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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, can not significantly improve the flash point of lithium-ion battery electrolyte, negative impact on lithium battery performance, etc., to achieve good thermal stability, radiation resistance and weather resistance, easy industrial production, and good reaction controllability.

Active Publication Date: 2017-10-27
SHANDONG UNIV
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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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[0027] The invention provides a method for synthesizing siloxyfluorocyclotriphosphazene, and the prepared siloxyfluorocyclotriphosphazene is used in high-performance lithium-ion battery electrolyte additives.

[0028] In the siloxy fluorocyclotriphosphazene compound, the substitution of the siloxy group can be mono-substituted, partially substituted or fully substituted.

[0029] The present invention also provides a synthetic method of siloxyfluorocyclotriphosphazene, comprising the following steps:

[0030] Dissolving the fluorinated cyclotriphosphazene in an organic solvent, adding a siloxy compound, selecting a catalyst, reacting for 0.5-72 hours, replacing the fluorine atom with a siloxy group to obtain a siloxyfluorocyclotriphosphazene.

[0031] Preferably, the siloxy compound is potassium trimethylsiliconate, sodium trimethylsiliconate or lithium trimethylsiliconate. It has been verified by experiments that the siloxylation effect of these three siloxy compounds is bet...

Embodiment 1

[0047] 49.8g of hexafluorocyclotriphosphazene crystals are dissolved in 200ml of tetrahydrofuran to form a hexafluorocyclotriphosphazene solution, and 12.9g of potassium trimethylsiliconate and a small amount of graphene are added to the solution as a catalyst, stirred until uniform, and in 10 React for 20 hours at ℃, filter and distill under reduced pressure to obtain the phosphazene derivative siloxyfluorocyclotriphosphazene, which has the following structural formula, with a yield of 95%, and its structure is determined by infrared, as shown in figure 1 shown.

Embodiment 2

[0049] 49.8g of hexafluorocyclotriphosphazene crystals were dissolved in 300ml of n-hexane to form a hexafluorocyclotriphosphazene solution, and 12.9g of potassium trimethylsiliconate and an appropriate amount of Raney nickel were added to the solution as a catalyst, stirred until uniform, and React at 40°C for 10 hours, filter and distill under reduced pressure to obtain the phosphazene derivative, siloxyfluorocyclotriphosphazene, with a yield of 96%.

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Abstract

The invention discloses an efficient flame retardant siloxy fluoro-cyclotriphosphazene and a synthesis method thereof. Fluoro-cyclotriphosphazene is dissolved into an organic solvent, and a siloxy compound and a catalyst are added to perform a reaction for 0.5-72h to replace fluorine atoms by siloxy to obtain siloxy fluoro-cyclotriphosphazene, wherein the siloxy compound is potassium trimethylsilanolate, sodium trimethylsilanolate or lithium trimethylsilanolate. The adopted synthesis method is mild in reaction conditions, high in reaction controllability and capable of realizing industrial production conveniently; and in addition, the technological process is simple, the reactants and the solvent can be recycled, and the product purity and yield are relatively high.

Description

technical field [0001] The invention belongs to the field of lithium ion batteries, and in particular relates to a high-efficiency flame retardant siloxyfluorocyclotriphosphazene and a synthesis method thereof. Background technique [0002] Phosphazene compounds are a class of organic-inorganic hybrid compounds whose skeletons are alternately arranged with nitrogen and phosphorus, and can be divided into polyphosphazenes and cyclic phosphazenes. Among them, chlorocyclotriphosphazene is the most representative compound among cyclophosphazene compounds, because the chlorine atom has a strong reactivity and 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 more researched phosphazene derivatives are: hexaanilinocyclotriphosphazene, hexaethylaminocyclotriphosphazene, hexafluorocyclotriphosphazene, hexaisopropoxycycl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0567H01M10/0525
CPCH01M10/0525H01M10/0567Y02E60/10
Inventor 冯金奎安永灵
Owner SHANDONG UNIV
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