Condensation polymerization method for preparing hydroxylated acid condensation polymer
A technology of condensation polymerization and hydroxy acid, applied in the field of condensation polymerization for preparing hydroxy acid polycondensate, can solve the problems of undesired removal of catalyst post-treatment, technical difficulty of catalyst, shortage of resources, etc., achieves excellent biocompatibility, improves catalysis Effect, effect of large molecular weight
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Embodiment 1
[0044] Add 50 grams of 90% L-lactic acid aqueous solution into a 250 mL three-neck round bottom flask, start magnetic stirring, and heat in an oil bath. Dehydrate at 100°C for 2 hours under normal pressure; then gradually reduce the pressure to 1 300Pa (10 mm Hg), raise the temperature to 130°C, and dehydrate for 2 hours; the L-lactic acid with a weight average molecular weight of 520 is obtained. polymer; then continue dehydration for 4 hours at 150° C. and 520 Pa (4 mm Hg), to obtain a lactic acid oligomer with a weight average molecular weight of 1610. After cooling, add 0.002 moles of methyltriphenylphosphonium bromide to a three-necked round-bottomed flask, mix well, gradually raise the temperature to 170°C, and gradually reduce the pressure to 130Pa (1 mm Hg), After 10 hours of reaction, the yield of polylactic acid was 90.5%, the weight average molecular weight measured by gel permeation chromatography was 12870, and the polydispersity index was 1.36.
Embodiment 2
[0046]The preparation of lactic acid oligomer was as in Example 1. Add 0.002 mole of tetrabutylammonium chloride in the lactic acid oligomer of gained, gradually warming up to 170 ℃, gradually reducing pressure to 130Pa (1 mm Hg), react for 10 hours, the productive rate of polylactic acid is 84.7%, The weight average molecular weight measured by gel permeation chromatography was 6870, and the polydispersity index was 1.48.
Embodiment 3
[0048] The preparation of lactic acid oligomer was as in Example 1. Add 0.004 mole of N-butylpyridine bromide to the obtained lactic acid oligomer, gradually heat up to 170°C, gradually reduce the pressure to 130Pa (1 mm Hg), react for 10 hours, and the yield of polylactic acid is 93.1%. , the weight average molecular weight measured by gel permeation chromatography is 11000, and the polydispersity index is 1.26.
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