Method for synthesizing nano lithium iron phosphate without water of crystallization through atmospheric water phase

一种水磷酸亚铁锂、无结晶的技术,应用在常压水相合成纳米无结晶水磷酸亚铁锂的制备领域,能够解决不适合大规模的工业化生产、成组电池短板反应、产品批次稳定性差等问题,达到有利于工业化生产、产品性能好、批次稳定的效果

Active Publication Date: 2013-11-20
JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the main problem of the solid-phase method is that the product batch stability is poor, which directly leads to the short plate reaction of the battery pack; the precursor obtained by the solution co-precipitation method and the sol-gel method is not lithium iron phosphate, but a variety of substances It is difficult to achieve the consistency of each component of the mixture, and the obtained precursor needs to be calcined again at a high temperature to obtain the lithium iron phosphate crystal, which makes the process long, the product consistency is poor, and the equipment investment is large; the hydrothermal method and Although the solvothermal method can directly obtain lithium iron phosphate crystals, it requires high temperature and high pressure reaction equipment, which requires huge investment and is not suitable for large-scale industrial production.

Method used

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  • Method for synthesizing nano lithium iron phosphate without water of crystallization through atmospheric water phase
  • Method for synthesizing nano lithium iron phosphate without water of crystallization through atmospheric water phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 4800L of lithium sulfate solution containing 0.2mol / L lithium to a 6300L enamel reaction kettle, start stirring, add 36.9kg of 85% phosphoric acid and raise the temperature to 80°C, then add aqueous sodium hydroxide solution to the reaction kettle to adjust its pH value Adjust to 11, and finally carry out solid-liquid separation and washing to obtain lithium phosphate solid.

[0020] The obtained lithium phosphate was dispersed in water to prepare a lithium phosphate suspension with a concentration of 0.1 mol / L. At the same time, configure 582L ferrous sulfate solution containing 0.5mol / L iron, and adjust its pH value to 1 with sulfuric acid. Add 3000L of the 0.1mol / L lithium phosphate suspension obtained before into a 5000L reactor equipped with a reflux device, start stirring, heat the lithium phosphate suspension to a reflux state, and slowly add the previously configured 582L of ferrous sulfate solution containing 0.5 mol / L of iron, the time used is controlled ...

Embodiment 2

[0024] Add 4800L lithium hydroxide solution containing 0.4mol / L lithium to a 6300L enamel reaction kettle, start stirring, add 73.8% 85% phosphoric acid and raise the temperature to 70°C, then add sodium hydroxide aqueous solution to the reaction kettle to dissolve it The pH value was adjusted to 11, and finally solid-liquid separation and washing were carried out to obtain lithium phosphate solid.

[0025] The obtained lithium phosphate was dispersed in water to prepare a lithium phosphate suspension with a concentration of 0.2 mol / L. Take an appropriate amount of ferrous acetate and ferrous chloride to prepare 582L of a mixed solution of ferrous acetate and ferrous chloride containing 1mol / L of iron, and adjust its pH value to 1 with nitric acid. Add 3000L of the previously prepared 0.2mol / L lithium phosphate suspension into a 5000L reactor equipped with a reflux device, start stirring, and raise the temperature of the lithium phosphate suspension to a reflux state, and slow...

Embodiment 3

[0029] Add 3000L lithium chloride solution containing 4mol / L lithium to a 5000L enamel reaction kettle, start stirring, add 461kg of 85% phosphoric acid and raise the temperature to 20°C, then add sodium hydroxide aqueous solution to the reaction kettle to adjust its pH The value was adjusted to 9, and finally solid-liquid separation and washing were carried out to obtain lithium phosphate solid.

[0030] The obtained lithium phosphate was dispersed in water to prepare a lithium phosphate suspension with a concentration of 1.0 mol / L. Take an appropriate amount of ferrous chloride to configure 1000L of ferrous chloride solution containing 3 mol / L of iron, and adjust its pH value to 3 with hydrochloric acid. Add 3000L of the previously prepared 1.0mol / L lithium phosphate suspension into a 5000L reactor equipped with a reflux device, start stirring, and raise the temperature of the lithium phosphate suspension to a reflux state, and slowly add the previously prepared Configure t...

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Abstract

The invention discloses a method for synthesizing nano lithium iron phosphate without water of crystallization through an atmospheric water phase, belonging to a method for preparing lithium-ion positive materials. The preparation process comprises the following steps of: preparing lithium phosphate, preparing a lithium phosphate water-phase suspension, preparing a ferrous salt solution, preparing the nano lithium iron phosphate without water of crystallization and recovering and recycling lithium in a lithium iron phosphate mother solution. The method has the beneficial effects of mild reaction condition, less time bucket, low energy consumption, stable batch and uniform and controllable force; as the lithium in the mother solution is recovered and recycled, the cost can be reduced; the method is beneficial to industrial production.

Description

technical field [0001] The invention relates to a preparation method of a positive electrode material of a lithium ion battery, in particular to a preparation method of nanometer crystal-free lithium iron phosphate synthesized in an aqueous phase at normal pressure. Background technique [0002] Lithium ferrous phosphate is a kind of positive electrode material of lithium ion battery. Lithium ferrous phosphate (LiFePO 4 ) crystal has the advantages of low price, less pollution, high capacity, stable structure during charge and discharge process, small capacity attenuation and high safety performance compared with other lithium ion battery cathode materials. Therefore, since it was discovered by Goodenough et al. in 1997 that it has lithium intercalation and desorption properties, lithium iron phosphate has been considered as one of the ideal cathode materials for lithium-ion batteries. [0003] The main methods for synthesizing lithium ferrous phosphate include high-tempera...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/12C01B25/45H01M4/5825Y02E60/10H01M4/525H01M10/0525
Inventor 李南平何国瑞张勤蒋燕锋
Owner JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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