Biodegradable polymer, and preparation method
A biodegradable and polymer technology is applied in the field of new biodegradable polymers and their preparation, which can solve the problems of difficult reaction control, long reaction time, long reaction time, etc. The effect of good biocompatibility and simple synthesis process
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[0038] The preparation method of 5-hydroxylevulinic acid:
[0039] In a three-necked flask with stirring, dropping funnel and condenser, add 58 g of levulinic acid and 500 mL of methanol, place it in a 30°C water bath, and add 80 g of liquid bromine dropwise with stirring. After the dropwise addition, the reaction was continued for 8 hours at 30-40°C, and then the reaction was continued for 1 hour under reflux. The methanol was distilled off under reduced pressure, 500 mL of ether and 100 mL of water were added, and the layers were allowed to stand for separation. The ether layer was washed with an excess of saturated sodium bicarbonate solution and dried with anhydrous sodium sulfate and 4A molecular sieve. The ether was evaporated to obtain a brominated mixture. The bromination mixture was added to a mixed solvent of V (ether): V (cyclohexane) = 1:1, and recrystallized at low temperature (-20℃~-40℃) to obtain white needle-like 5-bromolevulin Methyl acid crystals. Methyl 5-bromol...
Embodiment 1
[0041] Add 5 grams of 5-hydroxylevulinic acid and 4.51 grams of 1,4-butanediol (molar ratio 1:1) into a 50ml flask, stir and mix well, and perform dehydration and esterification reaction at 130°C for 3 hours , A viscous prepolymer was obtained.
[0042] Add the stannous chloride / p-toluenesulfonic acid composite catalyst in an equimolar ratio of 0.7wt% of the total monomer mass to the prepolymer, and after mixing uniformly, add the reaction mixture to the polytetrafluoroethylene preheated to 130°C In the ethylene mold, the reaction was continued at 150°C for 37 minutes to obtain a biodegradable polymer prepared from 5-hydroxylevulinic acid and 1,4-butanediol with a gel content of 97.8% and a glass transition temperature of 22 ℃. See the infrared spectrum figure 1 . At 1405cm -1 The deformation vibration absorption peaks of methylene appear in the vicinity, and the absorption peaks of the terminal hydroxyl and carboxyl groups of the polymer are at 3440cm -1 Nearby, 1172cm -1 It is ...
Embodiment 2-5
[0044] Other conditions are the same as in Example 1, but the molar ratios of 5-hydroxylevulinic acid (5-HLA) and 1,4-butanediol (BDO) are 1:0.2, 1:0.4, 1:0.67, 1: 1.5, 1:2.3, 1:4, 1:6, the gel content of the obtained biodegradable polymer is 97.2%, 96.3%, 95.8%, 97.6%, 91.3%, 91.1%, 89.6%, respectively. The melting temperature is 60.1℃, 46.3℃, 30.4℃, 14.8℃, -9.2℃, -15.4℃, -31.4℃, respectively. The DSC curve of the biodegradable polymer prepared under the condition that the molar ratio of 5-hydroxylevulinic acid to 1,4-butanediol is 1:4 figure 2 , The relationship between the glass transition temperature of the polymer obtained under different monomer ratios and the monomer ratio is shown in image 3 . image 3 Also includes the glass transition temperature data in Example 1.
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