Poly (2,2-dimethylene dioxy group-1, 3 propylene glycol carbonic ester), preparaton method and application
A dimethylene dioxy, propylene carbonate technology, applied in the field of polymer chemistry, can solve the problem of difficult to obtain higher molecular weight, etc., to improve biocompatibility, increase glass transition temperature, improve hydrophilicity Effect
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example 1
[0027] The preparation of 1,3-dioxolane-2,2-dimethanol: at room temperature, slowly add ( It is best to add within 2 hours) containing 50.0 grams (0.23 moles) of 1,3-dioxolane-2,2-dicarboxylic acid diethyl ester in 200 ml of tetrahydrofuran solution, and then reacted for 2 hours, adding 50 ml ethyl acetate to decompose excess lithium aluminum hydride, and then add 50 ml of water to continue the reaction for 2 hours. Filter, wash the solid with 100 ml THF 3 times, dry the resulting filtrate with anhydrous sodium sulfate, evaporate the solvent under reduced pressure, and distill the residual liquid under reduced pressure, collect the fraction at 130-2°C / 35Pa to obtain 22.54 g of colorless or light yellow Viscous liquid 1,3-dioxolane-2,2-dimethanol, yield 73%.
[0028] The preparation of 2,2-dimethylene dioxy-1,3-propanediol carbonate: at 0°C, add 13.40 grams (0.1 moles) of 1,3-dioxolane-2,2-dimethanol and 22.80 g (0.21 mol) of ethyl chloroformate in 500 ml of anhydrous tetrahy...
example 2
[0030] The preparation of poly(2,2-dimethylene dioxy-1,3-propanediol carbonate): the 2,2-dimethylene dioxy-1,3-propanediol carbonate monomer of 0.3203g and 20 microliters of anhydrous toluene solution of 0.1 mol / liter stannous isooctanoate are successively transferred to a dry polymerization tube with magnets, the solvent is removed under reduced pressure, and argon gas is introduced, and this is repeated three times. Seal the tube down, place the polymerization tube in an oil bath preheated to 110°C for 24 hours, add 2 milliliters of dichloromethane to the polymerization tube to dissolve the polymer, and reprecipitate with 40 milliliters of methanol. °C for 24 hours under vacuum. The yield was 91.1%, the number average molecular weight was 44200, and the polydispersity was 1.81. IR (KBr): 1758.7cm -1 (vs, C=O), 1255.3 cm -1 , 1181.9cm -1 , 1043.0cm -1 (vs, C-O-C); 1 HNMR (300MHz): 4.181ppm (4H, s, CH 2 OCOCH 2 ), 4.012ppm (4H, s, OCH 2 CH 2 O); 13CNMR (300MHz): 153...
example 3
[0032] The preparation of poly(2,2-dimethylene dioxy-1,3-propanediol carbonate): the 2,2-dimethylene dioxy-1,3-propanediol carbonate monomer of 0.3203g and 10 microliters of 0.1 mol / liter stannous isooctanoate in anhydrous toluene were successively transferred to a dry polymerization tube with magnets, the solvent was removed under reduced pressure, and argon gas was introduced, and so repeated three times, in high vacuum Seal the tube down, place the polymerization tube in an oil bath preheated to 110°C for 24 hours, add 2 milliliters of dichloromethane to the polymerization tube to dissolve the polymer, and reprecipitate with 40 milliliters of methanol. °C for 24 hours under vacuum. The yield was 84.3%, the number average molecular weight was 42400, and the polydispersity was 1.48.
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