Epichlorohydrin → Diglycidyl ether

Temperature

118 °C

To a 5-liter, 4-necked round-bottomed flask fitted with a condenser, addition funnel, stirrer, and thermometer were charged 1260 g (1.71 moles) above polyisopropylphenol. A 50% NaOH solution (137.3 g, 1.71 moles) was then added and the mixture heated with stirring to reflux (118° C.) and held there for 0.5 hours. The mixture was vacuum stripped at 100° (0.5 mm) to remove water, recharged with 50 g toluene, and restripped (105°, 0.2 mm) to azeotropically remove the last traces of water. The reaction was then cooled to 65° C. and 792 g (8.55 moles) epichlorohydrin was added and the reaction heated to reflux (~120° C.) for three hours. The excess epichlorohydrin was then vacuum stripped at 120° (0.05 mm) to yield ~1450 g of the crude glycidyl ether.

1. customTo a 5-liter, 4-necked round-bottomed flask fitted with a condenser, addition funnel, stirrer
2. additionthermometer were charged 1260 g (1.71 moles) above polyisopropylphenol
3. temperaturethe mixture heated
4. customstripped at 100°
5. customto remove water
6. custom(105°, 0.2 mm)
7. customto azeotropically remove the last traces of water
8. temperatureThe reaction was then cooled to 65° C.
9. temperaturethe reaction heated
10. temperatureto reflux (~120° C.) for three hours
11. customstripped at 120°

ORD record

ord-072ccbeeb7fa4113a7fdf461a3000432

Source dataset

uspto-grants-1981_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04259086