Preparation method of double-layer composite low-cost lithium-rich manganese-based precursor

A lithium-rich manganese-based, double-layer composite technology, applied in chemical instruments and methods, nickel compounds, structural parts, etc., can solve the problems of narrow particle size distribution, high sphericity, high vibration, etc., to achieve narrow particle size distribution, sphericity High, high vibration effect

Pending Publication Date: 2022-05-10
浙江格派钴业新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method provided by the invention solves the problem that the pH of the reaction process is uncontrollable and easy to oxidize. The obtained lithium-rich manganese-based precursor has high sphericity, high vibration, and narrow particle size distribution. The general formula is (Ni x mn (1-x) )OH 2 @CO 3 (0.1≤x≤0.3)

Method used

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  • Preparation method of double-layer composite low-cost lithium-rich manganese-based precursor
  • Preparation method of double-layer composite low-cost lithium-rich manganese-based precursor
  • Preparation method of double-layer composite low-cost lithium-rich manganese-based precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Prepare soluble nickel-manganese sulfate in a ratio of 1:3 (nickel element to manganese element is 1:3), and prepare a mixed solution with a concentration of 1.6mol / L; add citric acid with a concentration of 1.5g / L to the mixed solution , configure a mixed alkali solution with a molar ratio of sodium hydroxide and sodium carbonate of 1:40; add 35L of pure water to a 50L reactor, add 3.5g of ascorbic acid, 2L of ammonia water and 400ml of sodium hydroxide solution to prepare a bottom solution; heat up to 50°C , pass nitrogen gas for 2 hours, wait for the temperature and rotation speed to be constant, the first stage of reaction: flow sodium hydroxide solution, ammonia water and metal salt solution into the reactor; adjust the flow rate of sodium hydroxide solution, adjust the ph at about 11.8, and make the particle size grow steadily to 5 microns; the second stage of reaction: stop feeding ammonia water, and replace the sodium hydroxide solution with the above-mentioned m...

Embodiment 2

[0029] The soluble nickel-manganese sulfate is formulated into a mixed solution with a concentration of 1.8mol / L according to the ratio of 1:3; citric acid with a concentration of 2.0g / L is added to the mixed solution, and the molar ratio of sodium hydroxide and sodium carbonate is configured as 1:30 mixed alkali solution; add 35L of pure water to a 50L reactor, add 3.5g of ascorbic acid, 2L of ammonia water and 400ml of sodium hydroxide solution to make a bottom solution; raise the temperature to 55°C, blow nitrogen for 2 hours, wait until the temperature and speed are constant, and react The first stage: flow sodium hydroxide solution, ammonia water and metal salt solution into the reactor; by adjusting the flow rate of sodium hydroxide solution, adjust the pH at about 11.6, so that the particle size can grow steadily to 5 microns; the second stage of the reaction: stop the process ammonia water, and replace the sodium hydroxide solution with the above-mentioned mixed alkali ...

Embodiment 3

[0031] The soluble nickel-manganese sulfate is formulated into a mixed solution with a concentration of 1.8mol / L according to the ratio of 1:3; citric acid with a concentration of 2.0g / L is added to the mixed solution, and the molar ratio of sodium hydroxide and sodium carbonate is configured as 1:20 mixed alkali solution; add 35L of pure water to a 50L reactor, add 3.5g of ascorbic acid, 2L of ammonia water and 400ml of sodium hydroxide solution to make a bottom solution; raise the temperature to 55°C, blow nitrogen for 2 hours, wait until the temperature and speed are constant, and react The first stage: flow sodium hydroxide solution, ammonia water and metal salt solution into the reactor; by adjusting the flow rate of sodium hydroxide solution, adjust the pH at about 11.4, so that the particle size can grow steadily to 5 microns; the second stage of the reaction: stop the process ammonia water, and replace the sodium hydroxide solution with the above-mentioned mixed alkali ...

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Abstract

The invention discloses a preparation method of a double-layer composite low-cost lithium-rich manganese-based precursor, and belongs to the technical field of lithium battery material preparation. The general formula of the lithium-rich manganese-based precursor is (NixMn (1-x)) OH2 (at) CO3, wherein x is more than or equal to 0.1 and less than or equal to 0.3. Preparing a nickel-manganese mixed solution and adding a complexing agent with a certain concentration; preparing a mixed alkali solution of sodium hydroxide and sodium carbonate; adding a buffer solution into the reaction kettle as a base solution; a first-stage reaction: adding the nickel-manganese mixed solution, ammonia water and a sodium hydroxide solution into a reaction kettle in a parallel flow manner, and carrying out a co-precipitation reaction; a second-stage reaction: after the particle size grows to 5 microns, replacing the sodium hydroxide solution with the mixed alkali solution prepared in the step (1), and closing the ammonia water; continuously reacting; controlling the temperature, stirring speed and feed liquid flow in the reaction process to be constant, and introducing nitrogen in the whole reaction process; according to the invention, the problems of uncontrollable pH and easy oxidation in the reaction process are solved, and the obtained lithium-rich manganese-based precursor has the advantages of high sphericity, high tap density and narrow particle size distribution.

Description

technical field [0001] The invention relates to the technical field of lithium-ion battery preparation, in particular to a preparation method of a double-layer composite low-cost lithium-rich manganese-based precursor. Background technique [0002] The development of high-performance, low-cost new electrode cathode materials has always been a hot research direction for lithium-ion batteries. Although as early as 1991 LiCoO 2 Cathode materials have been commercially used, but their reversible capacity is low and expensive; so researchers have focused on LiCoO 2 material substitutes. Among many layered cathode materials, lithium-rich manganese-based layered cathode materials have attracted widespread attention due to their high reversible specific capacity, high operating voltage, and excellent storage performance at room temperature. The key electrode material is regarded as the most promising cathode material. [0003] At present, the coprecipitation method is the most c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/50H01M4/505H01M10/0525
CPCC01G53/00H01M4/505H01M4/50H01M10/0525C01P2004/03C01P2002/72C01P2004/61C01P2004/32C01P2006/10C01P2006/11
Inventor 许益伟曹栋强龚丽锋方明郝培栋曹天福苏方哲李晓升邓明曾启亮丁何磊陈艳芬柴冠鹏张旭王博周忍朋郑红韩宇航张伟伟
Owner 浙江格派钴业新材料有限公司
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