A kind of preparation method of highly flame-retardant cross-linked polyphosphazene elastomer

An elastomer, polyphosphazene technology, applied in fire-resistant coatings and other directions, can solve the problems affecting polyphosphazene, flame retardancy, thermal stability reduction, etc., and achieve strong steric hindrance effect, excellent flame retardancy, and large volume. Effect

Active Publication Date: 2021-04-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polyphosphazene elastomer prepared by the chemical crosslinking method has a stable structure and good crosslinking effect, but the introduction of functionalized side groups and crosslinking agents often affects the performance of polyphosphazene, making it have certain flame retardancy and thermal stability. reduced degree

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0015] Take 0.72mol of sodium hydride, 0.1molg of ethylene glycol, 0.5mol of phenol, and 0.1mol of hexachlorocyclotriphosphazene (molar ratio 7.2:1:5:1), and use tetrahydrofuran as a solvent to configure a corresponding solution, and the sodium hydride solution Put it in a three-necked flask, protect it with nitrogen gas, under the condition of ice-water bath, drop ethylene glycol and phenol solution into the sodium hydride solution drop by drop at constant pressure, react until the system changes from turbid liquid to clear, and then add hexachlorocyclotri The phosphazene solution was dripped into the reaction system drop by drop at constant pressure. After reacting for 4 hours, the reaction solution was poured out. After standing still, the layers were separated. The lower layer was milky white impurities, and the upper layer was light yellow hydroxyethoxyphenoxycyclotriphosphazene solution. Separate the supernatant for later use; take 100.0g of hexachlorocyclotriphosphazene,...

Embodiment example 2

[0017] Take 1.44mol of sodium hydride, 0.2mol of ethylene glycol, 1.0mol of phenol, and 0.2mol of hexachlorocyclotriphosphazene (molar ratio 7.2:1:5:1), and use tetrahydrofuran as a solvent to configure a corresponding solution, and the sodium hydride solution Put it in a three-necked flask, protect it with nitrogen gas, under the condition of ice-water bath, drop ethylene glycol and phenol solution into the sodium hydride solution drop by drop at constant pressure, react until the system changes from turbid liquid to clear, and then add hexachlorocyclotri The phosphazene solution was dripped into the reaction system drop by drop at constant pressure. After reacting for 8 hours, the reaction solution was poured out. After standing still, the layers were separated. The lower layer was milky white impurities, and the upper layer was light yellow hydroxyethoxyphenoxycyclotriphosphazene solution. Separate the supernatant for later use; take 200.0 g of hexachlorocyclotriphosphazene,...

Embodiment example 3

[0019]Take 1.44mol of sodium hydride, 0.2mol of ethylene glycol, 1.0mol of phenol, and 0.2mol of hexachlorocyclotriphosphazene (molar ratio 7.2:1:5:1), and use tetrahydrofuran as a solvent to configure a corresponding solution, and the sodium hydride solution Put it in a three-necked flask, protect it with nitrogen gas, under the condition of ice-water bath, drop ethylene glycol and phenol solution into the sodium hydride solution drop by drop at constant pressure, react until the system changes from turbid liquid to clear, and then add hexachlorocyclotri The phosphazene solution was dripped into the reaction system drop by drop at constant pressure. After reacting for 6 hours, the reaction solution was poured out. After standing still, the layers were separated. The lower layer was milky white impurities, and the upper layer was light yellow hydroxyethoxyphenoxycyclotriphosphazene solution. Separate the supernatant for later use; take 200.0 g of hexachlorocyclotriphosphazene, ...

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Abstract

The invention discloses a preparation method of a high-flame-retardant cross-linked polyphosphazene elastomer. The technical scheme specifically comprises the following steps: performing a substitution reaction process on ethylene glycol monosodium, sodium phenolate and hexachlorocyclotriphosphazene under an ice bath condition and nitrogen protection to prepare hydroxyethyl phenoxy cyclotriphosphazene, and performing a substitution reaction process on ethoxy phenoxy cyclotriphosphazene sodium, sodium phenolate and polydichlorophosphazene to prepare the ethoxy phenoxy cyclotriphosphazene phenoxy polyphosphazene elastomer. The ethoxyphenoxy cyclotriphosphazene substituent synthesized in the scheme is large in volume, strong in steric effect and high in phosphorus and nitrogen element content, the polyphosphazene elastomer can be used as the cross-linking point of phosphazene chain segment entanglement, such that the product has advantages of excellent flame retardancy, excellent thermalstability and excellent mechanical property while the room temperature cross-linking is achieved, the synthesis process of the high-flame-retardant high-performance polyphosphazene elastomer is effectively optimized, and the important significance is provided for the low-cost and large-scale industrial production of the high-performance cross-linked polyphosphazene elastomer.

Description

Technical field: [0001] The invention prepares a highly flame-retardant crosslinked polyphosphazene elastomer, which has excellent flame retardancy and heat resistance, and can form a crosslinked structure at room temperature without adding a crosslinking agent. The production process of the flame-retardant polyphosphazene elastomer can be effectively simplified and the production cost thereof can be reduced. Background technique: [0002] Polyphosphazene and its derivatives have a stable main chain structure, a synergistic flame-retardant effect, many types of side chains, and good functionality. They have outstanding advantages in high flame-retardant and high-performance polymer materials. As an elastomer material, polyphosphazene needs to achieve a certain degree of cross-linking in order to have mechanical characteristics such as resilience. At present, the common cross-linking method of polyphosphazene is chemical cross-linking method. By introducing functionalized si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/025C09K21/14
CPCC08G79/025C09K21/14
Inventor 王秀芬周克亮赵媛西李妍
Owner BEIJING UNIV OF CHEM TECH
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