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Method for preparing halogen-free high-efficiency flame retardant aryloxy cyclotriphosphazene compound

A technology of aryloxycyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of flame retardant preparation, can solve the problems of high production cost, long reaction time, and yellowish product color, and achieve low production cost, The effect of low smoke density and good flame retardant effect

Active Publication Date: 2012-12-26
JINAN TAIXING FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a preparation method of a halogen-free high-efficiency flame retardant aryloxycyclotriphosphazene compound, the preparation method of this kind of flame retardant overcomes the long reaction time and the discoloration of the product in the existing synthesis methods. Huang, high production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] a. take raw material sodium phenate 12.5 and hexachlorocyclotriphosphazene 5.0 by weight for subsequent use;

[0017] b. Add 100 parts by weight of dioxane as a solvent in the reaction vessel, dissolve the weighed sodium phenate and hexachlorocyclotriphosphazene in dioxane, and carry out heating and stirring reaction at a reaction temperature of 85°C , the reaction time is 12.5 hours;

[0018] c. The reaction product is cooled and left standing, and the reaction product is layered. When the upper layer is a yellow solution and the lower layer is a light yellow solid, filter and remove the lower layer solid, and carry out a purification process to the yellow solution obtained by filtration (the processing method is: use a medium Crystallization and purification of the yellow solution with distilled water, drying) to obtain a crude product, and the resulting crude product was subjected to secondary purification treatment (processing method: the crude product was recrystal...

Embodiment 2

[0020] a. take by weight raw material sodium phenate 14 and hexachlorocyclotriphosphazene 4.5 for subsequent use;

[0021] b. Add 92 parts by weight of dioxane as a solvent in the reaction vessel, dissolve the weighed sodium phenate and hexachlorocyclotriphosphazene in dioxane, heat and stir the reaction, and the reaction temperature is 75°C , the reaction time is 14.5 hours;

[0022] c. The reaction product is cooled and left standing, and the reaction product is layered. When the upper layer is a yellow solution and the lower layer is a light yellow solid, filter and remove the lower layer solid, and carry out a purification process to the yellow solution obtained by filtration (the processing method is: use a medium Crystallization and purification of the yellow solution with distilled water, drying) to obtain a crude product, and the resulting crude product was subjected to secondary purification treatment (processing method: the crude product was recrystallized and purifi...

Embodiment 3

[0024] a. take by weight raw material sodium phenate 16.0 and hexachlorocyclotriphosphazene 5.5 for subsequent use;

[0025] b. Add 118 parts by weight of dioxane as a solvent in the reaction vessel, dissolve the weighed sodium phenate and hexachlorocyclotriphosphazene in dioxane, and carry out heating and stirring reaction with a reaction temperature of 92°C , the reaction time is 10 hours;

[0026] c. The reaction product is cooled and left standing, and the reaction product is layered. When the upper layer is a yellow solution and the lower layer is a light yellow solid, filter and remove the lower layer solid, and carry out a purification process to the yellow solution obtained by filtration (the processing method is: use a medium Crystallization and purification of the yellow solution with distilled water, drying) to obtain a crude product, and the resulting crude product was subjected to secondary purification treatment (processing method: the crude product was recrystal...

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Abstract

The invention discloses a method for preparing a halogen-free high-efficiency flame retardant aryloxy cyclotriphosphazene compound. The flame retardant is a pure white crystal product prepared by reacting sodium phenate and hexachlorocyclotriphosphazene serving as raw materials with dioxane serving as a solvent under heating and stirring, filtering and purifying. The preparation method of the flame retardant overcomes the defects of long reaction time, a yellow product color and high production cost existing in the conventional synthesis method commonly. The prepared flame retardant has the characteristics of high efficiency, no halogen, flame retardance, no toxicity, low smoke and the like, has high compatibility with most of organic polymer materials, and has processing stability and using stability.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant, in particular to a method for preparing a halogen-free high-efficiency flame retardant aryloxycyclotriphosphazene compound. Background technique [0002] Low-brominated ether compound flame retardants, tetrabromodiphenyl ether, pentabromodiphenyl ether, hexabromodiphenyl ether, heptabromodiphenyl ether, octabromodiphenyl ether and other organic substances have persistent organic pollution to the environment, so they have been It is listed in Appendix A of the Stockholm Convention and its use is prohibited. Decabromodiphenyl ether, as one of the widely used organic brominated flame retardants, is widely used in polyolefin (PE, PP, ABS), polyester (PBT, PET), epoxy resin, fiber and other organic polymer materials Although decabromodiphenyl ether is not directly included in the banned scope of the "Stockholm Convention", various low-substituted brominated ethers produced during its product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6593C08K5/5399
Inventor 王秀芬杨新改牛民卜
Owner JINAN TAIXING FINE CHEM
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