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Preparation method of phosphonitrile flame retardant

The technology of a phosphazene flame retardant, hexachlorocyclotriphosphazene, is applied in the field of preparing materials by chemical synthesis methods, and achieves the effect of reducing the number of emissions

Inactive Publication Date: 2012-07-25
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] As an environmentally friendly flame retardant product, phosphazene flame retardants have developed rapidly in recent years, among which hexaphenoxycyclotriphosphazene can be used in the commercial field at present, and domestic and foreign companies are concerned about the flame retardant series of phosphazenes A large number of patents have been applied for the preparation and application of flame retardants. In the above application materials, hexa-(aldehyde phenoxy)-cyclotriphosphazene series flame retardants and other rings containing aldehyde phenoxy groups have not been used. Triphosphazene included in its patent protection scope

Method used

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  • Preparation method of phosphonitrile flame retardant
  • Preparation method of phosphonitrile flame retardant
  • Preparation method of phosphonitrile flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 Add 348g of hexachlorocyclotriphosphazene and 805g of p-hydroxybenzaldehyde into 2000g of toluene, add 7g of tetramethylammonium bromide, keep the reaction temperature at 108°C under stirring conditions, react for 24 hours, and add alkali to the reaction system Stir the water for washing, keep the temperature at 80°C, wash for 0.5 hours, let stand to separate, remove the water layer, add 300g of water to the organic phase for washing, keep the temperature at 80°C, wash for 0.5 hours, let stand to separate, remove the water layer, washed with water three times repeatedly, and the organic solvent was distilled off to obtain 848.9 g of product HAP with a purity of 98.6%.

Embodiment 2

[0018] Example 2 Add 348g of hexachlorocyclotriphosphazene and 805g of p-hydroxybenzaldehyde into 2000g of chlorobenzene, add 7g of tetramethylammonium bromide, keep the reaction temperature at 130°C under stirring conditions, react for 24 hours, and add Wash with alkaline water, keep the temperature at 80°C, wash for 0.5 hours, let stand to separate, remove the water layer, add 600g of water to the organic phase for washing, keep the temperature at 80°C, wash for 0.5 hours, let stand to separate, remove After the aqueous layer was washed with water three times, the organic solvent was distilled off to obtain 852.4 g of product HAP with a purity of 99.0%.

Embodiment 3

[0019] Example 3 Add 348g of hexachlorocyclotriphosphazene, 610g of p-hydroxybenzaldehyde, and 103g of phenol into 2000g of toluene, add 15g of tetraethylammonium bromide, keep the reaction temperature at 108°C under stirring conditions, and react for 24 hours. Add alkaline water and stir to wash, keep the temperature at 80°C, wash for 0.5 hours, let stand to separate, remove the water layer, add 500g water to the organic phase to wash, keep the temperature at 80°C, wash for 0.5 hours, let stand and separate , after removing the water layer, repeated washing with water 3 times, and distilled off the organic solvent to obtain 819.7g product HAP with a purity of 98.4%.

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Abstract

The invention relates to a synthesis preparation method of an aldehyde phenoxyl substituted cyclotriphosphazene flame retardant. According to the preparation method, phosphonitrilic chloride trimer, p-hydroxybenzaldehyde, phenol and an ammonium catalyst are adopted as raw materials, the removal of chlorine hydride is realized by an elimination reaction under the catalytic action of ammonium in an organic solvent, aldehyde phenoxyl cyclotriphosphazene (HAP) can be synthetized with a high yield without using an acid-binding agent, the excessive raw materials and the catalyst are removed by washing, and the solvent is removed to obtain aldehyde phenoxyl cyclotriphosphazene.

Description

technical field [0001] The invention relates to a method for synthesizing and preparing an aldehyde phenoxycyclotriphosphazene flame retardant, and belongs to the technical field of preparing materials by chemical synthesis methods. Background technique [0002] As an environmentally friendly flame retardant product, phosphazene flame retardants have developed rapidly in recent years, among which hexaphenoxycyclotriphosphazene can be used in the commercial field at present, and domestic and foreign companies are concerned about the flame retardant series of phosphazenes A large number of patents have been applied for the preparation and application of flame retardants. In the above application materials, hexa-(aldehyde phenoxy)-cyclotriphosphazene series flame retardants and other rings containing aldehyde phenoxy groups have not been used. Triphosphazene is included in the scope of its patent protection. [0003] Hexa-(formylphenoxy)-cyclotriphosphazene, as a new type of f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593
Inventor 钱立军冯发飞周侃
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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