Novel P-N-Si synergistic anti-flaming copolymerized polyamide 6 and preparation method thereof
A technology for flame retardant copolymerized polyamide and polyamide, which is applied in the field of flame retardant materials, can solve the problems of complex processing technology, influence of material mechanical properties, and high cost, and achieves good flame retardant effect.
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Embodiment 1
[0048] Example 1, P-N-Si synergistic copolymerization flame retardant copolymerized polyamide 6
[0049] 1. Add bis(4-carboxyphenyl)phenylethylphosphine oxide (R in formula I is ethylbenzene) and hexamethylenediamine to the reactor at a molar ratio of 1:1.2, and stir at 60°C for 1.5h. Let it mix completely. Then adjust the pressure to 0.2MPa, raise the temperature to 170°C, and prepolymerize for 1 hour. After cooling down to room temperature, it was suction filtered and washed with deionized water to obtain a phosphorus-containing flame retardant prepolymer with a molecular weight of 5000.
[0050]2. Add 5 parts of deionized water, 100 parts of caprolactam, 1 part of catalyst sodium hypophosphite and 0.5 part of antioxidant 1098 into the reaction kettle, repeat vacuuming and nitrogen filling for 6 times, remove all the air in the kettle, and fill the kettle with nitrogen to make the Pressure 0.2MPa. Heating the reaction kettle and starting stirring at the same time, the tem...
Embodiment 2
[0051] Example 2, P-N-Si synergistic copolymerization flame retardant copolymerized polyamide 6
[0052] 1. Add bis(4-carboxyphenyl)phenylpropenylphosphine oxide (R in formula I is propenylbenzene) and decanediamine to the reactor at a molar ratio of 1:1.1, and stir at 80°C for 0.5h , to mix completely. Then adjust the pressure to 0.2MPa, raise the temperature to 170°C, and prepolymerize for 1 hour. After cooling down to room temperature, it was suction filtered and washed with deionized water to obtain a phosphorus-containing flame retardant prepolymer with a molecular weight of 1000.
[0053] 2. Add 10 parts of deionized water, 100 parts of caprolactam, 0.1 part of catalyst potassium phosphite and 1 part of antioxidant 1076 into the reaction kettle, repeat vacuuming and nitrogen filling for 3 times, remove all the air in the kettle, and keep the pressure in the kettle at 0.1 MPa. Heating the reaction kettle and starting stirring at the same time, the temperature was raise...
Embodiment 3
[0054] Example 3, P-N-Si synergistic copolymerization flame retardant copolymerized polyamide 6
[0055] 1. Add bis(4-carboxyphenyl)phenylbutanylphosphine oxide (R in formula I is butylbenzene) and hexamethylenediamine to the reactor at a molar ratio of 1:1.15, and stir at 70°C for 1h. Let it mix completely. Then adjust the pressure to 0.2MPa, raise the temperature to 170°C, and prepolymerize for 1 hour. After cooling down to room temperature, it was suction filtered and washed with deionized water to obtain a phosphorus-containing flame retardant prepolymer with a molecular weight of 3500.
[0056] 2. Add 8 parts of deionized water, 100 parts of caprolactam, 0.5 parts of catalyst sodium phosphate and 0.1 part of antioxidant 1010 into the reaction kettle, repeat vacuuming and nitrogen filling for 5 times, remove all the air in the kettle, and keep the pressure in the kettle at 0.15MPa ; Heating the reactor, while starting to stir, the temperature was raised to 180°C, the pre...
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