Method for precisely preparing aliphatic polyester by utilizing betaine
An aliphatic polyester and betaine technology, applied in the field of polymer synthesis chemistry, can solve problems such as limited application, and achieve the effects of narrow molecular weight distribution, controllable reaction, and no metal residues
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Embodiment 1
[0018] In a dry 10 mL polymerization tube, add valerolactone (0.23 mL, 2.5 mmol), 2.5 mL dichloromethane, betaine (0.018 g, 0.1 mmol), benzyl alcohol (10.3 μl, 0.1 mmol) in Magnetic stirring at 20°C for 5h. After the completion of the reaction, the reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of dichloromethane, and then added to the cold methanol solution, and polymer was precipitated. The white solid was obtained by centrifugal separation, which was transferred to a vacuum drying oven for drying. Polymer structure passes 1 H NMR and 13 C NMR identification, 1 For H NMR, please refer to the instructions attached figure 1 According to the analysis of the characteristic peaks on the spectrum, the polyvalerolactone is well synthesized. The molecular weight and degree of dispersion of the polymer are measured by GPC. The polymer is finally analyzed by time-of-flight mass spectrometry, the spectra are attached to the in...
Embodiment 2
[0020] In a dry 10 mL polymerization tube, add caprolactone (0.28 mL, 2.5 mmol), 2.5 mL dichloromethane, betaine (0.018 g, 0.1 mmol), benzyl alcohol (10.3 μl, 0.1 mmol) in Magnetic stirring at 20°C for 13h. After the completion of the reaction, the reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of dichloromethane, and then added to the cold methanol solution, and polymer was precipitated. The white solid was obtained by centrifugal separation, which was transferred to a vacuum drying oven for drying. Polymer structure passes 1 H NMR and 13 CNMR identification, 1 For H NMR, please refer to the instructions attached figure 2 According to the analysis of the characteristic peaks on the spectrum, the polycaprolactone is well synthesized. The molecular weight and degree of dispersion of the polymer are measured by GPC. The polymer is finally analyzed by time-of-flight mass spectrometry, the spectra are attached in the ins...
Embodiment 3
[0022] In a dry 10 mL polymerization tube, add valerolactone (0.23 mL, 2.5 mmol), 2.5 mL tetrahydrofuran, betaine (0.018 g, 0.1 mmol), and benzyl alcohol (10.3 μl, 0.1 mmol) at 20°C. Magnetic stirring for 7h. After the completion of the reaction, the reaction solution was rotary evaporated, and the obtained crude product was dissolved in a minimum amount of tetrahydrofuran, and then added to the cold methanol solution, and polymer was precipitated. The white solid was obtained by centrifugal separation, which was transferred to a vacuum drying oven for drying. The polymer was determined to have a conversion rate of 92% and a yield of 69%. M n / M w Is 1.12.
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