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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 any organic solvent, so it can only be prepared by cold pressing sintering and high temperature molding process.

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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Effect test

Embodiment 1

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

[0027] (1) In a 100mL three-neck flask equipped with a magnetic rotor stirring, a condenser, and a thermometer, dissolve 6.94g and 0.02mol of hexachlorocyclotriphosphazene prepared by multiple sublimation in 50mL of tetrahydrofuran solvent, and add dropwise 9.28g of the prepared , 0.08mol sodium phenate (under nitrogen protection, 1.84g, 0.08mol metal sodium and 7.52g, 0.08mol phenol reacted in 50mL tetrahydrofuran solution at 25°C for 2 hours) tetrahydrofuran solution, under nitrogen protection, reacted at 40°C for 12 hours . Remove tetrahydrofuran by rotary distillation, wash with deionized water several times, and dry in vacuum at 50°C for 24 hours to obtain a milky white colloid, namely 2,4-dichlorotetraphenoxycyclotriphosphazene; where hexachlorocyclotriphosphazene and phenol The molar ratio of sodium is 1: (3.9~4.1);

[0028] (2) In a...

Embodiment 2

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

[0033] (1) In a 100mL three-neck flask equipped with a magnetic rotor stirring, a condenser, and a thermometer, dissolve 3.47g, 0.01mol of hexachlorocyclotriphosphazene prepared by multiple sublimation in 50mL of tetrahydrofuran solvent, and add dropwise 4.64g of the prepared , 0.04 mol of sodium phenate (under nitrogen protection, 0.92 g, 0.04 mol of metal sodium and 3.76 g, 0.04 mol of phenol were reacted in 50 mL of tetrahydrofuran solution at 25 ° C for 2 hours to prepare a tetrahydrofuran solution, under nitrogen protection, reacted at 40 ° C for 12 hours. Remove tetrahydrofuran by rotary distillation, wash with deionized water several times, and dry in vacuum at 50°C for 24 hours to obtain a milky white colloid, namely 2,4-dichlorotetraphenoxycyclotriphosphazene; where hexachlorocyclotriphosphazene and phenol The molar ratio of sodium i...

Embodiment 3

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

[0039] (1) In a 100mL three-necked flask equipped with a magnetic rotor stirring, a condenser, and a thermometer, dissolve 34.70g and 0.10mol of hexachlorocyclotriphosphazene prepared by multiple sublimation in 50mL of tetrahydrofuran solvent, and add dropwise 46.40g of the prepared , 0.40mol of sodium phenate (prepared by reacting 9.20g, 0.40mol of sodium metal and 37.60g, 0.40mol of phenol in 50mL of tetrahydrofuran solution at 25°C for 2 hours under nitrogen protection) tetrahydrofuran solution, under nitrogen protection, reacted at 40°C for 12 Hour. Remove tetrahydrofuran by rotary distillation, wash with deionized water several times, and dry in vacuum at 50°C for 24 hours to obtain a milky white colloid, namely 2,4-dichlorotetraphenoxycyclotriphosphazene; where hexachlorocyclotriphosphazene and phenol The molar ratio of sodium is 1: (3...

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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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