Gamma-Butyrolactone → Lactic acid hydroxybutyric acid

Temperature

200 °C

A 90% aqueous solution of L-lactic acid (32.4 g) and 3.75 g of γ-butyrolactone were put in a reaction vessel equipped with a stirrer and a nitrogen-introducing tube. After substitution of nitrogen gas was carried out three times, the temperature was raised by 10° C. per minute to 120° C. in a stream of nitrogen, and the mixture was concentrated at 120° C. for 5 hours with stirring. To the resulting concentrate was added 2.2 g of commercially available synthetic aluminum silicate containing 17% aluminum oxide. Then the temperature was raised to 200° C. and the pressure was reduced gradually to 20 mmHg over 30 minutes, followed by stirring at 220±15° C. for 3 hours. After the pressure was reduced gradually to 1 mmHg over 30 minutes, the mixture was stirred at 210±10° C. for 18 hours to give copolymer in the molten state. The product was cooled to room temperature to give 21.2 g of lactic acid-hydroxybutyric acid copolymer as a dark brown solid. The weight-average molecular weight of this copolymer was 65,000.

1. customequipped with a stirrer
2. additiona nitrogen-introducing tube
3. temperaturethe temperature was raised by 10° C. per minute to 120° C. in a stream of nitrogen
4. concentrationthe mixture was concentrated at 120° C. for 5 hours
5. concentrationTo the resulting concentrate
6. additionwas added 2.2 g of commercially available synthetic aluminum silicate containing 17% aluminum oxide
7. stirringby stirring at 220±15° C. for 3 hours
8. waitAfter the pressure was reduced gradually to 1 mmHg over 30 minutes
9. stirringthe mixture was stirred at 210±10° C. for 18 hours
10. customto give copolymer in the molten state
11. temperatureThe product was cooled to room temperature

ORD record

ord-b6f8906653f349a8af266a52f41e6113

Source dataset

uspto-grants-1999_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05952455