A kind of preparation method of structurally stable pH-responsive polymer vesicles
A technology with stable structure and polymer, which is applied in the field of polymer compound synthesis to achieve high application value and stable structure
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Embodiment 1
[0036] Step a. Weigh 3.80g mPEG with a molecular weight of 1900, 1.116g CPADB, 0.048g DMAP and 25mL anhydrous CH 2 Cl 2 Put into a 100mL round bottom flask and stir, dissolve 0.619g DCC in 5mL anhydrous CH 2 Cl 2And added dropwise to the above system, the reaction was carried out at room temperature for 72h, after filtration, it was settled in glacial ether for three times, and vacuum-dried to obtain pink solid powder. The obtained pink solid powder was subjected to nuclear magnetic detection. figure 1 , the calculated grafting rate of mPEG was higher than 95%.
[0037] Step b. Add 0.0588g of the product in step a, 0.273g of DIPEMA, 0.0455g of GlyMA, 0.0015g of AIBN, 1.212g of ethanol, and 0.303g of deionized water to a 25mL reaction flask, and pass argon gas for 30min under ice-water bath conditions, Then, after three pumping operations, the reaction bottle was sealed and reacted in an oven at 70 °C for 7 hours. The reaction bottle was taken out and placed in an ice-water ...
Embodiment 2
[0040] The preparation process of step a and macromolecular chain transfer agent is the same as step a in Example 1.
[0041] Step b. Add the prepared macromolecular chain transfer agent 0.066g, 0.410g DIPEMA, 0.068g GlyMA, 0.0015g AIBN, 5.182g ethanol, and 5.182g deionized water into a 25mL reaction flask, freeze and vacuumize with liquid nitrogen, and repeat three times. The tube was sealed, reacted in an oven at 70° C. for 7 h, and the reaction flask was taken out and placed in an ice-water bath to stop the reaction to obtain PEG-b-P (DIPEMA-GlyMA) polymer vesicles.
[0042] Step c, take 0.1 g of PEG-b-P (DIPEMA-GlyMA) polymer vesicles prepared in step b, dilute 10 times with a mixed solvent of ethanol and water, then add ethylenediamine, and stir at room temperature for 24 hours to obtain a cross-linked polymer vesicles, which were characterized by TEM, the results are as follows Image 6 As shown, the average particle size of the cross-linked polymer vesicles prepared un...
Embodiment 3
[0044] Step a. Weigh 1.0g mPEG with a molecular weight of 2000, 0.698g CPADB, 0.024g DMAP and 15mL anhydrous CH 2 Cl 2 Put into a 50mL round bottom flask and stir, dissolve 0.206g DCC in 5mL anhydrous CH 2 Cl 2 It was added dropwise to the above system, the reaction was carried out at room temperature for 72 hours, after filtration, it was settled in glacial ether for three times, and dried in vacuo to obtain a pink solid powder.
[0045] Step b. Add 0.092g, 0.614g DIPEMA, 0.102g GlyMA, 0.002g AIBN, 2.710g ethanol, and 2.710g deionized water of the product in step a into a 25mL reaction flask, freeze and evacuate with liquid nitrogen, repeat three times before sealing. tube, react in an oven at 70 °C for 7 h, take out the reaction flask and put it in an ice-water bath to stop the reaction to obtain PEG-b-P (DIPEMA-GlyMA) polymer vesicles.
[0046] Step c, take 0.1 g of the product in step b, dilute it 20 times with a mixed solvent of ethanol and water, then add ethylenediam...
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