A hindered Lewis acid-base pair catalyzed method for the copolymerization of cyclic anhydrides and epoxy compounds into aliphatic polyesters
A technology of Lewis acid-base pair and epoxy compound, which is applied in hindered Lewis acid-base pair to catalyze the copolymerization of cyclic anhydride and epoxy compound into aliphatic polyester and the synthesis field of aliphatic polyester, which can solve the limitation of polyester application, Can not be recycled, unfavorable for large-scale industrial production and other issues
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Embodiment 1
[0025] Weigh 0.05g of indium oxyhydroxide nanoparticles and 3.84g of succinic anhydride into a reaction flask, and vacuumize; put 3mL of epichlorohydrin and 5mL of N,N-dimethylformamide into the reaction flask, and heat up to 80 ℃, stirred for 10 hours, and then cooled to room temperature to obtain a polymer; the polymer was dissolved from the reaction flask with chloroform, centrifuged and the catalyst was recovered, and n-hexane was used as a precipitating agent. Dry in vacuo to obtain 1.05 g of aliphatic polyester, and the polyester content in the aliphatic polyester is 99%.
[0026] The aliphatic polyester that embodiment 1 makes 1 H NMR spectrum, such as figure 2 shown. It can be seen from the figure that the aliphatic polyester has been successfully synthesized, and there is almost no polyether chain proton peak at 3.4-3.7ppm calculated by NMR, indicating that the polyester content in the copolymer is 99%.
Embodiment 2
[0028] Weigh 0.05g of indium oxyhydroxide nanoparticles and 3.84g of succinic anhydride into a reaction flask, and vacuumize; put 2.68mL of propylene oxide and 5mL of N,N-dimethylformamide into the reaction flask, and heat up to 100 ℃, heated for 10h, and then cooled to room temperature; the polymer was dissolved from the reaction flask with chloroform, centrifuged and the catalyst was recovered, and n-hexane was used as the precipitating agent. After the product was precipitated, it was dried in a vacuum oven at 80°C to obtain Aliphatic polyester 2.2g, the polyester content in this aliphatic polyester is 99%.
[0029] The aliphatic polyester that embodiment 2 makes 1 H NMR spectrum, such as image 3 shown. It can be seen from the figure that the aliphatic polyester has been successfully synthesized, and there is almost no polyether proton peak at 3.4-3.7ppm. The calculation of the NMR shows that the polyester content in the copolymer is 99%.
Embodiment 3
[0031] 0.05 g of indium oxide oxyhydroxide nanoparticles and 3.84 g of succinic anhydride were weighed and put into a reaction flask, and vacuumed. Pour 3.2mL epibromohydrin and 5mL N,N-dimethylformamide into the reaction flask, raise the temperature to 120°C, heat for 10h, then cool to room temperature; dissolve the polymer from the reaction flask with chloroform, Centrifuge and recover the catalyst, use n-hexane as the precipitant, precipitate the product, and dry it in a vacuum oven at 80°C to obtain 7.5 g of aliphatic polyester, the polyester content of which is 92%.
[0032] The aliphatic polyester that embodiment 3 makes 1 H NMR spectrum, such as Figure 4 shown. It can be seen from the figure that the protons of the polyester chain come out, and a small amount of polyether protons come out at 3.4-3.7ppm. The polyester content is calculated to be 92% by nuclear magnetic integration.
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