Synthesis method of hexafluorocyclotriphosphazene

A technology for hexafluorocyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of synthesis of hexafluorocyclotriphosphazene, can solve the problems of long reaction time and high reaction temperature, and achieves short reaction time, high purity, and secondary The effect of less product

Pending Publication Date: 2021-01-05
NANJING NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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The weak point of this method is: the temperature o

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  • Synthesis method of hexafluorocyclotriphosphazene
  • Synthesis method of hexafluorocyclotriphosphazene
  • Synthesis method of hexafluorocyclotriphosphazene

Examples

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Example Embodiment

[0032]Example 1

[0033]Put 104.3g of hexachlorocyclotriphosphazene, 113.3g of potassium fluoride, 0.011g of ionic liquid catalyst [Nbmm]OH, and 217.6g of anhydrous acetonitrile in a flask with electric stirrer, thermometer and reflux condenser at 30℃ The reaction was carried out under the conditions, the reaction was closed after 2h, filtered, and the filtrate was rectified to obtain hexafluorocyclotriphosphazene with a yield of 98.7%.

[0034]The liquid phase diagram of the raw material hexachlorocyclotriphosphazene is as followsfigure 1 As shown, the product liquid phase diagram and mass spectrum are asfigure 2 with3As shown, it shows that hexafluorocyclotriphosphazene has been synthesized.

Example Embodiment

[0035]Example 2

[0036]Put 104.3g hexachlorocyclotriphosphazene, 113.3g potassium fluoride, 0.011g ionic liquid catalyst [Nbmm]OH, 217.6 anhydrous acetonitrile in a flask with electric stirrer, thermometer and reflux condenser at 50℃. The reaction was carried out under the following conditions, the reaction was closed after 3h, filtered, and the filtrate was rectified to obtain hexafluorocyclotriphosphazene with a yield of 98.1%.

Example Embodiment

[0037]Example 3

[0038]Put 104.3g of hexachlorocyclotriphosphazene, 113.3g of potassium fluoride, 0.011g of ionic liquid catalyst [Nbmm]OH, 217.6g of 1,4-dioxane in a flask with electric stirrer, thermometer and reflux condenser In the medium, the reaction was carried out at 30°C, the reaction was closed after 2h, filtered, and the filtrate was rectified to obtain hexafluorocyclotriphosphazene with a yield of 86%.

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Abstract

The invention discloses a synthesis method of hexafluorocyclotriphosphazene, which comprises the following steps: dissolving hexachlorocyclotriphosphazene in an organic solvent, adding a fluorinatingagent and a catalyst, carrying out fluorination reaction, and rectifying to obtain the target product hexafluorocyclotriphosphazene. The synthesis method of hexafluorocyclotriphosphazene has the advantages of mild reaction temperature, simple and easy-to-operate process, high yield, short time consumption, high purity, greenness, economy and convenience in industrial production.

Description

technical field [0001] The invention belongs to the field of hexafluorocyclotriphosphazene, and in particular relates to a synthesis method of hexafluorocyclotriphosphazene. Background technique [0002] Phosphazene compounds are a kind of inorganic-organic hybrid compounds arranged alternately by P-N. Due to the good synergistic effect between phosphorus and nitrogen, phosphazene flame retardant has a high thermal decomposition temperature and flame retardant effect, and has less smoke and toxic gases. It is an environmentally friendly flame retardant material. Hexachlorocyclotriphosphazene is the most representative of phosphazene compounds, and the chlorine atom therein has high activity and is easily replaced by many nucleophiles. Therefore, hexachlorocyclotriphosphazene can be synthesized with various A functional group of phosphazene derivatives. Hexafluorocyclotriphosphazene is an important intermediate, and some of its derivatives are high-end flame retardants, whi...

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Application Information

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IPC IPC(8): C07F9/6593
CPCC07F9/65815Y02E60/10
Inventor 职慧珍何珍妮杨锦飞
Owner NANJING NORMAL UNIVERSITY
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