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Preparation method of hexafluorocyclotriphosphazene

A technology of hexafluorocyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of preparation of hexafluorocyclotriphosphazene, can solve the problems of unreachable product yield, low boiling point of cocatalyst, poor separation effect, etc., and achieve The effect of short preparation time, complete reaction and high product yield

Active Publication Date: 2021-06-22
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In CN105732718A, hexafluorocyclotriphosphazene was synthesized in a non-polar solvent using polyethylene glycol as a catalyst, but the reaction time was long and the reaction was not complete
However, there is still the defect that the cocatalyst has a low boiling point and poor separation effect from the product when post-processing the product, which leads to the failure of the product yield to achieve the optimal effect

Method used

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  • Preparation method of hexafluorocyclotriphosphazene

Examples

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Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: In a 2000mL three-neck flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 600g of n-hexane, cool down to 0°C, add 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, and stir evenly. 10 g of ethylene glycol monomethyl ether and 10 g of ethylene glycol monobutyl ether were added dropwise, and the temperature was raised to 50° C. for reaction, and then the temperature was lowered to 20° C. and kept for 1 hour of reaction. There is no hexachlorocyclotriphosphazene residue in the reaction solution, and the reaction is complete. 128 g of hexafluorocyclotriphosphazene were obtained by rectification, with a molar yield of 90.1%.

Embodiment 2

[0020] Example 2: In a 2000mL three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 400g of n-hexane, cool down to -10°C, add 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, and stir evenly , 16 g of ethylene glycol monomethyl ether and 24 g of ethylene glycol monobutyl ether were added dropwise, the temperature was raised to 52° C. for reaction, and then the temperature was lowered to 25° C. and kept for 2 hours for reaction. There is no hexachlorocyclotriphosphazene residue in the reaction solution, and the reaction is complete. 125 g of hexafluorocyclotriphosphazene was obtained by rectification, with a molar yield of 88.0%.

Embodiment 3

[0021] Example 3: In a 2000mL three-neck flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 500g of n-hexane, cool down to 20°C, add 200g of hexachlorocyclotriphosphazene and 200g of potassium fluoride, and stir evenly. 20 g of ethylene glycol monomethyl ether and 2 g of ethylene glycol monobutyl ether were added dropwise, and the temperature was raised to 30° C. for 2 hours to react. 50% of hexachlorocyclotriphosphazene remains in the reaction solution, and the reaction is not complete. Finally, rectification obtained 70 g of hexafluorocyclotriphosphazene with a molar yield of 49.3%. In this embodiment, the catalyst ratio is 1:0.1, although the reaction can be carried out, but the reaction is not complete, which is not preferred.

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Abstract

The invention discloses a preparation method of hexafluorocyclotriphosphazene, which comprises the steps of adding hexachlorocyclotriphosphazene and a fluorinating agent in a non-polar solvent in the presence of a catalyst, and carrying out a fluorination reaction to obtain the hexafluorocyclotriphosphazene, wherein the catalyst is a combined catalyst formed by ethylene glycol monomethyl ether and ethylene glycol monobutyl ether, the mass ratio of ethylene glycol monomethyl ether to ethylene glycol monobutyl ether is 1: (0.1-10), and the dosage of the combined catalyst is 0.1%-20% of the mass of hexachlorocyclotriphosphazene. The method has the advantages that the preparation time is short, the route is simple, the reaction is complete under the condition of proper proportion and dosage of the combined catalyst, and the boiling point of the combined catalyst is far higher than that of the product, so that the combined catalyst is easily separated from the product, and then the product is high in yield and high in purity.

Description

technical field [0001] The invention relates to a preparation method of hexafluorocyclotriphosphazene. Background technique [0002] Phosphazene compounds have excellent flame retardant properties, and hexafluorocyclotriphosphazene is an intermediate of many phosphazene compounds. The synthesis of hexafluorocyclotriphosphazene has a good application prospect. [0003] Hexafluorocyclotriphosphazene has the following structural formula: [0004] [0005] The synthesis of hexafluorocyclotriphosphazene is carried out in polar solvents, for example, in CN102757026A, KI is used as a catalyst to synthesize hexafluorocyclotriphosphazene in a polar solvent. Hexafluorocyclotriphosphazene is relatively active in polar solvents, and there are many side reactions when synthesizing other phosphazene derivatives. Therefore, it is best to synthesize hexafluorocyclotriphosphazene in non-polar solvents. [0006] In CN105732718A, hexafluorocyclotriphosphazene was synthesized in a non-pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593B01J31/02
CPCC07F9/65815B01J31/0204B01J35/0006
Inventor 陈晓华刘栋成刘磊卢云龙常楠陈晓龙
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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