Preparation method of composite lithium salt concentrated solution

A technology of composite lithium salt and concentrated solution, which is applied in the field of preparation of composite lithium salt concentrated solution, can solve problems such as difficult product separation and purification, unfavorable industrialization implementation, poor thermal stability, etc., achieve short process production cycle, improve cycle performance and High-temperature storage performance and good product performance

Inactive Publication Date: 2020-11-13
湖南法恩莱特新能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lithium hexafluorophosphate has good electrical conductivity and electrochemical performance, can effectively purify aluminum foil, and has good compatibility with graphite negative electrodes, but lithium hexafluorophosphate has the problems of being sensitive to water and poor thermal stability
At this stage, the methods for preparing lithium difluorophosphate are mainly divided into two categories: difluorophosphoric acid method and lithium hexafluorophosphate method according to the source of raw materials, both of which have disadvantages such as high raw material price, complicated process, high energy consumption, difficult product separation and purification, and low yield. , is not conducive to the implementation of industrialization

Method used

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  • Preparation method of composite lithium salt concentrated solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] This example has prepared a kind of composite lithium salt concentrate, and concrete steps are as follows:

[0034] Replace the reaction vessel with nitrogen in advance, then add 69 g of phosphorus pentoxide, start stirring, and slowly add 97.2 g of anhydrous hydrofluoric acid and 155.5 g of sulfur trioxide gas at the same time, control the reaction temperature at 80°C, and the reaction time for 1 h. The produced gas was purified to obtain 120 g of phosphorus pentafluoride gas.

[0035] Under the protection of nitrogen, add 280 g of dimethyl carbonate and 35 g of lithium carbonate to a closed container equipped with mechanical stirring, thermometer, and condenser, start stirring, control the reaction temperature at 30°C, and continuously introduce purified Phosphorus pentafluoride gas, the gas flow rate is 0.35 L / min, continue to react for 3 h. After the reaction is finished, the reaction liquid is subjected to precision filtration, and then the filtrate is concentrate...

Embodiment 2

[0038] This example has prepared a kind of composite lithium salt concentrate, and concrete steps are as follows:

[0039] Replace the reaction vessel with argon in advance, then add 113 g of phosphorus pentoxide, start stirring, and slowly add 188.1 g of anhydrous hydrofluoric acid and 286.4 g of sulfur trioxide gas at the same time, control the reaction temperature at 120 °C, and the reaction time for 40 min. The resulting gas was purified to obtain 197.5 g of phosphorus pentafluoride gas.

[0040] Under the protection of argon, add 580 g of triethylene glycol dimethyl ether and 58 g of lithium carbonate into a closed container with mechanical stirring, thermometer, and condenser tube, start stirring, control the reaction temperature at 40 °C, and insert the gas tube through the bottom The phosphorus pentafluoride gas was continuously introduced at a gas flow rate of 0.44 L / min, and the reaction was continued for 2 h. After the reaction is finished, the reaction liquid is s...

Embodiment 3

[0043] This example has prepared a kind of composite lithium salt concentrate, and concrete steps are as follows:

[0044] Replace the reaction vessel with helium in advance, then add 162.2 g of phosphorus pentoxide, start stirring, and slowly add 339.2 g of anhydrous hydrofluoric acid and 456 g of sulfur trioxide gas at the same time, control the reaction temperature at 150 °C, and the reaction time for 0.5 h. The resulting gas was purified to obtain 285 g of phosphorus pentafluoride gas.

[0045]Under the protection of helium, add 860 g of acetone and 86 g of lithium carbonate to the airtight container equipped with mechanical stirring, thermometer, and condenser, start the stirring, control the reaction temperature at 50 °C, and continuously introduce pentafluoride Phosphorus gas, the gas flow rate was 0.65 L / min, and the reaction was continued for 1 h. After the reaction is finished, the reaction solution is subjected to precision filtration, and then the filtrate is conc...

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Abstract

The invention provides a preparation method of a composite lithium salt concentrated solution. The method comprises the following steps of: putting lithium carbonate into an organic solvent in an inert atmosphere to obtain slurry, and introducing phosphorus pentafluoride gas into the slurry to react to obtain a composite lithium salt concentrated solution. According to the preparation method provided by the invention, the composite lithium salt concentrated solution containing lithium difluorophosphate and lithium hexafluorophosphate can be prepared by taking phosphorus pentafluoride and lithium carbonate as raw materials through a gas-solid reaction under a non-aqueous solvent condition and a one-step method, has the advantages of short process flow, no side reaction, high reaction efficiency, good product performance, high yield and no emission of three wastes, and is short in process production period and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a preparation method of a composite lithium salt concentrated solution. Background technique [0002] The high and low temperature cycle performance of lithium-ion batteries directly determines the cruising range and service life of electric vehicles. At present, the most widely used electrolyte material is lithium hexafluorophosphate, the molecular formula is LiPF 6 , is currently the most important electrolyte lithium salt used in commercial lithium-ion batteries, and is mainly used for lithium-ion energy storage batteries and other daily-use batteries. The production methods of lithium hexafluorophosphate mainly include hydrogen fluoride solvent method and organic solvent method, among which hydrogen fluoride solvent method is currently the main method for industrially producing lithium hexafluorophosphate. Lithium hexafluorophosphate has good elect...

Claims

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Application Information

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IPC IPC(8): C01D15/00C01B25/455C01B25/10
CPCC01B25/10C01B25/455C01D15/005
Inventor 邵俊华孔东波李海杰张利娟王郝为郭飞闫国锋宋东亮王亚洲侯红歧谢佳庆韩飞乔文忠
Owner 湖南法恩莱特新能源科技有限公司
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