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Synthesis method of fluorocyclotriphosphazene

A technology of fluorocyclotriphosphazene and synthesis method, which is applied in the field of synthesis of fluorocyclotriphosphazene, can solve the problems of reducing the speed of fluorocyclotriphosphazene and fluorine salt, high catalyst cost, harmful to human body, etc., and achieves Good controllability of the reaction, the effect of increasing the speed of the fluorination reaction and increasing the yield

Active Publication Date: 2016-07-06
SHANDONG ZESHI NEW MATERIALS TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis of fluorocyclotriphosphazene is mainly carried out by fluorination reaction of fluorocyclotriphosphazene and fluorine salt, and the yield is low. The catalysts mainly include tetramethylammonium chloride, tetramethylammonium bromide and 18 -Crown-6 and phosphonium bromide, but these catalysts are costly and harmful to the human body; if no catalyst is added, the speed of the fluorination reaction of fluorocyclotriphosphazene and fluoride salt is greatly reduced

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 34.7g of hexachlorocyclotriphosphazene crystals are dissolved in 200ml of tetrahydrofuran to form a hexachlorocyclotriphosphazene solution, 27g of sodium fluoride is added to the solution as a fluorinating agent, and 2g of polyethylene glycol monomethyl ether 800 is added as a catalyst. And react at 30° C. for 1 h, filter and distill under reduced pressure to obtain the phosphazene derivative hexafluorocyclotriphosphazene with a yield of 99%.

Embodiment 2

[0022] 34.7g of hexachlorocyclotriphosphazene crystals are dissolved in 300ml of n-hexane to form a hexachlorocyclotriphosphazene solution, 28g of sodium fluoride is added as a fluorinating agent in the solution, 0.6g of polyethylene glycol 5000 is added as a catalyst, and React at 60° C. for 10 h, filter and distill under reduced pressure to obtain the phosphazene derivative hexafluorocyclotriphosphazene with a yield of 94%.

Embodiment 3

[0024] Dissolve 40g of ethoxypentachlorocyclotriphosphazene crystals in 200ml of toluene to form an ethoxylated pentachlorocyclotriphosphazene solution, add 35g of sodium fluoride to the solution as a fluorinating agent, and add 8g of polyethylene glycol dimethyl Ether 200 was used as a catalyst, and reacted at a temperature of 90°C for 4 hours. After filtration and vacuum distillation, the phosphazene derivative ethoxypentafluorocyclotriphosphazene was obtained with a yield of 92%.

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Abstract

The invention discloses a synthesis method of fluorocyclotriphosphazene. The synthesis method includes: dissolving chlorocyclotriphosphazene in an organic solvent; adding a fluorinating agent and a catalyst for reaction for 1-20 h to obtain fluorocyclotriphosphazene. The catalyst accounts for 1-20% of total mass of raw materials and is polyethylene glycol, methoxypolyethylene glycol or polyethylene glycol dimethyl ether.Polyethylene glycol, methoxypolyethylene glycol or polyethylene glycol dimethyl ether is used as the catalyst and is nontoxic, low in price and high in catalytic capability; using of polyethylene glycol, methoxypolyethylene glycol or polyethylene glycol dimethyl ether can greatly increase fluorinating reaction speed and lower cost. Polyethylene glycol, methoxypolyethylene glycol or polyethylene glycol dimethyl ether is used, yield of synthetic fluorocyclotriphosphazene is increased, and yield is higher than 92% and is up to 99% maximumly.

Description

technical field [0001] The invention relates to a method for synthesizing fluorocyclotriphosphazene. 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. Among them, chlorocyclotriphosphazene is the most representative compound among cyclophosphazene compounds, because the chlorine atom has a strong activity, it is easy to be replaced by various nucleophiles. Therefore, using chlorocyclotriphosphazene as an intermediate, phosphazene derivatives with various organic functional groups can be synthesized. Chlorine atoms have poor compatibility in lithium battery electrolytes, while fluorocyclotriphosphazenes have good electrochemical compatibility. [0003] At present, the synthesis of fluorocyclotriphosphazene is mainly carried out by fluorination reaction of fluorocyclotriphosphazene and fluori...

Claims

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Application Information

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IPC IPC(8): C07F9/6593H01M10/056
CPCC07F9/65814H01M10/056Y02E60/10
Inventor 冯金奎安永灵
Owner SHANDONG ZESHI NEW MATERIALS TECH CO LTD
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