Melamine modified polyamino cyclotriphosphazene and preparation method thereof

A technology of polyaminocyclotriphosphazene and melamine, which is applied in the field of melamine-modified polyaminocyclotriphosphazene and its preparation, can solve the problems of poor thermal stability, high water solubility, limitations, etc., and achieve improved thermal stability and water-soluble The effect of reducing property and hygroscopicity and improving phosphorus yield

Active Publication Date: 2015-06-24
嘉兴卓十生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As reported in the patent [Tang Linsheng, Li Li, Wang Yong, etc. A new type of intumescent flame retardant. The intumescent flame retardant compounded by cyanurate (Sike for short) has a good flame retardant effect on polyolefins, but polyaminocyclotriphosphazene has high water solubility, strong hygroscopicity, and low thermal stability. Poor, so its application may be limited

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  • Melamine modified polyamino cyclotriphosphazene and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0028] The preparation technology of melamine modified polyaminocyclotriphosphazene comprises the steps:

[0029] (1) Condensation: Add 10g of hexachlorocyclotriphosphazene, 3.6g of melamine, 60g of chlorobenzene and 8.5g of triethylamine into a 250mL three-necked flask, and heat the material to 80-85°C in a water bath under nitrogen protection and stirring. After maintaining the temperature for 18 hours, cool down to room temperature, sample and analyze the free chlorine content, and calculate the degree of substitution of chlorine in the hexachlorocyclotriphosphazene according to the free chlorine content (the percentage of free chlorine mass and total chlorine mass in the sample). The free chlorine content is analyzed by the mercury method, and the specific steps refer to GB / T3051-2000. After analysis, the substitution degree of chlorine was 43.3%.

[0030] (2) Ammonification: The above materials are further cooled to about 0°C with an ice-salt bath, and ammonia gas is intro...

Embodiment 2

[0034] The preparation technology of melamine modified polyaminocyclotriphosphazene comprises the steps:

[0035] (1) Condensation: Add 10g of hexachlorocyclotriphosphazene, 5.4g of melamine, 60g of chlorobenzene and 13.0g of triethylamine into a 250mL three-necked flask, and heat the material to 80-85°C in a water bath under nitrogen protection and stirring. And maintain the temperature for 18h and then cool down to room temperature. After analysis, the substitution degree of chlorine was 54.0%.

[0036] (2) Ammonification: The above materials are further cooled to about 0°C with an ice-salt bath, and ammonia gas is introduced at a constant speed under stirring for 18 hours, and a total of about 10 g of ammonia gas is introduced, and then filtered, and the filter cake is dried to obtain a white powder Solid 30.2g—melamine-modified aminocyclotriphosphazene and the mixture of by-product water-soluble ammonium salts (triethylamine hydrochloride and ammonium chloride). After an...

Embodiment 3

[0040] The preparation technology of melamine modified polyaminocyclotriphosphazene comprises the steps:

[0041] (1) Condensation: Add 10g of hexachlorocyclotriphosphazene, 7.2g of melamine, 60g of chlorobenzene and 17.4g of triethylamine into a 250mL three-necked flask, and heat the material to 80-85°C in a water bath under nitrogen protection and stirring. And maintain the temperature for 18h and then cool down to room temperature. After analysis, the substitution degree of chlorine was 64.4%.

[0042] (2) Ammonification: The above materials are further cooled to about 0°C with an ice-salt bath, and ammonia gas is introduced at a constant speed under stirring for 18 hours, and a total of about 10 g of ammonia gas is introduced, and then filtered, and the filter cake is dried to obtain a white powder 35.8 g of solids—a mixture of melamine-modified aminocyclotriphosphazene and ammonium salts. After analysis, the substitution degree of chlorine was 99.1%.

[0043] (3) Polyc...

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Abstract

The invention discloses a novel phosphonitrile compound (melamine modified polyamino cyclotriphosphazene) and a preparation method thereof, and belongs to the field of chemical engineering and high polymer material additives. The novel phosphonitrile compound is prepared by condensing melamine and hexachlorocyclotriphosphazene, re-ammoniating and finally heating for condensation polymerization. Compared with polyamino cyclotriphosphazene, the melamine modified polyamino cyclotriphosphazene is remarkably low in water solubility and hygroscopicity, is remarkably high in thermal stability, and is relatively suitable for being used as a flame retardant for plastic and the like as the initial thermal decomposition temperature (temperature for 2% of weight loss) is increased to be greater than 200 DEG C from about 70 DEG C. In addition, the phosphorus yield of the product is also remarkably increased.

Description

technical field [0001] The present invention relates to a new phosphazene compound and its preparation method, specifically melamine-modified polyaminocyclotriphosphazene and its preparation method. The compound can be used as a flame retardant and belongs to chemical and polymer materials auxiliary drug field. Background technique [0002] Flame retardant is an important additive for polymer materials, and many varieties have been reported. Due to the excellent cost performance, brominated flame retardants are currently one of the most produced organic flame retardants in the world, but the high polymers flame-retardant with brominated flame retardants generate more smoke, corrosive gases and toxic gases when burned , and reduce the anti-ultraviolet stability of the flame-retardant substrate. Some brominated flame retardants (such as polybrominated diphenyl ethers) also have potential hazards to the environment and human health, especially the thermal cracking and combust...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08K5/5399
Inventor 唐林生王玉冲宋红兵何为
Owner 嘉兴卓十生物科技有限公司
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