Method for preparing phosphaphenanthrene and phosphazene halogen-free retardant agent

A technology of miscellaneous phenanthrene phosphazene and flame retardant, which is applied in the field of preparation of phosphorus-nitrogen additive flame retardants, can solve problems such as non-existence, and achieve high yield, high preparation efficiency, and high purity

Inactive Publication Date: 2011-03-30
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Except the applicant's report, there is no report about the synthesis and patent of phosphaphenanthrene-yl phosphazene derivatives at home and abroad that are six-(phosphaphenanthrene-hydroxymethyl-phenoxy)-cyclic triphosphazene

Method used

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  • Method for preparing phosphaphenanthrene and phosphazene halogen-free retardant agent
  • Method for preparing phosphaphenanthrene and phosphazene halogen-free retardant agent

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Example 1 Heat 18g of DOPO to 130°C, add 4g of hexa(4-formyl-phenoxy)-cyclotriphosphazene, and melt for 10 hours; after the reaction is completed, cool down to 120°C, and add 12g of xylene as a washing solvent while stirring , the holding temperature is 100°C, stirred for 3 hours, filtered the white powder with a Buchner funnel, added the same amount of xylene and washed it repeatedly for 3 times, after the white powder was obtained, it was dried at 80°C, and the final product hexa-(phosphora The phenanthrene-hydroxymethyl-phenoxy)-cyclotriphosphazene powder was 11.88g, the yield was 99.0%, and the purity was 99.2%.

Embodiment 2

[0016] Example 2 Heat 12g of DOPO to 160°C, add 4g of hexa(4-formyl-phenoxy)-cyclotriphosphazene, and melt for 5 hours; after the reaction is completed, cool down to 100°C, and add 24g of toluene as a washing solvent while stirring, The heat preservation temperature was 100°C, stirred for 3 hours, filtered the white powder with a Buchner funnel, repeated washing 4 times, after the white powder was obtained, dried at 80°C, and the final product hexa-(phosphaphenanthrene-hydroxymethyl-benzene Oxygen)-cyclotriphosphazene was 11.82 g of powder, with a yield of 98.5% and a purity of 99.1%.

Embodiment 3

[0017] Example 3 Heat 180g of DOPO to 160°C, add 40g of hexa(4-formyl-phenoxy)-cyclotriphosphazene, and melt for 12 hours; after the reaction is completed, cool down to 130°C, and add 180g of chlorobenzene as a washing solvent while stirring , the holding temperature was 110°C, stirred for 1 hour, filtered the white powder with a Buchner funnel, repeated washing 3 times in the same way, after the white powder was obtained, dried at 80°C, and the final product hexa-(phosphaphenanthrene-hydroxyl Methyl-phenoxy)-cyclotriphosphazene was 119.04 g of powder, with a yield of 99.2% and a purity of 99.3%.

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Abstract

The invention relates to a method for preparing a phosphaphenanthrene and phosphazene halogen-free retardant agent hexa-(phosphaphenanthrene-hydroxymethyl-phenoxyl)-cyclotriphosphazene. The structural formula of the hexa-(phosphaphenanthrene-hydroxymethyl-phenoxyl)-cyclotriphosphazene is shown in a figure 1. The hexa-(phosphaphenanthrene-hydroxymethyl-phenoxyl)-cyclotriphosphazene is prepared through a fusion addition reaction on hexa(4-formyl-phenoxyl)-cyclotriphosphazene and a compound of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), and is purified by adopting an organic solvenet washing method to obtain the white powder of the hexa-(phosphaphenanthrene-hydroxymethyl-phenoxyl)-cyclotriphosphazene with high purity and high yield.

Description

(1) Technical field [0001] The invention belongs to the technical field of a preparation process of a phosphorus-nitrogen additive flame retardant. The invention relates to a preparation method of hexa-(phosphaphenanthrene-hydroxymethyl-phenoxy)-cyclotriphosphazene with two kinds of flame retardant elements, phosphorus and nitrogen. (2) Background technology [0002] Hexa-(phosphaphenanthrene-hydroxymethyl-phenoxy)-cyclotriphosphazene is an additive phosphorus nitrogen flame retardant with a phosphorus content of 12.93% and a nitrogen content of 1.95%, which can be used as a flame retardant additive for Epoxy resin, polyester, polyolefin and other polymer materials, coatings and special engineering plastics. [0003] Since the 1980s, foreign countries have begun to study phosphazene derivatives, which have developed rapidly due to the proposal of halogen-free flame retardant in recent years. Professor Allcock of the University of Pennsylvania synthesized six (4-formylpheno...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593
Inventor 钱立军郭秀安叶龙健
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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