Catalyst for aliphatic polycarbonate polymerization, preparation method and use method thereof
A technology of polycarbonate and catalyst, which is applied in the field of catalyst to achieve the effects of simple preparation, stable structure and simple operation
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Embodiment 1
[0019] Catalyst 2,2`-zinc diphenylcarboxylate [Zn(C 14 h 8 o 4 )·H 2 O] preparation.
[0020] Weigh 0.48g (2mmol) of biphenyl dicarboxylic acid into a 100mL Erlenmeyer flask equipped with a magnetic stirrer, add 20mL of methanol, and stir to dissolve. Under stirring at room temperature, slowly add a solution of 0.44g (2mmol) zinc acetate dissolved in 20mL of methanol, and a large amount of white precipitates will appear. Continue to stir and react for 0.5h, let it stand, and filter with suction. The precipitate was washed several times with methanol, transferred to a watch glass, and placed in a vacuum drying oven at 100° C. for 24 hours in vacuum to obtain 0.54 g of a white powdery solid product with a yield of 89%. IR(KBr): 1605(v as COO - ), 1402 (v s COO - ), 753(Zn-O)cm -1 .
Embodiment 2
[0022] Catalyst 2,2`-zinc diphenylcarboxylate [Zn(C 14 h 8 o 4 )·H 2 O] preparation.
[0023] Weigh 0.48g (2mmol) biphenyl dicarboxylic acid into a 100mL Erlenmeyer flask equipped with a magnetic stirrer, add 20mL 95% ethanol, and stir to dissolve. A solution of 0.55 g (2 mmol) of zinc acetate dissolved in 20 mL of 95% ethanol was slowly added under stirring at 60°C. After the addition is complete, continue to stir and react for 2.5 hours, then cool, let stand, and filter with suction. The precipitate was washed several times with ethanol, transferred to a watch glass, and placed in a vacuum drying oven at 100° C. for 24 hours in vacuum to obtain 0.52 g of a white powdery solid product with a yield of 86%. IR(KBr): 1605(v as COO - ), 1402 (v s COO - ), 753(Zn-O)cm -1 .
Embodiment 3
[0025] Copolymerization of carbon dioxide and cyclohexane oxide (solvent-free).
[0026] Put 0.10g of the catalyst 2,2`-zinc biphenyldicarboxylate and a stirrer into a 100mL stainless steel autoclave that has been vacuum-dried at 100°C in advance, heat up to 100°C and vacuum-dry for 12h, cool to room temperature, and fill with carbon dioxide to normal pressure . Add 10 mL (9.6 g) of epoxycyclohexane into the reaction kettle with a glass syringe, fill with carbon dioxide, keep the pressure at 2.5 MPa, stir with magnetic force, react at 80 ° C for 30 h, cool to room temperature, and stop the reaction.
[0027] The reaction solution was taken out, the unreacted epoxycyclohexane was distilled, the residue was dissolved in dichloromethane, filtered, the filtrate was washed with dilute acid, dilute alkali and distilled water successively, dried, and part of dichloromethane was recovered. Slowly drop the concentrated solution after evaporating dichloromethane into a sufficient amoun...
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