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Phenyl-modified polyaminocyclotriphosphazene and its preparation method

A technology of polyaminocyclotriphosphazene and hexachlorocyclotriphosphazene, which is applied in the field of phenyl-modified polyaminocyclotriphosphazene and its preparation, can solve problems such as poor thermal stability and limitations, and achieve improved thermal stability , water solubility and hygroscopicity reduction, and the effect of phosphorus yield improvement

Active Publication Date: 2019-02-19
东营睿港招商服务有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyaminocyclotriphosphazene is a new type of phosphazene flame retardant, which has good flame retardant effect on polyethylene, polypropylene and epoxy resin [Tang Linsheng, Li Li, Wang Yong, etc. A kind of polyaminocyclotriphosphazene Intumescent flame retardant compounded by cyclotriphosphazene and tris (2-hydroxyethyl) isocyanurate. CN103524885B, 2015-08-26; Ke Yang, Zhao Jing, Cheng Guoliang, et al. Flame retardant effect of aminocyclotriphosphazene on cured epoxy resin. Modern Plastics Processing and Application, 2016, 28(1): 34-37], but polyaminocyclotriphosphazene has high water solubility and strong hygroscopicity. Poor thermal stability limits its application

Method used

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  • Phenyl-modified polyaminocyclotriphosphazene and its preparation method
  • Phenyl-modified polyaminocyclotriphosphazene and its preparation method
  • Phenyl-modified polyaminocyclotriphosphazene and its preparation method

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Effect test

Embodiment 1

[0046] The preparation technology of phenyl modified polyaminocyclotriphosphazene comprises the steps:

[0047] (1) Condensation: Add 17.4g of hexachlorocyclotriphosphazene, 6.1g of aniline, 6.6g of triethylamine, and 60g of chlorobenzene into a 250mL three-necked flask equipped with a thermometer, mechanical stirring, and reflux condenser, and pass the oil under stirring. The material was heated in a bath to 90°C and reacted at this temperature for 8h. Cool to room temperature, take a sample and analyze the free chlorine content, and calculate the degree of substitution of chlorine in the hexachlorocyclotriphosphazene (for the percentage of free chlorine mass and total chlorine mass in the sample) according to the free chlorine content. After analysis, the substitution degree of chlorine is 17.5%, which means that about 1.05 chlorine atoms in each phosphazene ring are replaced by anilino groups.

[0048] (2) Ammonification: The above materials are further cooled to about 0°C...

Embodiment 2

[0056] The preparation technology of phenyl modified polyaminocyclotriphosphazene comprises the steps:

[0057] (1) Condensation: Add 17.4g of hexachlorocyclotriphosphazene, 6.1g of aniline, 6.6g of triethylamine, and 60g of chlorobenzene into a 250mL three-necked flask equipped with a thermometer, mechanical stirring, and reflux condenser, and pass the oil under stirring. The material was heated in a bath to 90 °C and reacted at this temperature for 6 h. Cool to room temperature, take a sample to analyze the free chlorine content, and calculate the substitution degree of chlorine in hexachlorocyclotriphosphazene according to the free chlorine content. After analysis, the substitution degree of chlorine is 13.6%, which means that about 0.82 chlorine atoms in each phosphazene ring are substituted by anilino groups.

[0058] (2) Ammonification: The above materials are further cooled to about 0°C with an ice-salt bath, and ammonia gas is introduced at a uniform speed for 18 hour...

Embodiment 3

[0063] The preparation technology of phenyl modified polyaminocyclotriphosphazene comprises the steps:

[0064] (1) Condensation: Add 17.4g of hexachlorocyclotriphosphazene, 6.1g of aniline, 6.6g of triethylamine, and 60g of chlorobenzene into a 250mL three-necked flask equipped with a thermometer, mechanical stirring, and reflux condenser, and pass the oil under stirring. The material was heated in a bath to 90° C. and reacted at this temperature for 10 h. Cool to room temperature, take a sample to analyze the free chlorine content, and calculate the substitution degree of chlorine in hexachlorocyclotriphosphazene according to the free chlorine content. After analysis, the substitution degree of chlorine is 17.6%, which means that about 1.05 chlorine atoms in each phosphazene ring are replaced by anilino groups.

[0065] (2) Ammonification: The above materials are further cooled to about 0°C with an ice-salt bath, and ammonia gas is introduced at a uniform speed for 18 hours...

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Abstract

The invention relates to a new phosphazene compound (phenyl-modified polyamino-cyclotriphosphazene) and a preparation method thereof, belonging to the fields of chemical industry and high polymer material auxiliary agents. The structure of the phenyl-modified polyamino-cyclotriphosphazene is described in the description, wherein M represents -NH2 and two different functional groups which are described in the description. The compound is obtained by enabling aniline and hexachlor-cyclotriphosphazene to be subjected to condensation, then carrying out ammoniation and finally heating for carrying out polycondensation. Compared with polyamino-cyclotriphosphazene, the phenyl-modified polyamino-cyclotriphosphazene has obviously reduced water solubility and moisture absorption and improved thermal stability, thus being more suitable for being used as flame retardants for materials such as plastics. Furthermore, the phosphorus recovery rate of a product is also obviously improved.

Description

technical field [0001] The present invention relates to a new phosphazene compound and its preparation method, specifically phenyl-modified polyaminocyclotriphosphazene and its preparation method. The compound can be used as a flame retardant and belongs to chemical and polymer materials Auxiliary field. Background technique [0002] Flame retardant is an important additive for polymer materials. There are many varieties reported, mainly including halogen-based, metal hydroxide, and phosphorus-based flame retardants. Although halogenated flame retardants are widely used due to their excellent cost performance, their application is increasingly restricted due to serious environmental and safety problems. Metal hydroxides such as aluminum hydroxide (AHT) and magnesium hydroxide (MH) are known as "pollution-free flame retardants", which are non-volatile, non-precipitating, good stability, non-toxic smoke, low cost and abundant resources And other advantages, it has become the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6593C08G79/025
CPCC07F9/65815C08G79/025
Inventor 唐林生杨晶巍毕伟朱凤丽隋晓彤
Owner 东营睿港招商服务有限责任公司
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