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Reactive flame retardants adopting bridged cyclophosphazene and preparation methods of reactive flame retardants

A technology based on cyclotriphosphazene and chlorinated cyclotriphosphazene is applied in the field of bridged cyclophosphazene reactive flame retardant and its preparation, and can solve the problem of poor thermal stability, limited environmental conditions, and lowering the initial thermal decomposition temperature of the matrix, etc. problem, to achieve the effect of good thermal stability, large steric hindrance and high content

Active Publication Date: 2015-11-18
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its thermal stability is poor, and the initial thermal decomposition temperature of the matrix is ​​significantly reduced after being introduced into the matrix, thus limiting the environmental conditions for its actual use.

Method used

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  • Reactive flame retardants adopting bridged cyclophosphazene and preparation methods of reactive flame retardants
  • Reactive flame retardants adopting bridged cyclophosphazene and preparation methods of reactive flame retardants
  • Reactive flame retardants adopting bridged cyclophosphazene and preparation methods of reactive flame retardants

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 250mL round-bottomed flask, nitrogen gas was introduced, and 56.0g (0.6mol) of aniline, 16.0g (0.12mol) of potassium carbonate, and 10.0g (0.012mol) of bisphenol S bridged chlorinated cyclotriphosphazene (BCP-BPS) were added. ). Stir at room temperature and react for 2h; heat up to 80°C, react for 2h; heat up to reflux, react for 12h. After filtration, the filtrate was distilled under reduced pressure to remove aniline to obtain a yellow solid. Wash 3 times with deionized water and dry to remove residual moisture. Recrystallized three times using diethyl ether / petroleum ether to obtain 15.3 g of a light yellow solid with a yield of 93.0%.

Embodiment 2

[0027] In a 250mL round-bottomed flask, nitrogen gas was introduced, and 56.0g (0.6mol) of aniline, 12.7g (0.12mol) of sodium carbonate, and 10.0g (0.012mol) of bisphenol S bridged chlorinated cyclotriphosphazene (BCP-BPS) were added. ). The reaction was stirred at room temperature for 3 hours; the temperature was raised to 80° C., and the reaction was made for 4 hours; the temperature was raised to reflux, and the reaction was made for 14 hours. After filtration, the filtrate was distilled under reduced pressure to remove aniline to obtain a yellow solid. Wash 5 times with deionized water and dry to remove residual moisture. Recrystallized three times using diethyl ether / petroleum ether to obtain 14.6 g of light yellow solid with a yield of 89.0%.

Embodiment 3

[0029] Into a 500mL round-bottomed flask, nitrogen was introduced, and 279.0g (3.0mol) of aniline, 80.0g (0.6mol) of potassium carbonate, and 50.0g (0.06mol) of bisphenol S bridged chlorinated cyclotriphosphazene (BCP-BPS) were added. ). Stir the reaction at room temperature for 4 hours; raise the temperature to 80° C., and react for 3 hours; raise the temperature to reflux, and react for 24 hours. After filtration, the filtrate was distilled under reduced pressure to remove aniline to obtain a yellow solid. Wash 4 times with deionized water and dry to remove residual moisture. Recrystallized three times using diethyl ether / petroleum ether to obtain 75.0 g of light yellow solid with a yield of 91.0%.

[0030] (2) Bisphenol A bridged anilino cyclotriphosphazene compound

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PUM

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Abstract

The invention relates to the field of reactive flame retardants, in particular to reactive flame retardants adopting bridged cyclophosphazene and preparation methods of the reactive flame retardants. The two reactive flame retardant compounds adopting bridged cyclophosphazene take hexachlorocyclotriphosphazene as the raw material, two phosphazene rings are bridged through a rigid structure and have a substitution reaction with aniline, and products are obtained. The two novel flame retardants have the characteristics of high rigidity, large steric hindrance, multiple active sites, high content of phosphorus and nitrogen and the like as well as excellent thermal stability and can be applied to epoxy resin; further, the flame retardants are halogen-free, cannot release poisonous gas such as halogen hydride and the like during burning, and meet the environment-friendly development trend of the current flame retardants.

Description

technical field [0001] The invention relates to the field of reactive flame retardants, in particular to a bridged cyclophosphazene reactive flame retardant and a preparation method thereof. Background technique [0002] Epoxy resin has excellent mechanical properties, high thermal stability, chemical corrosion resistance and anti-aging characteristics, and is widely used in construction, transportation, electronic and electrical products, aerospace and other fields. However, the limiting oxygen index of the common epoxy resin system is less than 21%, which is a flammable material and cannot meet the safety standards in many fields, so it must be treated with flame retardancy. Halogen flame retardants have been widely used in the flame retardant treatment of epoxy resins, but they produce toxic and corrosive gases and are carcinogenic. Halogen-free flame retardants represented by phenyl phosphate compounds have excellent thermal stability and flame retardancy, and their pro...

Claims

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Application Information

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IPC IPC(8): C07F9/6593C08K5/5399C08L63/00
Inventor 刘亚青梁文俊赵斌赵贵哲王晓峰柳学义
Owner ZHONGBEI UNIV
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