Polymerization with strong alkali phosphazene compound as catalyst
A polymerization reaction and compound technology, applied in the field of polymer synthesis, can solve problems such as difficult to use biomedical materials, difficult removal of metal ions, adverse effects of drugs and human body, etc., and achieve the effect of easy removal and mild reaction conditions
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[0024] Example 1
[0025] In a dry 50mL three-necked flask with a stirrer and a thermometer, add 2.0g acrylamide, 20mL N,N-dimethylacetamide (DMAc), and add 100μL t-BuP 4 After reacting at 80 °C for 48 h, 2 mL of 10 wt% hydrochloric acid solution was added dropwise to terminate the above reaction, and nylon 3 was washed, and then 2 × 100 mL of methanol was used to fully wash the polymer with rapid stirring to remove unreacted monoliths. bulk, (protonated) t-BuP 4 and N,N-dimethylacetamide, filtered, and dried under vacuum at 50°C for 12h, the calculated yield was 90%, and the molecular weight was 1.0×10 4 g / mol. Different from the polymerization of acrylamide initiated by the traditional strong base, the nylon 3 synthesized by the polymerization method does not contain double bond polymerization units, and does not need to add any free radical polymerization inhibitor.
Example Embodiment
[0026] Example 2
[0027] Add 1.0g β-lactam to a 25mL sealed tube, stir with a magnetic bar and 10mL N,N-dimethylacetamide (DMAc) solution containing 10wt% LiCl, freeze with liquid nitrogen, replace nitrogen three times and inject under nitrogen atmosphere 7 μL of t-BuP 4 The n-hexane solution was melted and sealed, and the reaction was carried out at 25 °C. After 2 hours, the system was difficult to stir, and then the reaction was continued at this temperature for 10 hours. After adding 2 mL of 10 wt% hydrochloric acid solution and 100 mL of methanol, the reaction was terminated and the nylon 3 was washed. 2 × 100 mL of methanol was thoroughly washed with rapid stirring to remove unreacted monomers, (protonated) t-BuP4 and N,N-dimethylacetamide, filtered, and dried under vacuum at 50 °C for 12 h. Calculate the yield. The rate is 94% and the molecular weight is 1.1×10 5 g / mol.
Example Embodiment
[0028] Example 3
[0029] In a 25 mL sealed tube, add 1.0 g β-lactam, 0.005 g activator N-benzoyl β lactam (NBL), a stirring magnet, and 10 mL N,N-dimethylacetamide (N,N-dimethylacetamide) containing 10 wt% LiCl ( DMAc) solution, frozen in liquid nitrogen, replaced with nitrogen three times, and quickly injected 70 μL of t-BuP4 in n-hexane solution under nitrogen atmosphere, sealed the tube, and reacted at 25 °C for 12 h. After the reaction, 2 mL of 10 wt% hydrochloric acid solution and 100 mL of methanol were added to terminate the reaction and wash nylon 3, and then the polymer was thoroughly washed with 2 × 100 mL of methanol under rapid stirring to remove unreacted monomers, (protonated) t-BuP4 and N,N-dimethylacetamide, filtered, vacuum dried at 50°C for 12h, the calculated yield was 95%, and the molecular weight was 1.2×10 4 g / mol
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