Preparation method of ternary precursor

A precursor and volume technology, which is applied in chemical instruments and methods, inorganic chemistry, nickel compounds, etc., can solve the problems of narrow particle size distribution of precursors, poor circulation, stability and safety of precursors, etc., to improve charge conduction rate, The effect of uniform size and ensuring structural integrity

Active Publication Date: 2020-02-18
帕瓦(兰溪)新能源科技有限公司
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Problems solved by technology

[0008] The process of combining intermittent concentration and separate kettles is adopted to ensure that the precursor is in a stable state during the reaction process by controlling the process parameters of each stage, ensuring that the particle size distribution of the precursor is narrow, uniform in size, and good in sphericity. The control of the growth of precursor particles enables the prepared precursor to have a loose-dense multi-layer core-shell structure, which solves the above-mentioned problems of poor circulation, stability and safety of the ternary precursor

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Embodiment 1

[0039] A preparation method of a ternary precursor, comprising the following steps:

[0040] (1) Take 30L of 25% industrial ammonia water to obtain complexing agent aqueous solution A; uniformly mix 12kg of sodium hydroxide and hot pure water to prepare 30L of precipitant aqueous solution B; mix 15.39kg of nickel sulfate hexahydrate, 1.508kg Cobalt sulfate heptahydrate, 7.203kg manganese sulfate monohydrate (nickel-cobalt-manganese molar ratio Ni:Co:Mn=5.5:0.5:4.0) and hot pure water are fully mixed and prepared into 50L aqueous solution C;

[0041] (2) Complexing agent aqueous solution A, precipitant aqueous solution B, and aqueous solution C are kept at a constant temperature of 40°C; adjust the temperature of the constant temperature reactor to 68°C, add hot pure water to 1 / 4 of the reactor, and then add complexing agent aqueous solution A, The precipitant aqueous solution B is adjusted to the ammonia concentration of the system at 14g / L and the pH at 12.5, and is prepared ...

Embodiment 2

[0047] A preparation method of a ternary precursor, comprising the following steps:

[0048] (1) Take 25L of 25% industrial ammonia water and prepare complexing agent aqueous solution A; mix 6.6kg lithium hydroxide with hot pure water evenly to prepare 25L precipitant aqueous solution B; mix 18.447kg nickel chloride hexahydrate, 6.157kg of cobalt chloride hexahydrate, 5.131kg of manganese chloride tetrahydrate (nickel-cobalt-manganese molar ratio Ni:Co:Mn=6:2:2) are fully mixed with hot pure water to prepare 50L aqueous solution C;

[0049] (2) Keep complexing agent aqueous solution A, precipitant aqueous solution B, and aqueous solution C at a constant temperature of 35°C, control the temperature of the constant temperature reactor at 62°C, add hot pure water to 1 / 2 of the reactor, and then add complexing agent aqueous solution A, Aqueous precipitant solution B, the ammonia concentration of the control system is 13g / L, the pH is 12.3, and it is prepared as the reaction kettle...

Embodiment 3

[0054] A preparation method of a ternary precursor, comprising the following steps:

[0055] (1) Select 20L of 25% ammonia water to obtain complexing agent aqueous solution A; uniformly mix 11.2kg potassium hydroxide with hot pure water to prepare 20L precipitant aqueous solution B; mix 14.128kg nickel nitrate hexahydrate, 5.655kg Cobalt nitrate, 7.319 kg of manganese nitrate tetrahydrate (nickel-cobalt-manganese molar ratio Ni:Co:Mn=5:2:3) and deionized water were fully mixed and evenly adjusted to 120L to prepare aqueous solution C;

[0056] (2) Complexing agent aqueous solution A, precipitating agent aqueous solution B, and aqueous solution C are kept at a constant temperature of 38°C, and the temperature of the constant temperature reactor is controlled at 60°C. Add hot pure water to 1 / 4 of the reactor, and then add complexing agent aqueous solution A, The precipitant aqueous solution B is adjusted to the ammonia concentration of the system at 13.5g / L and the pH at 12.4, a...

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Abstract

The invention provides a preparation method of a ternary precursor, and belongs to the technical field of lithium ion battery materials. A technology combining intermittent concentration with a separation kettle is adopted to stably control the reaction condition of each step. The growth of secondary particles of a precursor is controlled by gradually reducing the pH in the reaction process, and the structure of the precursor is gradually changed from loose to dense by setting a precise clearing amount. The solid content of a slurry in a kettle is adjusted through the separation kettle to makethe precursor have a multilayer core-shell design with a loose-compact structure. The precursor prepared in the invention has the advantages of narrow particle size distribution, good sphericity degree and uniform size, has the multilayer core-shell with the loose-compact structure, and has enough space during circulation and crystal form mutation to avoid structural collapse and ensure the circularity, stability and safety of the precursor. Compared with precursors with internal complete voids, the ternary precursor of the invention has the advantages of compact and stable structure, high energy density, and solving of the problems of poor circularity, stability and safety of common ternary precursors.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a preparation method of a ternary precursor with a narrow particle size distribution and a multi-core-shell structure. Background technique [0002] Lithium-ion batteries have been widely used due to their good cycle performance, high capacity, low price, convenient use, safety and environmental protection. With the rapid development of the industry, the performance requirements of lithium-ion batteries are also getting higher and higher. High-performance cathode materials are crucial to the commercial development of lithium-ion batteries, so improving the performance of ternary precursors is imminent. At present, the preparation of ternary precursors by traditional processes has brought a series of safety and performance problems due to structural powdering, cyclic diving, and crystal mutations. For this, doping, coating, and structural design are generally used t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00
CPCC01G53/006C01P2004/03C01P2004/32C01P2004/52
Inventor 欧星张佳峰彭春丽
Owner 帕瓦(兰溪)新能源科技有限公司
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