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Nitropolyphenoxyphosphazene and its preparation method

A technology of nitropolyphenoxyphosphazene and polyphenoxyphosphazene is applied in the field of polyphosphazene flame retardant and its preparation, which can solve the problems of low carbon residue, poor stability and the like, and achieve the improvement of nitrogen content, The effect of low cost and simple preparation process

Inactive Publication Date: 2017-09-22
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, polyphenoxyphosphazene still has the disadvantages of poor stability at high temperature and low carbon residue.

Method used

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  • Nitropolyphenoxyphosphazene and its preparation method
  • Nitropolyphenoxyphosphazene and its preparation method
  • Nitropolyphenoxyphosphazene and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] First take by weighing 35g of nitric acid (concentration is 65%, 0.36mol) with Erlenmeyer flask, then slowly add 24g of sulfuric acid (concentration is 98%, 0.24mol) while stirring under the condition of ice-water bath, mix well. Add 3.5 g of polyphenoxyphosphazene to a 100 ml three-neck flask equipped with a stirring paddle and a reflux condensing device, and the polyphenoxyphosphazene was purchased from Beijing Xinhui Technology Co., Ltd. Under the condition of ice-water bath, slowly add the mixed acid into the three-necked flask, nitric acid: polyphenoxyphosphazene = 10:1. The reaction temperature is maintained at 30°C. After 4 hours of reaction, wash with sodium hydroxide solution to pH = 7.0, then wash with distilled water until the color of the solution is colorless and transparent, and then filter and dry to obtain white powdery nitropolyphenylene oxide. Phosphazene 3.89g.

[0030] It can be seen from the infrared spectrum of nitropolyphenoxyphosphazene that 127...

Embodiment 2

[0032] First take by weighing 35g of nitric acid (concentration is 65%, 0.36mol) with Erlenmeyer flask, then slowly add 24g of sulfuric acid (concentration is 98%, 0.24mol) while stirring under the condition of ice-water bath, mix well. Add 3.5 g of polyphenoxyphosphazene to a 100 ml three-neck flask equipped with a stirring paddle and a reflux condensing device, and the polyphenoxyphosphazene was purchased from Beijing Xinhui Technology Co., Ltd. Under the condition of ice-water bath, slowly add the mixed acid into the three-necked flask, nitric acid: polyphenoxyphosphazene = 10:1. The reaction temperature is maintained at 40°C. After 4 hours of reaction, wash with sodium hydroxide solution to pH = 7.0, then wash with distilled water until the color of the solution is colorless and transparent, and then filter and dry to obtain white powdery nitropolyphenylene oxide. Phosphazene 4.19g.

Embodiment 3

[0034] First take by weighing 35g of nitric acid (concentration is 65%, 0.36mol) with Erlenmeyer flask, then slowly add 24g of sulfuric acid (concentration is 98%, 0.24mol) while stirring under the condition of ice-water bath, mix well. Add 3.5 g of polyphenoxyphosphazene to a 100 ml three-neck flask equipped with a stirring paddle and a reflux condensing device, and the polyphenoxyphosphazene was purchased from Beijing Xinhui Technology Co., Ltd. Under the condition of ice-water bath, slowly add the mixed acid into the three-necked flask, nitric acid: polyphenoxyphosphazene = 10:1. The reaction temperature is maintained at 50°C. After 4 hours of reaction, wash with sodium hydroxide solution to pH = 7.0, then wash with distilled water until the color of the solution is colorless and transparent, and then filter and dry to obtain white powdery nitropolyphenylene oxide. Phosphazene 4.21g.

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Abstract

The invention discloses a fire retardant nitro poly(bisphenoxy)phosphazene and a preparation method therefor. The preparation method comprises the following steps: uniformly mixing 98% concentrated sulfuric acid and 65% nitric acid in the molar ratio of 1: 0.5 to 1: 7.5 under the condition of an ice-water bath, adding the mixture into poly(bisphenoxy)phosphazene under room temperature, and reacting in a reactor with a condensation circulator, wherein the mass ratio of the nitric acid to the poly(bisphenoxy)phosphazene is (1-10): 1; controlling the reaction temperature to be 20-80 DEG C and the reaction time to be 15 minutes to 10 hours; washing with aqueous alkali until the pH is 7.0 after the reaction is ended, then continuing washing with distilled water or ethanol water, and finally performing suction filtration drying treatment so as to obtain a product. The nitrogen content of the nitro poly(bisphenoxy)phosphazene prepared by the invention is obviously improved, the synergist flame resistant effect of nitrogen and phosphorous elements is good, a good flame resistant effect can be achieved even if the additive amount of flame resistant agent is small, and an obvious expansion effect is achieved during flame resistance.

Description

technical field [0001] The invention relates to the field of flame retardants in engineering plastics, in particular to a polyphosphazene flame retardant and a preparation method thereof. Background technique [0002] Flame retardants are often added to engineering plastics. Due to environmental requirements, halogen-free flame retardants have become a hot spot in the field of flame retardant development and application research. In terms of halogen-free flame retardant modification, flame retardants are mainly achieved through phosphorus-based flame retardants, boron-based flame retardants, aromatic sulfonate flame retardants and silicon-based flame retardants. Phosphazene flame retardant is an environmentally friendly flame retardant product. Phosphazenes are mainly divided into cyclophosphazenes and polyphosphazenes. Cyclotriphosphazenes are gradually being used in flame retardant research because of their unique high stability phosphorus-nitrogen alternating arrangement...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04C08L85/02C08L69/00
Inventor 蔡绪福杨云云曹席磊王有川
Owner SICHUAN UNIV
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