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Preparation method of high-aluminum-doped small-particle-size cobalt carbonate particles

A technology of cobalt carbonate particles and small particle size, applied in the direction of cobalt carbonate, etc., can solve the problems of porous particle size, uneven distribution of aluminum, increase the amount of aluminum doping, etc., to eliminate large particles of agglomerates and avoid excessive nucleation. Fast, consistent crystallinity results

Pending Publication Date: 2021-11-12
취저우화여우코발트뉴머터리얼컴퍼니리미티드 +1
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Problems solved by technology

[0006] The invention provides a method for preparing high-aluminum-doped cobalt carbonate particles with a small particle size, the purpose of which is to solve the problems of uneven distribution of aluminum, internal pores of particles and uneven particle size caused by agglomeration while increasing the amount of aluminum doped

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  • Preparation method of high-aluminum-doped small-particle-size cobalt carbonate particles
  • Preparation method of high-aluminum-doped small-particle-size cobalt carbonate particles
  • Preparation method of high-aluminum-doped small-particle-size cobalt carbonate particles

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preparation example Construction

[0033] Based on above-mentioned findings, propose the preparation method of highly aluminum-doped small particle diameter cobalt carbonate particle of the present invention, this preparation method comprises the following steps:

[0034] (1) Prepare solution: prepare a mixed salt solution of soluble cobalt salt and aluminum salt, wherein the mass ratio of aluminum element to cobalt element is 0.011~0.014, and prepare ammonium bicarbonate solution;

[0035] (2) Preparation of seed crystals: add water and ammonium bicarbonate solution as the bottom liquid in the reactor, add mixed salt solution and ammonium bicarbonate solution in a parallel feeding mode, so that the feeding rate of cobalt ions relative to the volume of the reactor is 0.048 ±0.012mol / L / hour, control the reaction temperature at 35±5°C and keep it substantially constant, and react until cobalt carbonate seeds with a particle size D50 of 1.3-1.5 μm are obtained; and

[0036] (3) Synthetic growth: continue to add mi...

Embodiment 1

[0051] Preparation of solution: preparation of cobalt sulfate solution with a cobalt content of 115g / L, doping with aluminum salt to obtain a mixed salt solution, so that the mass ratio of aluminum element to cobalt element in the mixed salt solution is 0.0113. Prepare ammonium bicarbonate solution.

[0052] Preparation of seed crystals: prepare 10 L of diluted ammonium bicarbonate solution with a concentration of 15 g / L in a reaction kettle with a volume of 50 L as the bottom liquid, and adjust the pH value of the bottom liquid to ≥ 8 by heating, stirring and drafting. Under the condition of constant temperature water bath at 30°C, the mixed salt solution and the ammonium bicarbonate solution were pumped into the reaction kettle concurrently, so that the pumping flow rate of the mixed salt solution was 16mL / min (approximately the feeding rate of cobalt ions relative to the volume of the reaction kettle) is 0.036mol / L / hour). During the co-current feeding process, the mass rat...

Embodiment 2

[0056] Prepare the solution: prepare a cobalt sulfate solution with a cobalt content of 120g / L, and dope it with an aluminum salt to obtain a mixed salt solution, so that the mass ratio of the aluminum element to the cobalt element in the mixed salt solution is 0.0126. Prepare ammonium bicarbonate solution.

[0057] Preparation of seed crystals: prepare 10 L of diluted ammonium bicarbonate solution with a concentration of 20 g / L in a reaction kettle with a volume of 50 L as the bottom liquid, and adjust the pH value of the bottom liquid to ≥ 8 by heating, stirring and drafting. Under the condition of constant temperature water bath at 35°C, the mixed salt solution and the ammonium bicarbonate solution were pumped into the reaction kettle in parallel, so that the pumping flow rate of the mixed salt solution was 20mL / min (approximately the feeding rate of cobalt ions relative to the volume of the reaction kettle) is 0.048mol / L / hour). During the co-current feeding process, the m...

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Abstract

The invention discloses a preparation method of high-aluminum-doped small-particle-size cobalt carbonate particles, and the method mainly comprises the following steps: preparing a mixed salt solution of soluble cobalt salt and aluminum salt, the mass ratio of the aluminum element to the cobalt element being 0.011-0.014; adding a mixed salt solution of cobalt and aluminum sulfate and an ammonium bicarbonate solution into a diluted ammonium bicarbonate solution, and preparing a cobalt carbonate seed crystal with D50 of 1.3-1.5 [mu] m by adopting a low-temperature and low-feeding-rate synthesis process; and then preparing small-particle-size cobalt carbonate particles through a subsequent synthesis growth process. The prepared cobalt carbonate has the characteristics of high aluminum doping amount and consistent overall crystallinity of particles, and the problems that aluminum in cobaltosic oxide particles obtained after high-aluminum-doping cobalt carbonate is calcined is not uniformly distributed, and the interiors of the particles are porous are effectively solved.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a method for preparing cobalt carbonate as a precursor of lithium battery cathode materials. Background technique [0002] Cobalt carbonate is an extremely important raw material in the lithium cobalt oxide cathode material industry. Cobalt carbonate can be calcined into tricobalt tetroxide, which can be further sintered with lithium carbonate to produce lithium cobaltate. [0003] Improving the energy density of batteries by increasing the charge cut-off voltage and compaction density of lithium cobalt oxide is the current and future technology development direction. This correspondingly caused cobalt tetroxide and cobalt carbonate to develop in two directions: one is that the product particles develop towards both ends of the large particle size and small particle size, in order to increase the compaction density of the positive electrode material by mixing and matching ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/06
CPCC01G51/06C01P2004/03C01P2004/61
Inventor 郑德洲田礼平刘人生夏勇刘冠宇
Owner 취저우화여우코발트뉴머터리얼컴퍼니리미티드
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