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Preparation method of homogeneous-phase aluminum-doped small-particle-size cobaltosic oxide

A technology of cobalt tetroxide and small particle size, applied in cobalt oxide/cobalt hydroxide, electrochemical generators, structural parts, etc., can solve the problems of incomplete precipitation of Co metal ions, increased wastewater treatment costs, and general uniformity of aluminum doping.

Active Publication Date: 2021-02-12
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical route of carbonate has the following disadvantages: 1. Ammonium bicarbonate is used as precipitant, which is unstable and easy to decompose to produce ammonia gas, which affects the environment; Co complexed to a certain extent 2+ , leading to incomplete precipitation of Co metal ions, increased concentration of metal ions in wastewater, increased wastewater treatment costs, and a certain pressure on the environment; 3. The uniformity of aluminum doping in carbonate systems is general, especially when the amount of aluminum is high. Poor sex

Method used

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  • Preparation method of homogeneous-phase aluminum-doped small-particle-size cobaltosic oxide
  • Preparation method of homogeneous-phase aluminum-doped small-particle-size cobaltosic oxide
  • Preparation method of homogeneous-phase aluminum-doped small-particle-size cobaltosic oxide

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Embodiment 1

[0030] ①Prepare 110g / L cobalt sulfate solution, and add 2.713kg aluminum sulfate octadecahydrate and 0.11kg isopropanol and glycine mixed compound complexing agent to each cobalt solution, and stir evenly;

[0031] ② Add an appropriate amount of deionized water to the reaction vessel as the bottom liquid, adjust the pH of the bottom liquid to 11.0 with sodium hydroxide, and feed compressed air with an air flow rate of 0.7m 3 / h, the temperature is 68°C, under the stirring speed of 400rpm, the prepared cobalt-aluminum mixed solution and 80g / L sodium hydroxide solution are added to the reaction vessel at the same time, and the particle size of the slurry is measured every 2 hours during the process. The pH is measured once an hour, and the process pH is controlled at 11.5;

[0032] ③When the particle size of the slurry reaches the target particle size of 2.0-2.2 μm, stop inputting the cobalt-aluminum mixed solution, and continue to input the lye alone until the pH of the slurry ...

Embodiment 2

[0038] 1. Prepare 130g / L cobalt sulfate solution, and add 15.232kg aluminum sulfate octadecahydrate and 0.65kg glutamic acid and sodium sulfonate mixed compound complexing agent to each cobalt solution, and stir evenly;

[0039] ② Add an appropriate amount of deionized water to the reaction vessel as the bottom liquid, adjust the pH of the bottom liquid to 11.5 with sodium hydroxide, and feed compressed air with a flow rate of 1.4m 3 / h, the temperature is 72°C, under the stirring speed of 420rpm, the prepared cobalt-aluminum mixed solution and 100g / L sodium hydroxide solution are added to the reaction vessel at the same time, and the particle size of the slurry is measured every 2 hours during the process. The pH is measured once an hour, and the process pH is controlled at 11.0;

[0040] ③When the particle size of the slurry reaches the target particle size of 3.9-4.1 μm, stop inputting the cobalt-aluminum mixed solution, and continue to input the lye alone until the pH of t...

Embodiment 3

[0046] ① Prepare 150g / L cobalt sulfate solution, and add 31.450kg aluminum sulfate octadecahydrate and 1.5kg malic acid and ethanolamine mixed complexing agent to each cobalt solution, and stir evenly;

[0047] ② Add an appropriate amount of deionized water to the reaction vessel as the bottom liquid, adjust the pH of the bottom liquid to 12.0 with sodium hydroxide, and feed compressed air with an air flow rate of 2.1m 3 / h, the temperature is 75°C, under the stirring speed of 450rpm, the prepared cobalt-aluminum mixed solution and 120g / L sodium hydroxide solution are added to the reaction vessel at the same time, and the particle size of the slurry is measured every 2 hours during the process. The pH is measured once an hour, and the process pH is controlled at 10.6;

[0048] ③When the particle size of the slurry reaches the target particle size of 5.8-6.0 μm, stop inputting the cobalt-aluminum mixture, and continue to input the lye alone until the pH of the slurry is 11.8-12...

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Abstract

The invention relates to the technical field of preparation of lithium ion battery precursor cobaltosic oxide, in particular to a preparation method of homogeneous-phase aluminum-doped small-particle-size cobaltosic oxide. According to the method, a composite complexing agent is adopted to balance the reaction rate of Co <2+> and Al <3+> in the system, so that Co <2+> and Al <3+> can be subjectedto homogeneous coprecipitation, and the purpose of uniformly doping aluminum is achieved, by adopting the composite complexing agent, the combination degree of the complexing agent and metal ions canbe effectively controlled, so that the concentration of the metal ions in the tail liquid is reduced. The particle size of the aluminum-doped cobaltosic oxide prepared by the method is 2.0-6.0 [mu]m,the morphology of the aluminum-doped cobaltosic oxide is spherical, the tap density of the aluminum-doped cobaltosic oxide is 2.6-3.0 g / cm <3>, and the mass percent of Al is 0.1-1.2%.

Description

technical field [0001] The invention relates to a preparation method of a lithium-ion battery precursor for high-voltage cobalt tetroxide, in particular to a preparation method of homogeneous aluminum-doped tricobalt tetroxide with a small particle size. Background technique [0002] Tricobalt tetroxide is used to prepare lithium cobalt oxide cathode materials, and its terminals are used in batteries of 3C electronic products such as large-capacity mobile phones, notebook computers, and digital cameras. With the continuous advancement of science and technology, people's consumption level continues to increase, and the performance requirements for electronic products such as battery life and charging rate are also getting higher and higher. The large capacity and high rate of lithium-ion batteries mainly depend on the positive electrode material lithium cobalt oxide. Performance, there are usually two ways to improve the energy density of lithium cobalt oxide: first, doping o...

Claims

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Application Information

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IPC IPC(8): C01G51/04H01M4/525H01M10/0525
CPCC01G51/04H01M4/525H01M10/0525Y02E60/10
Inventor 张荣洲田礼平刘人生秦才胜王能
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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