Preparation method of crystalline polylactic acid-glycolic acid
A technology of crystalline polylactic acid and glycolic acid, applied in the field of preparation of crystalline polylactic acid-glycolic acid materials, can solve the problems of reducing the crystallinity of PLGA, speeding up the degradation speed of PLGA, increasing the racemization of PLGA, etc., and achieving a simple and easy preparation process. the effect of expanding the application potential
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Embodiment 1
[0041] (1) Add 7.2g of poly-L-lactide and 1.3g of glycolide into a two-necked flask, add 0.0027g of catalyst stannous isooctanoate and 0.18g of initiator pentaerythritol, and use a vacuum pump to evacuate to 10Pa. Seal the flask and put it in an oven at 160°C for 4 hours, shaking it every 20 minutes. After the reaction is completed, maintain vacuum and cool to room temperature, dissolve the product with dichloromethane, then slowly add the solution to methanol in an amount more than ten times the volume of the solution to precipitate, and filter with suction to obtain 4arm-PLGA.
[0042] (2) Take 2 g of the 4arm-PLGA synthesized above and put it into a two-necked flask, add 10 mL of dichloromethane and 40 μL of dehydrated triethylamine, add a rotor in an ice-water bath and stir at 300 rpm. In addition, 0.02 g of triphosgene was dissolved in 5 mL of dichloromethane, and added dropwise to the stirred solution, and the stirring was continued for 4 h after the dropwise addition wa...
Embodiment 2
[0046](1) Add 4.3g poly-L-lactide and 4.3g glycolide into a two-necked flask, add 0.003g catalyst stannous isooctanoate and 0.045g initiator pentaerythritol, and use a vacuum pump to evacuate to 10Pa. Seal the flask and put it in an oven at 165°C for 4 hours, shaking it every 20 minutes. After the reaction is completed, maintain vacuum and cool to room temperature, dissolve the product with dichloromethane, then slowly add the solution to methanol in an amount more than ten times the volume of the solution to precipitate, and filter with suction to obtain 4arm-PLGA.
[0047] (2) Take 2 g of the 4arm-PLGA synthesized above and put it into a two-necked flask, add 20 mL of dichloromethane and 30 μL of dehydrated pyridine, add a rotor in an ice-water bath and stir at 300 rpm. In addition, 0.015 g of triphosgene was dissolved in 5 mL of dichloromethane, and added dropwise to the stirred solution, and the stirring was continued for 4 h after the dropwise addition was completed.
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Embodiment 3
[0051] (1) Add 1.3g poly-L-lactide and 7.2g glycolide into a two-necked flask, add 0.002g catalyst stannous isooctanoate and 0.17g initiator pentaerythritol, and use a vacuum pump to vacuum below 10Pa. Seal the flask, put it in an oven at 170°C for 6 hours, and shake it every 20 minutes. After the reaction, maintain a vacuum and cool to room temperature, dissolve the product with dichloromethane, and then slowly add the solution to an amount more than ten times the volume of the solution Precipitated in methanol, and obtained 4arm-PLGA by suction filtration.
[0052] (2) Take 2 g of 4arm-PLGA synthesized above and put it into a two-necked flask, add 30 mL of dichloromethane and 40 μL of dehydrated triethylamine, add a rotor in an ice-water bath and stir at 300 rpm. In addition, 0.02 g of triphosgene was dissolved in 5 mL of dichloromethane, and added dropwise to the stirred solution, and the stirring was continued for 3 h after the dropwise addition was completed.
[0053] (3...
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