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A kind of polycyclotriphosphazene-sulfone 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 field, can solve problems such as harsh processing and preparation techniques, and achieves high solid residue rate at high temperature and good polarity Solution solubility, high thermal decomposition temperature effect

Active Publication Date: 2016-04-13
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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  • A kind of polycyclotriphosphazene-sulfone phenyl ester and preparation method thereof
  • A kind of polycyclotriphosphazene-sulfone phenyl ester and preparation method thereof
  • A kind of polycyclotriphosphazene-sulfone phenyl ester and preparation method thereof

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Experimental program
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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 of sodium phenate (under nitrogen protection, 1.84g, 0.08mol of metal sodium and 7.52g, 0.08mol of phenol were 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);

[...

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 , 0.04mol sodium phenate (under nitrogen protection, 0.92g, 0.04mol metal sodium and 3.76g, 0.04mol phenol were reacted in 50mL tetrahydrofuran solution at 25°C for 2 hours to prepare 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);

[0034...

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 dropwise add the prepared 46.40g , 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, react 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~...

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Abstract

The invention relates to a polycyclotriphosphazene-sulfone phenyl ester and a preparation method thereof. The structural formula of the polycyclotriphosphazene-semiaryl ester is: wherein, R is, m=1-60. The polycyclotriphosphazene-sulfone phenyl ester of the present invention has good polar solution solubility, good flame retardancy, good thermal stability, high thermal decomposition temperature, high high-temperature solid residual rate, and POB polyphenylene ester Other similar excellent properties are mainly used in automotive engine parts, mechanical parts and aviation equipment parts, and provide new options for high-temperature solid lubricating materials for mechanical parts.

Description

Technical field [0001] The present invention involves a poly ring triangular-pyrodenate and its preparation method, which is a technical field of polymer materials. Background technique [0002] The special structure and superior performance of polyphoto and its derivatives determine its extensive research and application in many fields.At present, it is mainly concentrated in biomedical materials, flame retardant materials, membrane materials and electrolyte materials.The chemical structure of the important single of the polyphomo and its derivatives-hex chloride rings: [0003] [0004] Polyphenyl ester, also known as polyoxyzyl (POB), has excellent thermal stability, can be used for a long time at 315 ° C, and the short -term use temperature can be as high as 400 ° C.The best varieties of comprehensive performance such as performance, self -lubricating, hardness, electrical insulation, wear resistance, and abrasion resistance.At the same time, it has excellent dielectric str...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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