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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

AI Technical Summary

Problems solved by technology

The weak point of this method is: the temperature of reaction is higher, and the reaction time is long

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 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 equipped with an electric stirrer, a thermometer, and a reflux condenser, at 30°C The reaction was carried out under the conditions, the reaction was closed after 2 hours, the filtrate was filtered, and the filtrate was rectified to obtain hexafluorocyclotriphosphazene with a yield of 98.7%.

[0034] Wherein the liquid phase diagram of the hexachlorocyclotriphosphazene of raw material is as figure 1 As shown, the liquid phase diagram and mass spectrum of the product are shown as figure 2 with 3 As shown, it shows that hexafluorocyclotriphosphazene has been synthesized.

Embodiment 2

[0036] 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 equipped with an electric stirrer, a thermometer, and a reflux condenser, at 50°C After 3 hours, the reaction was closed, the filtrate was filtered, and the filtrate was rectified to obtain hexafluorocyclotriphosphazene with a yield of 98.1%.

Embodiment 3

[0038] 104.3g of hexachlorocyclotriphosphazene, 113.3g of potassium fluoride, 0.011g of ionic liquid catalyst [Nbmm]OH, 217.6g of 1,4-dioxane are placed in a flask with an electric stirrer, a thermometer, and a reflux condenser reaction at 30° C., shut down the reaction after 2 hours, filter, and rectify the filtrate 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...

Claims

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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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