Preparation method of intrinsic flame retardant polyphosphazene resin with high/low-temperature resistance and high performance

A high and low temperature resistant, polyphosphazene technology, applied in the field of intrinsic flame retardant polyphosphazene resin, can solve the problems of low flame retardant efficiency, limited amount of flame retardants, influence of additive performance, etc., to overcome inelasticity, volume Small size, the effect of expanding the operating temperature range

Inactive Publication Date: 2018-08-03
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The flame retardancy of traditional organic polymer materials is mainly achieved by adding flame retardants to the material. However, this method of flame retardancy has certain defects, such as the limitation of the amount of flame retardants added, and the dispersion of flame retardants in the material. properties, effects of additives on material properties, and low flame retardant efficiency

Method used

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  • Preparation method of intrinsic flame retardant polyphosphazene resin with high/low-temperature resistance and high performance
  • Preparation method of intrinsic flame retardant polyphosphazene resin with high/low-temperature resistance and high performance
  • Preparation method of intrinsic flame retardant polyphosphazene resin with high/low-temperature resistance and high performance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Under the protection of nitrogen, add tetrahydrofuran THF and sodium hydride to a flask connected with a condenser. Place ethanol in a constant pressure dropping funnel and add it dropwise to the flask. The molar ratio of sodium hydride to ethanol is 1.5:1 at room temperature. Stir until the ethanol is completely reacted to obtain a sodium ethoxide solution; under the protection of nitrogen, add THF as solvent and sodium hydride to a flask connected with a condenser, place phenol in a constant pressure dropping funnel and add dropwise to the flask, sodium hydride and The molar ratio of phenol is 1.5:1. Stir at room temperature until the phenol reaction is complete to obtain sodium phenolate solution; at room temperature, take the prepared sodium ethoxide solution and sodium phenate solution in a flask with a condenser. The molar ratio is 100:0, 75: 25, 50: 50, 25: 75, 0: 100; keep stirring, add the polydichlorophosphazene tetrahydrofuran solution through a constant pressu...

Embodiment 2

[0028] Under the protection of nitrogen, add THF and sodium hydride to a flask connected with a condenser. Place n-propanol in a constant pressure dropping funnel and add it dropwise to the flask. The molar ratio of sodium hydride to n-propanol is 1.5:1 , Stir at room temperature until the ethanol reaction is complete to obtain the sodium n-propoxide solution; under the protection of nitrogen, add the THF solvent and sodium hydride to the flask connected with the condenser, and place the phenol in a constant pressure dropping funnel and add dropwise to the flask , The molar ratio of sodium hydride to phenol is 1.5:1, stir at room temperature until the phenol reaction is complete to obtain sodium phenate solution; at room temperature, take the prepared sodium n-propoxide solution and sodium phenolate solution in a flask with a condenser, The molar ratios of sodium n-propoxide and sodium phenolate are 100:0,75:25,50:50,25:75,0:100 respectively; keep stirring, pass the tetrahydrofu...

Embodiment 3

[0031] Under the protection of nitrogen, add THF and sodium hydride to a flask connected with a condenser. Place n-butanol in a constant pressure dropping funnel and add it dropwise to the flask. The molar ratio of sodium hydride to n-butanol is 1.5:1 , Stir at room temperature until the n-butanol reaction is complete to obtain the sodium n-butoxide solution; under the protection of nitrogen, add the THF solvent and sodium hydride to the flask connected with the condenser, and place the phenol in a constant pressure dropping funnel and add dropwise In the flask, the molar ratio of sodium hydride to phenol is 1.5:1. Stir at room temperature until the phenol reaction is complete to obtain sodium phenolate solution; at room temperature, take the prepared sodium n-butoxide solution and sodium phenolate solution in a flask with a condenser Among them, the molar ratios of sodium n-butoxide and sodium phenolate are 100:0, 75:25, 50:50, 25:75, 0:100 respectively; keep stirring, pass the...

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Abstract

The invention discloses a preparation method of intrinsic flame retardant polyphosphazene resin with high / low-temperature resistance and high performance. According to the method, linear polydichlorophosphazene is subjected to co-substitution with two specific nucleophilic substitution reagents in the aspect of molecular design, separation, washing, purification, drying and other treatment are performed, and the intrinsic flame retardant polyphosphazene resin with high-temperature thermal stability and low-temperature flexibility is prepared. The high / low-temperature stability and elasticity of the intrinsic flame retardant polyphosphazene resin can be regulated by regulating the ratio of functionalized side groups. The scheme is as follows: phenoxyl and aliphatic straight-chain alkoxy indifferent molar ratios are used as the nucleophilic substitution reagents, tetrahydrofuran is taken as a reaction solvent, a reflux reaction is conducted at 60-70 DEG C for 36-48 h, a reaction mixtureis washed with deionized water and n-heptane 2-3 times, drying treatment is performed, and the intrinsic flame retardant polyphosphazene resin with high / low-temperature resistance and high performance is obtained. The resin has the Tg range of subzero 71.3 DEG C to subzero 7.1 DEG C, the maximum thermal weight loss temperature up to 530 DEG C and the residual rate up to 59.25%.

Description

Technical field [0001] The present invention prepares an intrinsic flame-retardant polyphosphazene resin with both high temperature thermal stability and low temperature flexibility. The thermal performance of this polyphosphazene resin can be adjusted by adjusting the content of functionalized side groups to obtain performance Controllable product. Background technique [0002] The main chain of alternating single and double bonds of linear polyphosphazene makes it have good flexibility and thermal stability. At the same time, the synergistic flame retardant effect of the phosphorus and nitrogen flame retardant elements contained in the main chain endows polyphosphazene with good flame retardancy. . Therefore, polyphosphazene is a potential intrinsic flame-retardant elastomer material. The main chain structure of polyphosphazene and the influence of a large number of side groups on its performance often play a decisive role in its application. Therefore, the introduction of f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/025
CPCC08G79/025
Inventor 王秀芬耿婷婷李双联蔡喜梅杨立鹏赵章启吴战鹏张立群
Owner BEIJING UNIV OF CHEM TECH
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