Polycyclotriphosphazene-sulphone phenyl ester and preparation method thereof

A technology of polycyclotriphosphazene and cyclotriphosphazene, which is applied in the field of polycyclotriphosphazene-sulfone phenyl ester and its preparation, can solve the problems of harsh processing and preparation technology, and achieve high temperature solid residual rate and good polarity The effect of solution solubility and high thermal decomposition temperature

Active Publication Date: 2014-02-12
IND RES INST ZHIJIANG COLLEGE OF ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] But for pure polyphenylene, its processing and preparation process is harsh, and it is insoluble in an

Method used

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  • Polycyclotriphosphazene-sulphone phenyl ester and preparation method thereof
  • Polycyclotriphosphazene-sulphone phenyl ester and preparation method thereof
  • Polycyclotriphosphazene-sulphone phenyl ester and preparation method thereof

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Example Embodiment

[0025] Example 1

[0026] The synthesis of the polycyclotriphosphazene-sulfone phenyl ester of the present invention is achieved through the following steps:

[0027] (1) In a 100mL three-necked flask equipped with magnetic rotor stirring, condenser and thermometer, 6.94g and 0.02mol of hexachlorocyclotriphosphazene prepared by multiple sublimation were dissolved in 50mL tetrahydrofuran solvent, and 9.28g prepared was added dropwise , 0.08mol sodium phenolate (prepared by reacting 1.84g, 0.08mol sodium metal and 7.52g, 0.08mol phenol in 50mL tetrahydrofuran solution at 25°C for 2 hours under nitrogen protection) tetrahydrofuran solution, nitrogen protection, reaction at 40°C for 12 hours . The tetrahydrofuran was removed by rotary distillation, washed with deionized water several times, and dried under vacuum at 50°C for 24 hours to obtain a milky white colloid, namely 2,4-dichlorotetraphenoxy cyclotriphosphazene; of which hexachlorocyclotriphosphazene and phenol The molar ratio...

Example Embodiment

[0031] Example 2

[0032] The synthesis of the polycyclotriphosphazene-sulfone phenyl ester of the present invention is achieved through the following steps:

[0033] (1) In a 100mL three-necked flask equipped with magnetic rotor stirring, condenser and thermometer, 3.47g and 0.01mol of hexachlorocyclotriphosphazene prepared by multiple sublimation were dissolved in 50mL tetrahydrofuran solvent, and 4.64g prepared was added dropwise , 0.04mol sodium phenolate (under nitrogen protection, 0.92g, 0.04mol metal sodium and 3.76g, 0.04mol phenol are reacted in 50mL tetrahydrofuran solution at 25°C for 2 hours to prepare a tetrahydrofuran solution, protected by nitrogen, and reacted at 40°C for 12 hours. The tetrahydrofuran was removed by rotary distillation, washed with deionized water several times, and dried under vacuum at 50°C for 24 hours to obtain a milky white colloid, namely 2,4-dichlorotetraphenoxy cyclotriphosphazene; of which hexachlorocyclotriphosphazene and phenol The mola...

Example Embodiment

[0037] Example 3

[0038] The synthesis of the polycyclotriphosphazene-sulfone phenyl ester of the present invention is achieved through the following steps:

[0039] (1) In a 100mL three-necked flask equipped with magnetic rotor stirring, condenser, and thermometer, 34.70g, 0.10mol of hexachlorocyclotriphosphazene prepared by multiple sublimation was dissolved in 50mL of tetrahydrofuran solvent, and 46.40g prepared was added dropwise. , 0.40mol sodium phenate (under nitrogen protection, 9.20g, 0.40mol sodium metal and 37.60g, 0.40mol phenol are prepared by reacting in 50mL tetrahydrofuran solution at 25°C for 2 hours) tetrahydrofuran solution, nitrogen protection, 40°C reaction 12 hour. The tetrahydrofuran was removed by rotary distillation, washed with deionized water several times, and dried under vacuum at 50°C for 24 hours to obtain a milky white colloid, namely 2,4-dichlorotetraphenoxy cyclotriphosphazene; of which hexachlorocyclotriphosphazene and phenol The molar ratio o...

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Abstract

The invention relates to polycyclotriphosphazene-sulphone phenyl ester and a preparation method thereof. The structural formula of the polycyclotriphosphazene-sulphone phenyl ester is as shown in the specification, wherein R in the structural formula is as shown in the descriptions, and m is equal to 1-60. The polycyclotriphosphazene-sulphone phenyl ester has good polarity solution dissolving property, good flame retardant property, relatively good thermal stability, high thermal decomposition temperature, high residual rate of high-temperature solids and other excellent properties similar to those of POB polybenzoate, is mainly applied to automotive engine components, mechanical components and aeronautical facility components and provides a new choice for high-temperature solid lubrication materials for mechanical components and parts.

Description

technical field [0001] The invention relates to a polycyclotriphosphazene-sulfone phenyl ester and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] The special structure and superior performance of polyphosphazene and its derivative materials determine its extensive research and application in many fields. At present, it mainly focuses on biomedical materials, flame retardant materials, membrane materials and electrolyte materials. The chemical structural formula of hexachlorocyclotriphosphazene, an important monomer of polyphosphazene and its derivatives, is: [0003] [0004] Polyphenylene, also known as polyoxybenzoyl (POB), has excellent thermal stability. It can be used at 315°C for a long time, and the short-term use temperature can be as high as 400°C. It is the most thermally stable polymer material known so far. The variety with the best comprehensive properties such as thermal resistance, heat c...

Claims

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Application Information

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IPC IPC(8): C08G63/692C08G63/78C07F9/6593
Inventor 赵正平计建炳
Owner IND RES INST ZHIJIANG COLLEGE OF ZHEJIANG UNIV OF TECH
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