Preparation method of polylactic acid-chitose graft copolymer
A technology of graft copolymer and chitosan, which is applied in the field of preparation of biomedical materials, can solve problems such as complicated process routes, and achieve the effect of simple synthesis method, mild reaction conditions and low energy consumption
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Embodiment 1
[0015] Weigh 0.25g chitosan (90%) and add it to 6g L-lactic acid (80%), stir at room temperature to fully dissolve it, pour the solution into a 250ml three-necked flask and add an appropriate amount (about 200ml) of dichloromethane , Azeotropic dehydration at 40°C for 2-4h in the rectification water separation device. After dehydration, 0.184g of DMAP was added to the solution. After fully dissolving, it was cooled to 0°C in an ice-water bath, and then 5.846g of DCC was added within a short period of time. A condensing reflux device was used to ensure that the volume of the reaction solution was maintained at 60 ml, and the reaction was carried out at room temperature for 24 hours.
[0016] After the reaction was finished, the white precipitate dicyclohexyl urea (DCU) generated by the reaction was removed by suction filtration, the resulting filtrate was washed 3 times with 0.5M dilute hydrochloric acid, 1-2 times with distilled water, and the organic phase after water separat...
Embodiment 2
[0018] Weigh 0.25g chitosan (50%) and add it to 6g D-lactic acid (80%), stir at room temperature to fully dissolve it, pour the solution into a 250ml three-necked flask and add an appropriate amount (about 200ml) of dichloromethane , Azeotropic dehydration at 40°C for 2-4h in the rectification water separation device. After dehydration, 0.184g of DMAP was added to the solution. After fully dissolving, it was cooled to 0°C in an ice-water bath, and then 5.846g of DCC was added within a short period of time. A condensing reflux device was used to ensure that the volume of the reaction solution was maintained at 60 ml, and the reaction was carried out at room temperature for 24 hours.
[0019] After the reaction was finished, the white precipitate dicyclohexyl urea (DCU) generated by the reaction was removed by suction filtration, the resulting filtrate was washed 3 times with 0.5M dilute hydrochloric acid, 1-2 times with distilled water, and the organic phase after water separat...
Embodiment 3
[0021] Take by weighing 0.25g chitosan (90%) and join in 6g L-lactic acid (80%), stir at room temperature and make it fully dissolve, solution is poured in the 250ml there-necked flask and adds appropriate (about 200ml) toluene, in Azeotropic dehydration at 90°C for 2-4 hours in a rectification water separation device. After dehydration, add 0.56g of AlCl to the solution 3 . A condensing reflux device was used to ensure that the volume of the reaction solution was maintained at 60ml, and the reaction was carried out at 100°C for 4h.
[0022] After the reaction, the AlCl was removed by suction filtration 3 , the resulting filtrate was washed 1-2 times with distilled water, and the organic phase after water separation was washed with anhydrous Na 2 SO 4 dry. Overnight at room temperature, filter to remove Na 2 SO 4 , the reaction solution was concentrated by rotary evaporation, poured into absolute ethanol for purification, and a white precipitate was obtained, which was ...
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