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P-N-Si ternary synergistic flame retardant as well as preparation method and application thereof

A phosphorus-nitrogen-silicon and synergistic flame-retardant technology is applied in the field of phosphorus-nitrogen-silicon ternary synergistic flame retardants and their preparations, which can solve the problems of poor flame retardancy and high phosphorus content in flame retardants, and achieve good thermal stability and flame retardancy. The effect of improved combustion performance and good thermal stability

Inactive Publication Date: 2017-12-22
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a phosphorus nitrogen silicon ternary synergistic flame retardant and its preparation method in order to solve the performance problems of traditional synthetic resins such as poor flame retardancy. The raw materials of this method are easy to obtain and the reaction process is relatively simple , does not require too harsh reaction conditions, the prepared flame retardant has high phosphorus content and good flame retardant effect, and the flame retardant performance of the material is improved by blending with the material

Method used

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  • P-N-Si ternary synergistic flame retardant as well as preparation method and application thereof
  • P-N-Si ternary synergistic flame retardant as well as preparation method and application thereof
  • P-N-Si ternary synergistic flame retardant as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add 0.0167 mol of hexachlorocyclotriphosphazene and 40 ml of tetrahydrofuran into a three-neck flask, dissolve and stir evenly, and then add 0.0167 mol of triethylamine. N 2 Under protection, fully stirred, 0.0167mol KH550 was added dropwise to the reaction system at 0°C. The solution was heated to reflux at 40°C for 20 hours, cooled and filtered to remove triethylamine hydrochloride, and tetrahydrofuran and tetrahydrofuran were removed by rotary evaporation to obtain an oily product, which was a silanized hexachlorocyclotriphosphazene derivative.

[0022] (2) Add 0.005 mol tetrahydrofuran solution (20 ml) of silanized hexachlorocyclotriphosphazene derivative to a three-neck flask, and slowly add aniline (0.025 mol) and triethylamine tetrahydrofuran solution (0.025 mol) dropwise therein. Stir and reflux for 10 hours under the protection of nitrogen at 40°C. After the reaction, the material was cooled to room temperature, vacuum filtered, washed twice with deionized...

Embodiment 2

[0030] (1) Add 0.0167mol of hexachlorocyclotriphosphazene and 100ml of chloroform into a three-neck flask, dissolve and stir evenly, then add 0.0167mol of triethylamine. N 2 Under protection, fully stirred, 0.0167mol KH550 was added dropwise to the reaction system at 0°C. The solution was heated to reflux at 100°C for 50 hours, cooled and filtered to remove triethylamine hydrochloride, and chloroform was removed by rotary evaporation to obtain an oily substance, which was a silanized hexachlorocyclotriphosphazene derivative.

[0031] (2) Add the chloroform solution (50ml) of the hexachlorocyclotriphosphazene derivative of 0.005mol silanization in the there-necked flask, slowly drop the chloroform solution (0.025mol) of 0.025mol aniline and triethylamine therein . Stir and reflux reaction at 100°C under nitrogen protection for 20h. After the reaction, cool the material to room temperature, vacuum filter, wash with deionized water and chloroform for 5 times, and vacuum dry at ...

Embodiment 3

[0034] (1) Add 0.0167mol of hexachlorocyclotriphosphazene and 80ml of diethyl ether into a three-neck flask, dissolve and stir evenly, then add 0.0167mol of triethylamine. N 2 Stir well under protection, and drop 0.0167mol KH550 into the reaction system at 0°C. The solution was heated to reflux at 45°C for 30 hours, cooled and filtered to remove triethylamine hydrochloride, and the solvent was removed by rotary evaporation to obtain an oily product, which was a silanized hexachlorocyclotriphosphazene derivative.

[0035] (2) Add 0.005 mol of silanized hexachlorocyclotriphosphazene ethyl ether solution (30 ml) into a three-necked flask, and slowly dropwise add 0.025 mol of aniline and triethylamine solution (0.025 mol) thereinto. Stir and reflux for 15 hours under the protection of nitrogen at 45°C. After the reaction, the material was cooled to room temperature, vacuum filtered, washed with deionized water and ether three times, and vacuum-dried at 95°C for 2 hours to obtain ...

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Abstract

The invention discloses a P-N-Si ternary synergistic flame retardant. The flame retardant has the structural formula shown in the description, wherein x ranges from 1 to 5 and 6 substituent groups are linked to three phosphorous atoms. The flame retardant can be applied to epoxy resin. P, N and Si elements in molecules of the flame retardant can perform flame retardance independently and also have a synergistic flame retardance effect. The epoxy resin using the flame retardant for flame retardance has the limit oxygen index of 32% at most and has the vertical combustion class of class V-0. The invention also discloses a preparation method of the flame retardant.

Description

technical field [0001] The invention relates to a phosphorus-nitrogen-silicon ternary synergistic flame retardant and a preparation method thereof. The flame retardant is introduced into synthetic resins such as epoxy resin, and various flame retardant elements thereof play a synergistic flame retardant effect. Background technique [0002] As general-purpose materials, polymer materials are widely used in various fields. With the rapid development of the polymer industry, polymers can not only replace traditional materials such as steel, cotton, wood, natural rubber and ceramics, but also become a functional material. Although polymer materials have brought many conveniences to people's lives, their flammability limits their application in some special dangerous places. Therefore, it is a key problem to be solved urgently to improve the safety of people's living environment while enjoying the convenience of polymer materials for people. [0003] Additive flame retardant r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08K5/544C08L63/00
CPCC07F9/65815C08L63/00C08K5/5477
Inventor 丁寅潘政阁明泰
Owner NANJING UNIV
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