Tetraphenylethylene-labeled responsive quaternized polyvinyl alcohol, and preparation method and application thereof
A technology for salinizing polyvinyl alcohol and tetraphenylethylene, which is applied in the field of tetraphenylethylene-labeled responsive quaternary ammonium salted polyvinyl alcohol and its preparation and application, to achieve excellent antibacterial performance, simple process operation, and short reaction time Effect
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[0041] Example 1
[0042] (1) Preparation of PVA-DEEDA: Dissolve polyvinyl alcohol (5.0 g, hydroxyl molar weight of 0.12 mol) in 100 mL DMSO, and stir to dissolve at 90°C. After complete dissolution, it was cooled to room temperature, CDI (7.8 g, 0.048 mol) was added to the above solution for activation for 3 hours, and then DEEDA (6.7 mL, 0.048 mol) was slowly added to the above solution to react at 22° C. for 20 hours. Add 50 mL of 25% ammonia solution and stir for 1 hour to remove unreacted CDI. After finishing the reaction, precipitate in acetone, dissolve the precipitate in deionized water, dialyze for 3 days, and freeze-dry to obtain modified polyvinyl alcohol. The weight average molecular weight of polyvinyl alcohol is preferably 85,000 to 124,000.
[0043] (2) Preparation of PVA-TPE: PVA-DEEDA (600mg, 16.4mmol) obtained in step (1) was dissolved in 12mL DMSO, stirred until completely dissolved, and then TPE-CH was added 2 Br (35mg, 0.082mmol), heated at 70°C for 24 hours,...
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[0051] Example 2
[0052] (1) Preparation of PVA-DEEDA: Dissolve polyvinyl alcohol (5.0 g, hydroxyl molar weight of 0.12 mol) in 100 mL DMSO, and stir to dissolve at 90°C. After the solution was completely dissolved, it was cooled to room temperature and CDI (9.2g, 0.06mol) was added to the above solution for activation for 3 hours, and then DEEDA (8mL, 0.06mol) was slowly added to the above solution for reaction at 22°C for 20 hours. Add 50 mL of 25% ammonia solution and stir for 1 hour to remove unreacted CDI. After finishing the reaction, precipitate in acetone, dissolve the precipitate in deionized water, dialyze for 3 days, and freeze-dry to obtain modified polyvinyl alcohol. The weight average molecular weight of polyvinyl alcohol is preferably 85,000 to 124,000.
[0053] (2) Preparation of PVA-TPE: PVA-DEEDA (600mg, 16.4mmol) obtained in step (1) was dissolved in 12mL DMSO, stirred until completely dissolved, and then TPE-CH was added 2 Br (35mg, 0.082mmol), heated at 70°C...
Example Embodiment
[0054] Example 3
[0055] (1) Preparation of PVA-DEEDA: Dissolve polyvinyl alcohol (5.0 g, hydroxyl molar weight of 0.12 mol) in 100 mL DMSO, and stir to dissolve at 90°C. After complete dissolution, it was cooled to room temperature, CDI (11.7 g, 0.072 mol) was added to the above solution for activation for 3 hours, and then DEEDA (10 mL, 0.072 mol) was slowly added to the above solution to react at 22° C. for 20 hours. Add 50 mL of 25% ammonia solution and stir for 1 hour to remove unreacted CDI. After finishing the reaction, precipitate in acetone, dissolve the precipitate in deionized water, dialyze for 3 days, and freeze-dry to obtain modified polyvinyl alcohol. The weight average molecular weight of polyvinyl alcohol is preferably 85,000 to 124,000.
[0056] (2) Preparation of PVA-TPE: PVA-DEEDA (600mg, 16.4mmol) obtained in step (1) was dissolved in 12mL DMSO, stirred until completely dissolved, and then TPE-CH was added 2 Br (35mg, 0.082mmol), heated at 70°C for 24 hours,...
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