Nitrogen-phosphorus flame-retardant polybutadiene material and preparation method thereof
A polybutadiene, nitrogen and phosphorus flame retardant technology, applied in the field of polymer chemical synthesis, can solve problems such as poor compatibility, and achieve the effect of durable flame retardant performance
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Embodiment 1
[0024] Add carboxyl-terminated polybutadiene (2.0 mmol) and anhydrous tetrahydrofuran THF into the reactor, and after the reaction temperature rises to 70°C, slowly add SOCl dropwise 2 (10.0mmol), the dropwise addition completed the reaction for 2h, after finishing the reaction, the SOCl was removed by distillation under reduced pressure 2 and THF to obtain a carboxyl-terminated polybutadienyl chloride product with a yield of 78.4%.
Embodiment 2
[0026] Nitrogen-phosphorus flame retardant (1.0mmol) was added into a 50mL Schlenk bottle, and after pumping nitrogen three times, N 2 Under protection, add 30ml of anhydrous toluene to a disposable syringe, raise the temperature to 70°C, inject 1ml of pyridine after the nitrogen and phosphorus flame retardant is completely dissolved, and after stirring for 30min, add the above carboxyl-terminated polybutadienyl chloride dissolved in toluene dropwise The product (10.0mmol) was heated to 80°C and continued to react for 3 hours. The product was cooled to room temperature, and after two cycles of continuous dissolution / precipitation in toluene / methanol, it was dried in vacuum at 45°C to constant weight to obtain nitrogen-phosphorus flame-retardant polybutylene ene material with a yield of 80.2%.
Embodiment 3
[0028] Before processing, vacuum-dry the nitrogen-phosphorus flame-retardant polybutadiene material at 80°C for 12 hours, add 60wt% nitrogen-phosphorus flame-retardant polybutadiene material on an open heat refiner with a twin-roller temperature of 225°C, and wait for it to melt After wrapping and kneading for 10 minutes, the sheets are uniformly released, hot pressed on a flat vulcanizer at 230°C for 10 minutes, cold pressed at room temperature for 8 minutes, and then released. Various standard specimens are prepared on a universal prototype machine for flame retardant performance testing.
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