Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of lithium tetrafluoroborate phosphate, non-aqueous electrolyte and battery

A technology of lithium tetrafluorooxalate phosphate and non-aqueous electrolyte, applied in electrolytic capacitors, secondary batteries, chemical instruments and methods, etc., can solve the problems of high chlorine compounds, difficult separation, complicated reactions, etc., and achieves low cost and high price. Inexpensive, easy-to-use effects

Active Publication Date: 2020-09-01
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
View PDF9 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But adopting this method can generate toxic silicon tetrafluoride gas, which is harmful to the environment, and the product prepared simultaneously contains higher chlorine compounds, free acid is difficult to remove, and has a negative impact on the battery characteristics of the non-aqueous electrolyte battery. Not suitable for industrial production
[0005] CN105218348A prepares phosphorus pentafluoride by reacting phosphorus pentachloride and hydrofluoric acid. The method has complex reactions and many steps, and the product is accompanied by lithium hexafluorophosphate, which is difficult to separate
[0008] KR1020130102969A discloses through LiPF 6 React with bis(trimethylsilyl) oxalate to obtain the target product, but it is easy to generate by-products lithium difluorophosphate and lithium difluorobisoxalate phosphate, making it difficult to separate the target product

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of lithium tetrafluoroborate phosphate, non-aqueous electrolyte and battery
  • Preparation method of lithium tetrafluoroborate phosphate, non-aqueous electrolyte and battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] In a glove box, take 30 g (0.128 mol) of bis(trimethylsilyl) oxalate with a moisture content of less than 50 ppm in a three-necked flask, add 130 mL of acetonitrile with a moisture content of less than 10 ppm dried with molecular sieves, and dissolve to obtain bis(trimethylsilyl) oxalate. (trimethylsilyl)oxalate solution.

[0062] The solution was removed from the glove box, and 0.134 mol of phosphorus pentafluoride gas was introduced at 60° C. (the molar ratio of bis(trimethylsilyl) oxalate to phosphorus pentafluoride was 1:1.05) to participate in the reaction. After the addition was completed, stirring was continued for 2 h and the reaction was completed to obtain the first reaction mixture.

[0063] 3.64 g (0.14 mol) of dry lithium fluoride was added to the first reaction mixture, and then in a nitrogen atmosphere, the temperature was raised to 90° C. to carry out the reaction for 6 h. After the reaction was completed, the second reaction mixture was obtained.

[00...

Embodiment 2

[0070] In the glove box, take 60 g (0.256 mol) of bis(trimethylsilyl) oxalate with a moisture content of less than 50 ppm in a three-necked flask, add 430 mL of dimethyl carbonate with a moisture content of less than 10 ppm dried with molecular sieves, Dissolution gave a solution of bis(trimethylsilyl)oxalate.

[0071] The solution was removed from the glove box, and 0.28 mol of phosphorus pentafluoride gas was introduced at 80°C (the molar ratio of bis(trimethylsilyl) oxalate to phosphorus pentafluoride was 1:1.1) to participate in the reaction. After the addition was completed, stirring was continued for 10 h and the reaction was completed to obtain the first reaction mixture.

[0072] 7.54 g (0.29 mol) of dry lithium fluoride was added to the first reaction mixture, and then in a nitrogen atmosphere, the temperature was raised to 85° C. for 8 hours, and the second reaction mixture was obtained after the reaction was completed.

[0073] The second reaction mixture was subje...

Embodiment 3

[0079] In the glove box, take 100 g (0.427 mol) of bis(trimethylsilyl) oxalate with a moisture content of less than 50 ppm in a three-necked flask, add 540 mL of dimethyl carbonate with a moisture content of less than 10 ppm dried with molecular sieves, Dissolution gave a solution of bis(trimethylsilyl)oxalate.

[0080] The solution was removed from the glove box, and 0.49 mol of phosphorus pentafluoride gas was introduced at 85° C. (the molar ratio of bis(trimethylsilyl) oxalate to phosphorus pentafluoride was 1:1.16) to participate in the reaction. After the addition was completed, stirring was continued for 6 h and the reaction was completed to obtain the first reaction mixture.

[0081] 16.6 g (0.64 mol) of dry lithium fluoride was added to the first reaction mixture, and then in a nitrogen atmosphere, the temperature was raised to 90° C. for 8 h, and the second reaction mixture was obtained after the reaction was completed.

[0082] The second reaction mixture was subjec...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to the technical field of energy storage batteries, and provides a preparation method of lithium tetrafluoroborate phosphate, a non-aqueous electrolyte containing the lithium tetrafluoroborate phosphate and a battery. The method comprises the following steps of: reacting bis (trimethylsilyl) oxalate with PF5 to obtain a first reaction mixture; then adding LiF into the first reaction mixture, and performing reaction to obtain a second reaction mixture; and carrying out post-treatment on the obtained second reaction mixture to obtain the lithium tetrafluoroborate phosphate.The preparation method of the lithium tetrafluoroborate phosphate provided by the invention is simple to operate; the obtained product is single; the yield is high; synthetic raw materials are cheapand easily available; the cost is low; and the method is suitable for industrial production.

Description

technical field [0001] The present invention relates to the technical field of energy storage batteries, and more particularly, to a preparation method of lithium tetrafluorooxalate phosphate, a non-aqueous electrolyte solution and a battery containing lithium tetrafluorooxalate phosphate. Background technique [0002] Lithium tetrafluorooxalate phosphate is mainly used as an additive for non-aqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors. After the additive is added, the electrolyte has excellent high temperature resistance, and a more stable solid electrolyte interface film structure can be formed on the surface of the positive electrode material, thereby improving the cycle performance of the battery. [0003] At present, the preparation methods of this kind of additives mainly include the following: [0004] EP1308449A2 and CN102216311B disclose that lithium hexafluorophosphate is dissolved in an organic solvent, reacted in the pr...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574H01M10/0525H01M10/0567H01M10/42H01G11/06H01G11/64
CPCC07F9/65742H01M10/0567H01M10/0525H01M10/4235H01G11/64H01G11/06Y02E60/10
Inventor 冯天明余意何凤荣
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com