One-step preparation method of cross-linked carbon dioxide copolymer
A technology of carbon dioxide and copolymers, which is applied in the field of carbon dioxide copolymer materials, can solve problems such as the dimensional stability of polymers, the reduction of polymer yield and molecular weight, and the inability to significantly increase catalytic efficiency, etc., to achieve convenient thermal processing and molding, good Effects of thermal stability and short polymerization time
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Embodiment 1
[0020] Put 1 gram of zinc glutarate in an autoclave, vacuum-dry at 120°C for 8 hours, then cool to room temperature, then put 2.45 g of glycidyl furoate and 1.76 g of citraconic anhydride in the autoclave, and replace with nitrogen Air three times, then vacuum, then inject 220mL of propylene oxide, and fill with carbon dioxide. The polymerization temperature was maintained at 55°C, the carbon dioxide pressure was 4.2 MPa, and the reaction was stirred for 24 hours. After the reaction, the polymer was dissolved in 200ml of dichloromethane, and some of the gel did not dissolve. Then 10mL of 5% hydrochloric acid was added to dissolve the zinc glutarate catalyst and washed with distilled water until the pH value was neutral. The polymer was precipitated with ethanol and dried under vacuum at 80°C for 24 hours to obtain 69 g of polymer. The measured gel content was 13%. The 5% thermal decomposition temperature is 253°C, and the maximum thermal decomposition temperature is 281°C. T...
Embodiment 2
[0022] Put 1 gram of zinc glutarate in an autoclave, vacuum dry at 120°C for 8 hours, then cool to room temperature, then put 6.7 grams of glycidyl furoate and 4.8 grams of citraconic anhydride in the autoclave, and replace with nitrogen Air three times, then vacuum, and then inject 300mL of propylene oxide, and fill with carbon dioxide. The polymerization temperature was maintained at 60°C, the carbon dioxide pressure was 4.2 MPa, and the reaction was stirred for 24 hours. After the reaction, the polymer was dissolved in 200ml of dichloromethane, and some of the gel did not dissolve. Then 10mL of 5% hydrochloric acid was added to dissolve the zinc glutarate catalyst and washed with distilled water until the pH value was neutral. The polymer was precipitated with ethanol and dried under vacuum at 80°C for 24 hours to obtain 72 g of polymer. The measured gel content is 20%. The 5% thermal decomposition temperature is 260°C, and the maximum thermal decomposition temperature is ...
Embodiment 3
[0024] Put 1 g of zinc glutarate in an autoclave, vacuum-dried at 120°C for 8 hours, then cool to room temperature, then put 19.2 g of glycidyl furoate and 13.8 g of citraconic anhydride in the autoclave, and replace with nitrogen Air three times, then vacuum, and then inject 430mL of propylene oxide, and fill with carbon dioxide. The polymerization temperature was maintained at 70°C, the carbon dioxide pressure was 4.2 MPa, and the reaction was stirred for 20 hours. After the reaction, the polymer was dissolved in 200ml of dichloromethane, and some of the gel did not dissolve. Then 10mL of 5% hydrochloric acid was added to dissolve the zinc glutarate catalyst and washed with distilled water until the pH value was neutral. The polymer was precipitated with ethanol and dried under vacuum at 80°C for 24 hours to obtain 76 g of polymer. The measured gel content was 28%. The 5% thermal decomposition temperature is 262°C, and the maximum thermal decomposition temperature is 288°C....
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