Preparation method of pH-responsive polymethacrylic acid glyceride
A technology of polyglycerol methacrylate and polyglycerol methacrylate, applied in the field of preparation of pH-responsive polyglycerol methacrylate, achieving strong innovation, applicability, and low cost
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Embodiment 1
[0040] Take a 100ml three-necked flask, blow nitrogen gas for 5-10 minutes, take 0.3g of five-arm (Mn=16000) polyglycidyl methacrylate (S516) into a 100ml three-necked flask, add 20ml of acetonitrile and stir to dissolve, at a temperature of 90 ℃ Under the conditions, add ethylenediamine 10ml, stir and reflux for 12 hours, after the solution is cooled, stop stirring and nitrogen protection, dialyze with deionized water for 48 hours and freeze-dry, which is the target product amino polyglycidyl methacrylate S516- da.
Embodiment 2
[0042] Take a 100ml three-necked flask, blow nitrogen for 5-10 minutes, take 0.3g of five-arm (Mn=16000) polyglycerol methacrylate (S516OH) into a 100ml three-necked flask, add 20ml of N,N-dimethylacetamide and stir Dissolve, inject diluted 0.001g p-toluenesulfonic acid as a catalyst at 70°C, stir for 5-10 minutes, inject dissolved 0.187g succinic anhydride (SA), under nitrogen protection, stir and reflux for 4 hours , heated to 140 °C, continued to stir and reflux for 5 hours, after the solution was cooled, stop stirring and nitrogen protection, dialyzed with deionized water for 48 hours and freeze-dried to obtain the target product carboxypolyglycerol methacrylate S516OH-SA.
Embodiment 3
[0044] Take a 100ml three-neck bottle and vacuumize it, blow nitrogen, repeat three times, and dissolve 0.3g carboxyl polyglycerol methacrylate S516OH-SA (carboxyl substitution rate is 40%) in 20ml N,N-Dimethylacetamide to prepare Solution, injected into the reaction device, at a temperature of 70°C, add 0.002ml of dibutyltin dilaurate as a catalyst, under nitrogen protection, stir for 5-10 minutes, dilute 0.12ml of hexamethylene diisocyanate (HDI) with a solvent , injected into the reaction device, stirred and refluxed for 3 hours under nitrogen protection; after the solution was cooled, stop stirring and nitrogen protection, use diethyl ether as a precipitant, precipitate the product, filter it with suction, dissolve it with a small amount of solvent, and dialyze it with deionized water for 48 Hours, freeze-dried, that is the target product semi-interpenetrating carboxyl polyglycerol methacrylate polymer network S516OH-SA / HDI.
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