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Efficient flame retardant siloxy fluoro cyclotriphosphazene and synthesis method thereof

A technology of siloxy fluoro cyclotriphosphazene and fluoro cyclotriphosphazene, which is applied in the field of high-efficiency flame retardant siloxy fluoro cyclotriphosphazene and its synthesis, can solve the problem of not being able to completely prevent battery fire, Combustion or even explosion, inability to significantly improve the flash point of lithium-ion battery electrolyte, negative impact on lithium battery performance, etc., to improve battery capacity retention, facilitate industrial production, and improve cycle stability.

Inactive Publication Date: 2018-04-17
SHANDONG ZESHI NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, as flame retardant additives for lithium-ion battery electrolytes, the above-mentioned phosphazene derivatives have significant disadvantages
After research, it was found that hexaphenoxycyclotriphosphazene, hexamethoxycyclotriphosphazene, hexapropoxycyclotriphosphazene, 1-ethoxy-1,3,3,5,5-pentafluorocyclotriphosphazene Phosphazene cannot significantly increase the flash point of the lithium-ion battery electrolyte, and the flame-retardant temperature range is small, and the flame-retardant performance varies with temperature in a large range, so it cannot completely prevent the battery from igniting, burning or even explosion under the condition of abuse. some security issues
In addition, the addition of flame retardant additives will have a greater negative impact on the battery performance of lithium batteries

Method used

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  • Efficient flame retardant siloxy fluoro cyclotriphosphazene and synthesis method thereof
  • Efficient flame retardant siloxy fluoro cyclotriphosphazene and synthesis method thereof
  • Efficient flame retardant siloxy fluoro cyclotriphosphazene and synthesis method thereof

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Effect test

Embodiment 1

[0033] Dissolve 49.8g of hexafluorocyclotriphosphazene crystals in 200ml of tetrahydrofuran to form a hexafluorocyclotriphosphazene solution. Add 12.9g of potassium trimethylsiloxide to the solution, stir until uniform, and react at 10°C for 20h , After filtration and vacuum distillation, the phosphonitrile derivative siloxy fluorocyclotriphosphazene is obtained, which has the following structural formula:

[0034] The yield is 95%, and infrared is used to determine its structure, such as figure 1 Shown.

Embodiment 2

[0036] 49.8g of hexafluorocyclotriphosphazene crystals are dissolved in 300ml of n-hexane to form a hexafluorocyclotriphosphazene solution. Add 12.9g of potassium trimethylsiloxide to the solution, stir until uniform, and react for 10h at 40℃ After filtering and distillation under reduced pressure, the phosphonitrile derivative siloxy fluorocyclotriphosphazene is obtained with a yield of 96%.

Embodiment 3

[0038] 49.8g of hexafluorocyclotriphosphazene crystals are dissolved in 200ml of chlorobenzene to form a hexafluorocyclotriphosphazene solution. Add 12.9g of potassium trimethylsiloxide to the solution, stir until uniform, and react at 30°C After 15 hours, the phosphonitrile derivative siloxy fluorocyclotriphosphazene was obtained after filtration and distillation under reduced pressure with a yield of 95%.

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Abstract

The invention discloses an efficient flame retardant siloxy fluoro cyclotriphosphazene and a synthesis method thereof. The synthesis method comprises the following steps: dissolving fluorinated cyclotriphosphazene in an organic solvent, adding a siloxy compound, performing reaction for 0.5-72h, and replacing one fluorine atom with one siloxy so as to obtain the siloxy fluoro cyclotriphosphazene. The siloxy compound is potassium trimethylsilanolate or sodium trimethylsilanolate or lithium trimethylsilanolate. The synthesis method disclosed by the invention has mild reaction conditions and goodreaction controllability and is convenient for industrial production; and furthermore, technological processes are simple, reactants and solvents can be recycled, and the purity and yield of productsare higher.

Description

Technical field [0001] The invention relates to a high-efficiency flame retardant siloxy fluorocyclotriphosphazene and a synthesis method thereof. Background technique [0002] Phosphazene compounds are a kind of organic-inorganic hybrid compounds whose skeletons are alternately arranged by nitrogen and phosphorus, which can be divided into polyphosphazenes and cyclophosphazenes. Among them, chlorinated cyclotriphosphazene is the most representative compound among cyclophosphazene compounds. Due to the strong reactivity of chlorine atom, it is easily replaced by various nucleophiles. Therefore, using chlorocyclotriphosphazene as an intermediate, phosphazene derivatives with various organic functional groups can be synthesized. [0003] At present, the most studied phosphazene derivatives are: hexaphenylamino cyclotriphosphazene, hexaethylamino cyclotriphosphazene, hexafluorocyclotriphosphazene, hexaisopropoxy cyclotriphosphazene, hexamethoxy ring Triphosphazene, hexaethoxy cyclot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593H01M10/0567
CPCC07F9/65815H01M10/0567Y02E60/10
Inventor 周晓
Owner SHANDONG ZESHI NEW MATERIALS TECH CO LTD
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