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Method for reducing sulphur content of ternary precursor

A technology of sulfur content and precursors, which is applied in the field of preparation of ternary precursors, can solve the problems of low capacity and poor cycle performance of positive electrode materials, and achieve the effects of reducing impurity content, improving tap density and saving water resources.

Active Publication Date: 2020-02-21
宜宾光原锂电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problem that during the preparation of the ternary precursor of sulfate in the prior art, a large amount of sulfate radicals are physically and chemically adsorbed on the surface or inside of the ternary precursor, resulting in low capacity of the positive electrode material obtained after sintering. The problem of poor cycle performance, and provide a method to reduce the sulfur content of the ternary precursor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Flow the nickel-cobalt-manganese sulfate solution, ammonia water, and sodium hydroxide into the 50L reactor at the same time. The total volume of the feed liquid in the reactor is basically equal to the volume of the reactor, and nitrogen is introduced, and the stirring is set to 600rpm, and the temperature of the reaction system is set 40°C, ammonia value 8.0g / L, pH value 11.3, wherein the molar ratio of nickel-cobalt-manganese in the mixed salt solution is 5:2:3, the concentration of the mixed salt solution is 2.5mol / L, the mass of sodium hydroxide solution The percentage concentration is 32%, and the mass percentage concentration of ammonia water is 21%.

[0024] After reacting for 5 hours, open the clear liquid overflow port, feed pure water at 40°C at a flow rate of 36ml / min, automatically adjust the lye flow rate to stabilize the pH of the reaction system at 11.3, and adjust the flow rate of ammonia water to 8.2ml / min, so that The ammonia value was stable at 8.0±0...

Embodiment 2

[0027] Flow nickel-cobalt sulfate, sodium metaaluminate solution, ammonia water, and sodium hydroxide into a 500L reactor at the same time. The total volume of the feed liquid in the reactor is basically equal to the volume of the reactor, and nitrogen is introduced, and the stirring is set at 500rpm. The system temperature is set at 50°C, the ammonia value is 11.0g / L, and the pH value is 11.6, wherein the molar ratio of nickel sulfate, cobalt sulfate, and sodium metaaluminate is 88:9:3, and the concentration of nickel-cobalt sulfate is 1.3mol / L, the concentration of sodium metaaluminate solution is 0.2mol / L, the mass percent concentration of sodium hydroxide solution is 32%, and the mass percent concentration of ammonia water is 21%.

[0028] After reacting for 10 hours, open the overflow port of the clear liquid, feed pure water at 50°C at a flow rate of 400ml / min, automatically adjust the flow rate of lye to stabilize the pH of the reaction system at 11.6, adjust the flow r...

Embodiment 3

[0031] The mixed sulfate solution of nickel, cobalt and manganese, ammonia, and sodium hydroxide flow into the 200L reactor at the same time. The total volume of the feed liquid in the reactor is basically equal to the volume of the reactor, and nitrogen is fed into it. The stirring is set to 800rpm, and the temperature of the reaction system is set to Set at 60°C, ammonia value 14.0g / L, pH value 10.6, wherein the molar ratio of nickel-cobalt-manganese in the mixed salt solution is 5:2:3, the concentration of the mixed salt solution is 2.5mol / L, the sodium hydroxide solution The mass percent concentration is 32%, and the mass percent concentration of ammonia water is 21%.

[0032] After reacting for 12 hours, open the overflow port of the clear liquid, feed pure water at 60°C at a flow rate of 8L / h, automatically adjust the flow rate of lye to stabilize the pH of the reaction system at 10.6, adjust the flow rate of ammonia water to 115ml / min, and make ammonia The value was sta...

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Abstract

The invention discloses a method for reducing the sulphur content of a ternary precursor. Sulfate is used as a ternary salt raw material, and the ternary salt raw material, an alkaline solution and acomplexing agent are added to a reaction kettle for co-precipitation to prepare the ternary precursor, after co- precipitation reaction is carried out for 5-15 hours, pure water is added continuouslyor intermittently to the reaction kettle to replace clear liquid in the reaction kettle, and meanwhile, the alkaline solution and the complexing agent are added to keep a reaction system stable. The problem that the sulphur content in the ternary precursor exceeds the standard due to the fact that the sulfate is adsorbed on the surface of a crystal during the growth of the crystal and then wrappedinside the crystal is solved, the sulphur content of the prepared ternary precursor after one-time washing is less than 530 ppm, and during the subsequent water washing process, water resources are effectively saved; and the impurity content is reduced, the jolt ramming density of the ternary precursor is increased, and the morphology of the ternary precursor is not affected.

Description

technical field [0001] The present invention relates to the technical field of the preparation method of the ternary precursor, especially a method for reducing the sulfur content of the ternary precursor. Background technique [0002] At present, lithium-ion batteries occupy a large market share in the field of portable electronic devices by virtue of their advantages such as high specific capacity, long cycle life, low self-discharge rate, no memory effect, and environmental friendliness, and are recognized as the most promising electric battery. Vehicle power battery. The ternary nickel-cobalt-manganese cathode material is an important cathode material for lithium-ion batteries. It has important advantages such as better performance than lithium cobalt oxide, much lower cost than lithium cobalt oxide, and much higher energy density than lithium iron phosphate. Mainstream cathode material for automotive power batteries. [0003] In the preparation process of positive ele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00H01M4/505H01M4/525H01M10/0525
CPCC01G53/006C01P2006/80H01M4/505H01M4/525H01M10/0525Y02E60/10
Inventor 王政强宋方亨颜加明林江李袁琪杜先锋孙宏
Owner 宜宾光原锂电材料有限公司
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