-doped cobalt tetraoxide product is difficult to meet the demand of the market

Method used

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  • Preparation method of aluminum-doped cobaltosic oxide particles
  • Preparation method of aluminum-doped cobaltosic oxide particles
  • Preparation method of aluminum-doped cobaltosic oxide particles

Examples

Experimental program
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Embodiment 1

[0031] (1) preparation Co concentration is the cobalt salt solution of 110g / L;

[0032] (2) Prepare a sodium metaaluminate solution with an Al concentration of 3g / L: measure a certain amount of aluminum sulfate solid and add an appropriate amount of hot water to dissolve it. After the solid is completely dissolved, slowly add a certain amount of liquid caustic soda to keep the liquid caustic and aluminum sulfate The molar ratio is 12:1;

[0033] (3) prepare the ammonium bicarbonate solution of 220g / L;

[0034] (4) Add 25g / L ammonium bicarbonate solution to the 50L reactor until the first layer is stirred, and mix 110g / L cobalt salt solution, 3g / L aluminum salt solution and 220g / L ammonium bicarbonate solution with 2L The flow rate of / h, 1L / h, 4L / h is added to the 50L reactor in parallel. The starting conditions in the reactor are: temperature 42°C, rotation speed 770rpm, clarification process, process pH control of 7.1±0.1, growth rate control of 0.08 -0.1um / h, until the re...

Embodiment 2

[0037] (1) preparation Co concentration is the cobalt salt solution of 130g / L;

[0038] (2) Prepare a sodium metaaluminate solution with an Al concentration of 4g / L: measure a certain amount of aluminum sulfate solid and add an appropriate amount of hot water to dissolve it. After the solid is completely dissolved, slowly add a certain amount of liquid caustic soda to keep the liquid caustic soda and aluminum sulfate The molar ratio is 10:1;

[0039] (3) prepare the ammonium bicarbonate solution of 220g / L;

[0040] (4) Add 10g / L ammonium bicarbonate solution to the 50L reactor until the first layer is stirred, and mix 130g / L cobalt salt solution, 4g / L aluminum salt solution and 220g / L ammonium bicarbonate solution with 3L Flow rates of / h, 1.5L / h, and 7.5L / h are fed into a 50L reactor in parallel. The starting conditions in the reactor are: temperature 50°C, rotation speed 600rpm, clarification process, process pH control of 7.3±0.1, growth rate control 0.08-0.1um / h, until t...

Embodiment 3

[0043] (1) preparation Co concentration is the cobalt salt solution of 130g / L;

[0044] (2) Prepare a sodium metaaluminate solution with an Al concentration of 3g / L: measure a certain amount of aluminum sulfate solid and add an appropriate amount of hot water to dissolve it. After the solid is completely dissolved, slowly add a certain amount of liquid caustic soda to keep the liquid caustic and aluminum sulfate The molar ratio is 18:1;

[0045] (3) prepare the ammonium bicarbonate solution of 210g / L;

[0046] (4) Add 12L of pure water bottom liquid to the 50L reaction kettle to stir in the first layer, mix 130g / L cobalt salt solution, 3g / L aluminum salt solution and 210g / L ammonium bicarbonate solution at 2L / L The flow rates of h, 1L / h, and 4.3L / h are fed into a 50L reactor in parallel. The starting conditions in the reactor are: temperature 60°C, rotation speed 700rpm, clarification process, process pH control of 7.2±0.1, growth rate control of 0.08- 0.1um / h, until the rea...

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Abstract

The invention discloses a preparation method of aluminum-doped cobaltosic oxide particles, which comprises the following steps: firstly, respectively preparing a cobalt salt solution, an ammonium bicarbonate solution and a sodium metaaluminate solution with certain concentrations; then adding the solution into a reaction kettle in which a certain amount of base solution is reserved in advance through a peristaltic pump in a parallel flow manner, reacting, and controlling the reaction temperature to be 35-60 DEG C and the pH value of a reaction system to be 7-7.6; and finally, the obtained product is calcined, the calcination temperature is 200-900 DEG C, the calcination time is 4-15 h, and finally the aluminum-doped cobaltosic oxide particles are obtained. In the method disclosed by the invention, Al enters the reaction kettle in the form of anion AlO2 <->, so that the precipitation rate of aluminum ions in the reaction kettle is slowed down, the uniformity of Al doped in cobaltosic oxide is improved, and the aluminum salt adopts an independent feeding mode, so that the content of aluminum element in cobalt carbonate is better regulated and controlled, the reaction is easier to control, and the reaction yield is improved. Large-particle aluminum-doped uniform cobaltosic oxide can be prepared, and the particle size can reach 14-17 microns.

Description

technical field [0001] The invention relates to the field of preparation of tricobalt tetroxide, in particular to a preparation method of aluminum-doped tricobalt tetroxide particles. Background technique [0002] The rapid development of electronic products has led to an increase in the market demand for large-capacity, high-rate lithium-ion batteries, and lithium cobalt oxide is developing towards high voltages above 4.45V. The charging cut-off voltage of lithium cobalt oxide can be improved by doping elements such as aluminum. At present, there are two main methods of doping aluminum and other metal elements in lithium cobalt oxide: solid phase doping and wet doping. Among them, the solid-phase doping is to mix tricobalt tetroxide, aluminum-doped metal elements, and lithium carbonate, and obtain aluminum-doped lithium cobaltate through high-temperature calcination. The cost of this method is high, and it is easy to cause uneven distribution of aluminum elements in lithiu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/04
CPCC01G51/04C01P2004/03C01P2006/11C01P2004/61
Inventor 许开华唐佳琪刘文泽赵亚强陈颖
Owner JINGMEN GEM NEW MATERIAL
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