反应详情

温度

110 °C

A 750 ml reactor equipped with reflux condenser, thermometer, stirrer and metering device for epichlorohydrin is charged with 72.9 g (0.4 mol) of sorbitol and 1.25 g (0.008 mol) of tin difluoride in 88.5 g (0.957 mol) of epichlorohydrin, and the charge is heated to 110° C. Then, with stirring, 132.1 g (1.429 mol) of epichlorohydrin are added at a rate of 1.5 ml/min, while keeping the temperature at 110°-115° C. Stirring is continued for a further 8 hours at 125°-130° C. Excess epichlorohydrin is removed by distillation under a water jet vacuum and the residue is diluted with 441 g of methyl isobutyl ketone. With efficient stirring, 142.4 g (1.78 mol) of a 50% solution of sodium hydroxide are added dropwise over 1 hour and the reaction mixture is kept for another 2 hours at this temperature. The reaction mixture is neutralised by addition of dry ice and filtered, and the organic phase is dried over magnesium sulfate. The solvent is removed on a rotary evaporator and the residue is dried under vacuum (2 hours/60° C.), giving 155.2 g of sorbitol glycidyl ether for which the following analytical values are obtained: epoxy value: 5.5 eq/kg; total chlorine content 15.56%; hydrolysable chlorine content 1.09%; viscosity at 40° C.: 2460 mPa.s; average molecular weight Mn (GPC): 658.

1. customA 750 ml reactor equipped
2. temperaturewith reflux condenser
3. customat 110°-115° C
4. stirringStirring
5. customExcess epichlorohydrin is removed by distillation under a water jet vacuum
6. additionthe residue is diluted with 441 g of methyl isobutyl ketone
7. additionWith efficient stirring, 142.4 g (1.78 mol) of a 50% solution of sodium hydroxide are added dropwise over 1 hour
8. waitthe reaction mixture is kept for another 2 hours at this temperature
9. additionThe reaction mixture is neutralised by addition of dry ice
10. filtrationfiltered
11. dry with materialthe organic phase is dried over magnesium sulfate
12. customThe solvent is removed on a rotary evaporator
13. customthe residue is dried under vacuum (2 hours/60° C.)