Preparation method of polylactide regulated by organic small molecule catalyst
A polylactide, small molecule technology, applied in the field of biodegradable polymer synthesis chemistry, can solve the problems of long reaction time, difficult to obtain controlled polymerization products, poor catalytic effect, etc., and achieves short process cycle and narrow molecular weight distribution index. , the effect of white color
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Embodiment 1
[0051] In a 5 mL polymerization tube, add L-lactide (0.290 g, 2 mmol), 3 mL of dichloromethane, guanidinium tetrafluoroborate (0.035 g, 0.15 mmol), (-)-spartine ( 34.5 microliters, 0.15 mmol), and 10.4 microliters (0.1 mmol) of benzyl alcohol were stirred magnetically at 40°C for 10 minutes. After the reaction was over, the reaction was terminated. The reaction solution was rotary evaporated, and a small amount of the reaction solution was taken to measure 1 H NMR to determine the reaction conversion. The obtained crude product was dissolved in a minimum amount of dichloromethane, and then added to a cold methanol solution, and a polymer was precipitated. Centrifuge to obtain a white solid, which is transferred to a vacuum oven for drying. The polymer structure was determined by determining the white solid product 1 H NMR with 13 C NMR identified, see figure 1 with figure 2 , Figure 4 is the SEC graph of lactide and organic alcohol at different ratios, wherein line ...
Embodiment 2
[0053] In a 5 mL polymerization tube, add D-lactide (0.435 g, 3 mmol), 3 mL of dichloromethane, guanidinium tetrafluoroborate (0.035 g, 0.15 mmol), (-)-spartine ( 34.5 microliters, 0.15 mmol), and 13.6 microliters (0.1 mmol) of phenylpropanol were stirred magnetically at 20°C for 40 minutes. After the reaction was over, the reaction was terminated. The reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of dichloromethane, and then added into a cold methanol solution, and a polymer was precipitated. Centrifuge to obtain a white solid, which is transferred to a vacuum oven for drying. polymer structure through 1 H NMR with 13 C NMR identification, molecular weight and molecular weight distribution of the polymer were determined by SEC. After determination, the transformation rate of polymer is 97%, and productive rate is 71%, M n / M w is 1.13.
Embodiment 3
[0055] In a 5 mL polymerization tube, add DL-type lactide (0.435 g, 3 mmol), 3 mL of dichloromethane, guanidinium tetrafluoroborate (0.035 g, 0.15 mmol), (-)-spartine ( 34.5 μl, 0.15 mmol), 0.014 g (0.1 mmol) of 6-azidohexanol, and stirred magnetically at 25°C for 30 minutes. After the reaction was over, the reaction was terminated. The reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of dichloromethane, and then added into a cold methanol solution, and a polymer was precipitated. Centrifuge to obtain a white solid, which is transferred to a vacuum oven for drying. polymer structure through 1 H NMR with 13 C NMR identification, molecular weight and molecular weight distribution of the polymer were determined by SEC. After determination, the transformation rate of polymer is 96%, and productive rate is 78%, M n / M w is 1.11.
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