Nitrogen-phosphorus flame-retardant polypropylene block copolymer and preparation method thereof
A technology of flame-retardant polypropylene and block copolymers, which is applied in the field of polymer chemical synthesis and can solve problems such as poor compatibility
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Embodiment 1
[0030] Add diethyl chlorophosphate (5mmol) into a 100mL branched-necked flask, pump N 2 After three times, N 2 Under protection, add 20mL tetrahydrofuran to dissolve diethyl chlorophosphate, keep the temperature at 0°C in an ice bath, add triethylamine (5mmol), dropwise add methacrylamide (7.5mmol) dissolved in 10mL tetrahydrofuran, and drop During the addition process, the temperature of the reaction system was kept constant, and after the dropwise addition was completed, the temperature of the branched flask was raised to 35° C. for 10 h. After the reaction is completed, filter under reduced pressure, rotary evaporate, and wash with water to obtain diethyl-methacrylamide phosphate.
Embodiment 2
[0032] Add 2-(ethylmercaptothioformylthio)-2-methylpropionic acid (4.0mmol) and 20ml of anhydrous tetrahydrofuran THF into the reactor, and after the reaction temperature rises to 70°C, slowly add SOCl 2 (6.0mmol), dropwise completed reaction 2h, after finishing reaction, decompression distillation removes SOCl 2 and THF to give 2-(ethylmercaptothioformylthio)-2-methylpropionyl chloride.
[0033] Hydroxyl-terminated polypropylene (40mmol) was added into a 50ml Schlenk bottle, and after pumping nitrogen three times, N 2 Under protection, add 30ml of anhydrous toluene into a disposable syringe, raise the temperature to 70°C, inject 1ml of pyridine after the (acryloyloxyethyl) isocyanurate is completely dissolved, stir for 30min, then add dropwise the above-mentioned 2 -(Ethylmercaptothioformylthio)-2-methylpropionyl chloride, heat up to 80°C to continue the reaction for 2.5h, the product is cooled to room temperature, and after two cycles of continuous dissolution / precipitation...
Embodiment 3
[0035] Weigh polypropylene macromolecular chain transfer agent (0.1mmol), azobisisobutyronitrile (0.01mmol), diethyl-methacrylamide phosphate (10.0mmol) into a 25ml Schlenk bottle, pump nitrogen 3 times after N 2 Under protection, add 10mL of toluene / DMF (v / v=10:1), raise the temperature of the reactor to 70°C, react for 2h, put the product into liquid nitrogen to quench the reaction, and add the product dropwise to methanol / Precipitate in water, then dissolve the product in toluene, dissolve the precipitate three times continuously, filter, wash with methanol, and dry in vacuum at 45°C to constant weight to obtain a nitrogen-phosphorus flame-retardant polypropylene diblock copolymer.
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