A green and high-yield preparation method of aliphatic polycarbonate with zero catalyst addition
A polycarbonate and aliphatic technology, which is applied in the field of green high-yield preparation of aliphatic polycarbonate with zero catalyst addition, can solve the problems of small molecule organics that cannot be evaluated for safety, high toxicity, difficult conversion rate, etc., and achieve huge application transformation Potential, low equipment requirements, simple and efficient preparation method
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Embodiment 1
[0027] 1) Weigh 0.32 g of trimethylene carbonate, a six-membered ring carbonate, and put it into a glass container (reaction bottle), vacuum-dry it with an oil pump for 0.5 hour and seal it under the same conditions. Such as figure 2 As shown, the container was placed in an oil bath, under magnetic stirring (150rpm), intermittent ultrasonic (power 900W, ultrasonic 3s off 9s), 100 ° C reaction for 5 hours. After the polymerization was completed, the product was dissolved in 2 mL of dichloromethane and dropped into 40 mL of methanol to obtain a white precipitate. Pour off the liquid and wash the precipitate twice with clean methanol. After drying, the yield was 55% by weight. GPC (THF is used as mobile phase, and polystyrene is used as standard sample) records the weight-average molecular weight of 1.16×10 5 Dalton, dispersion 1.59.
[0028] 2) As a comparison, without ultrasound, the yield was 47%, and the weight average molecular weight was 9.65×10 4 Dalton, dispersion 1...
Embodiment 2
[0030] 1) Weigh 0.32 g of trimethylene carbonate, a six-membered ring carbonate, and put it into a glass container, dry it in vacuum with an oil pump for 0.5 hour, and seal it under the same conditions. Such as figure 2 As shown, the container was placed in an oil bath, under magnetic stirring (150rpm), intermittent ultrasonic (power 900W, ultrasonic 3s off 9s), 100 ° C reaction for 14 hours. After the polymerization was completed, the product was dissolved in 2 mL of dichloromethane and dropped into 40 mL of methanol to obtain a white precipitate. The liquid was poured out, and the precipitate was washed twice with clean methanol. It was dried under reduced pressure and weighed, and the yield was 96%. The weight average molecular weight measured by GPC is 1.67×10 5Dalton (THF as mobile phase, polystyrene as standard sample), dispersion 1.73. The GPC spectrum, NMR spectrum and product diagram of the obtained product are shown in Figure 3-5 .
[0031] 2) As a comparison,...
Embodiment 3
[0033] 1) Weigh 0.32 g of trimethylene carbonate, a six-membered ring carbonate, and put it into a specific container, vacuum-dry it with an oil pump for 0.5 hour and seal it under the same conditions. Such as figure 2 As shown, the container was placed in an oil bath, under magnetic stirring (150 rpm), intermittent ultrasonic (power 900W, ultrasonic 3s off 9s), 120 ° C for 5 hours. After the polymerization was completed, the product was dissolved in 2 mL of dichloromethane, and dropped into 40 mL of methanol solvent to obtain a white precipitate. The liquid was poured out, and the precipitate was washed twice with clean methanol. After drying, the weighing yield was 90%. Weight average molecular weight 6.6×10 4 Dalton, dispersion 1.57.
[0034] 2) As a comparison, without ultrasound, the yield was 85%, and the weight average molecular weight was 9.4×10 4 Dalton, dispersion 1.63. The results show that although increasing the reaction temperature to 120°C can effectively ...
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