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Synthesis method of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphonitrile

A technology of pentafluorocyclotriphosphazene and hexafluorocyclotriphosphazene, applied in the field of synthesis of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene, capable of solving lithium ion The electrochemical performance of the battery is unfavorable, the flash point of the lithium battery electrolyte solvent cannot be significantly improved, and the battery cannot completely prevent fire, combustion, explosion and other problems, so as to achieve the effects of good controllability of the reaction, avoiding unnecessary losses, and high yield

Inactive Publication Date: 2015-04-29
湖北诺邦科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] However, as lithium battery electrolyte additives, the above-mentioned substances have significant disadvantages
Hexamethoxycyclotriphosphazene, hexapropoxycyclotriphosphazene, and hexaphenoxycyclotriphosphazene cannot significantly increase the flash point of the lithium battery electrolyte solvent, and cannot completely prevent the battery from being abused and overcharged. Fire, combustion, explosion and other safety hazards
At the same time, the above substances are unfavorable for improving the electrochemical performance of lithium-ion batteries.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Place 10.0 g of hexachlorocyclotriphosphazene crystals, 100 ml of chlorobenzene, and catalyst tetramethylammonium bromide TMAB in a 250 ml three-necked flask with a stirrer, a thermometer, and a reflux condenser, and stir until it dissolves evenly. React with 12.03 g of potassium fluoride at 60°C for 3 hours, filter and distill under reduced pressure to obtain the phosphazene derivative hexafluorocyclotriphosphazene.

[0035] Put the hexafluorocyclotriphosphazene obtained above in 90 ml of chlorobenzene, add 5 g of ferric chloride and 1.63 g of sodium ethoxide as a catalyst under constant stirring, and react for 4 h at a temperature of 70 °C, carry out vacuum distillation, and refine Afterwards, the phosphazene derivative 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene was obtained.

Embodiment 2

[0037] 10.0 g of hexachlorocyclotriphosphazene crystals, 100 ml of chlorobenzene, and catalyst tetramethylammonium bromide TMAB were placed in a 250 ml three-necked flask with a stirrer, a thermometer, and a reflux condenser, and stirred until they were dissolved evenly. React with 13.53 g of potassium fluoride at 70 °C for 4 h to obtain the phosphazene derivative hexafluorocyclotriphosphazene after purification.

[0038] Put the hexafluorocyclotriphosphazene obtained above in 90 ml of chlorobenzene, add the catalyst ferric chloride and 1.45 g of sodium ethoxide under constant stirring, react at 75 °C for 4 h, carry out vacuum distillation, and obtain Phosphazene derivative 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene.

Embodiment 3

[0040] Put 10.00 g of hexachlorocyclotriphosphazene crystals, 100 ml of chlorobenzene, and catalyst tetramethylammonium bromide (TMAB) in a 250 ml three-necked flask equipped with a stirrer, thermometer, and reflux condenser, and stir until dissolved Evenly, react with 15.04 g of potassium fluoride at 80 °C for 5 h to obtain the phosphazene derivative hexafluorocyclotriphosphazene after purification.

[0041]Put the hexafluorocyclotriphosphazene obtained above in 90 ml of chlorobenzene, add the catalyst ferric chloride and 1.31 g of sodium ethoxide under constant stirring, react at 80°C for 4 h, carry out vacuum distillation, and obtain Phosphazene derivative 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene.

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PUM

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Abstract

The invention relates to a synthesis method of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphonitrile, which comprises the following steps: a. in a catalyst-added organic solvent, substituting six chlorine atoms of hexachlorocyclotriphosphonitrile with fluorate to prepare a hexafluorocyclotriphosphonitrile-containing product, and distilling to remove the byproduct and solvent, thereby obtaining the hexafluorocyclotriphosphonitrile; and b. reacting the hexafluorocyclotriphosphonitrile obtained in the step a with ethylate in a catalyst-added organic solvent to substitute one fluorine atom with one ethoxy group so as to obtain a product containing 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphonitrile, and distilling to remove the byproduct and solvent, thereby obtaining the 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphonitrile. The synthesis method has the advantages of mild reaction conditions and high reaction controllability, and is convenient for industrial production. The method also has the advantages of simple technical process, low energy consumption, recoverable solvent, higher yield and higher product purity.

Description

technical field [0001] The present invention relates to a synthesis method of phosphazene derivatives, in particular to a synthesis method of 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene, which is applied to high-performance lithium-ion batteries electrolyte additives. Background technique [0002] Phosphazene compounds are a kind of inorganic-organic hybrid compounds whose skeletons are alternately arranged by phosphorus and nitrogen, and can be divided into cyclic phosphazenes and polyphosphazenes. Wherein, hexachlorocyclotriphosphazene is the most representative compound in cyclic phosphazene compounds, and its structural formula is: [0003] [0004] In the above structural formula of hexachlorocyclotriphosphazene, the six-membered ring has a similar structure to the benzene ring, and the phosphorus and nitrogen bonds are of equal length, which can be regarded as being in the same plane, and the chlorine atoms are symmetrically distributed above and below the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593H01M10/0567
CPCY02E60/10
Inventor 刘建文陈建生彭劝李振民吴泽生尤雷周曦
Owner 湖北诺邦科技股份有限公司
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