Method for catalytically synthesizing hexachlorocyclotriphosphazene

A technology of hexachlorocyclotriphosphazene and a synthesis method is applied in the field of catalytic synthesis of hexachlorocyclotriphosphazene, and achieves the effects of reducing production cost, simple equipment, and reduced product yield and purity

Inactive Publication Date: 2009-12-16
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the use of ionic liquids to catalyze the synthesis of hexachlorocyclotriphosphazene has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 500mL three-neck flask equipped with a stirrer, thermometer, reflux condenser and hydrogen chloride gas absorption device, add 55.6g (0.2mol) tetrabutylammonium chloride, 2.7g (0.02mol) zinc chloride, and heat up to 100 React at ℃ for 1 hour to make an ionic liquid, then add 41.7g (0.2mol) of phosphorus pentachloride, 10.7g (0.2mol) of ammonium chloride, and 150ml of chlorobenzene, and keep it at 100℃~130℃ for 2 hours until no hydrogen chloride gas is released Afterwards, the material was cooled to 30° C., and the supernatant was separated. The ionic liquid phase of the lower layer continued to be used as a catalyst for the next reaction. Then, the supernatant was washed with water to neutrality, and chlorobenzene was evaporated under reduced pressure (recovery) to obtain a white Crystal, the yield is 96%, and the content of hexachlorocyclotriphosphazene is 91%.

Embodiment 2

[0024] In a 500mL three-necked flask equipped with a stirrer, thermometer, reflux condenser and hydrogen chloride gas absorption device, add 64.5g (0.2mol) tetrabutylammonium bromide, 2.7g (0.02mol) zinc chloride, and heat up to 80 React at ℃ for 1 hour to make an ionic liquid, then add 41.7g (0.2mol) of phosphorus pentachloride, 11.8g (0.22mol) of ammonium chloride, and 140ml of chlorobenzene, and keep it at 100℃~130℃ for 2 hours until no hydrogen chloride gas is released Afterwards, the material was cooled to 30° C., and the supernatant was separated. The ionic liquid phase of the lower layer continued to be used as a catalyst for the next reaction. Then, the supernatant was washed with water to neutrality, and chlorobenzene was evaporated under reduced pressure (recovery) to obtain a white Crystal, the yield is 96%, and the content of hexachlorocyclotriphosphazene is 90%.

Embodiment 3

[0026] Add 19.1g (0.2mol) of trimethylamine hydrochloride and 13.6g (0.1mol) of zinc chloride into a 500mL three-neck flask equipped with a stirrer, thermometer, reflux condenser and hydrogen chloride gas absorption device, and heat up to 120°C React for 2 hours to make an ionic liquid, then add 41.7g (0.2mol) of phosphorus pentachloride, 12.8g (0.24mol) of ammonium chloride, and 100ml of chlorobenzene, and maintain 100°C to 130°C for 2h until no hydrogen chloride gas is released. Afterwards, the material was cooled to below 60° C., filtered, and the ionic liquid solid residue was collected to continue to be used as a catalyst for the next reaction. Then, the filtrate was washed with water to neutrality, and chlorobenzene was evaporated under reduced pressure (recovery) to obtain white crystals with a yield of 95%. %, the content of hexachlorocyclotriphosphazene is 91%.

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Abstract

The invention discloses a method for catalytically synthesizing hexachlorocyclotriphosphazene. The method is characterized by comprising the following steps: taking raw materials according to a molar ratio that quaternary ammonium salt:anhydrous metal chloride:chlorobenzene:ammonium chloride:phosphorus pentachloride is 1-2:0.1-1:5-10:1-1.4:1; adding the quaternary ammonium salt and anhydrous metal chloride into a reactor to react by stirring for 1 to 2 hours at a temperature of between 80 and 120 DEG C to prepare ionic liquid; adding the chlorobenzene, the ammonium chloride and the phosphorus pentachloride into the reactor to react by stirring for 1 to 5 hours at a temperature of between 100 and 130 DEG C to obtain reaction mixed material; separating or / and filtering the reaction mixed material to separate the ionic liquid from chlorobenzene solution containing the reactant; and washing and distilling the chlorobenzene solution containing the reactant at reduced pressure to obtain the hexachlorocyclotriphosphazene product. The method has simple and safe operation and low cost, and is easy for industrial production and application.

Description

technical field [0001] The invention belongs to a preparation method of 1,3,5-triaza-2,4,6-triphosphazene compounds, and relates to a catalytic synthesis method of hexachlorocyclotriphosphazene. The hexachlorocyclotriphosphazene prepared by the method is suitable as the basic raw material for producing cyclophosphazene and polyphosphazene materials. Background technique [0002] Hexachlorocyclotriphosphazene, also known as trimeric phosphazene chloride, molecular formula: Cl 6 N 3 P 3 , Molecular weight: 347.66, as the basic raw material for the production of cyclophosphazene and polyphosphazene materials, it is a very important fine chemical intermediate, which plays a pivotal role in the development of phosphazene material chemistry. [0003] In the prior art, there are many preparation methods about hexachlorocyclotriphosphazene at home and abroad, wherein cheap ammonium chloride and phosphorus pentachloride are used as reaction raw materials, and chlorobenzene or symm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593B01J31/02
Inventor 黄杰唐安斌廖曦罗春明
Owner SICHUAN DONGFANG INSULATING MATERIAL
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