反应详情

温度

85 °C

A 2000 ml glass reaction flask was equipped with a stirrer, thermometer and condenser, Dean-Stock trap air inlet and heating mantle and used as the reaction vessel. 300 grams of a trihydroxyfunctional polycaprolactone polyol with an average hydroxyl number of 310 and an average molecular weight of 540 (TONE-0305 obtained from Union Carbide Corporation), 88.4 g. of glacial acrylic acid, 150 ml. of benzene, 5 ml. of concentrated sulfuric acid and 5 g. of hydroquinone were added to the reaction flask at room temperature. The contents of the flask were then heated to about 85° C. over a period of one hour and maintained at reflux at atmospheric pressure until no further water was produced (about 4.5 hours). During the reaction, air was continually bubbled through the reaction. The reaction mixture was cooled to about 60° C. in a separatory funnel and about 50 ml of benzene added. Then, about 200 g of a 15 percent aqueous sodium hydroxide solution was dripped through the separatory funnel. A second aliquot of 200 g of a 15 percent aqueous sodium hydroxide solution was added and then the contents shaken. Excess acid and hydroquinone inhibitor were washed out by shaking the solution three times with 50 g of a 15 percent aqueous sodium hydroxide solution. After the contents settled, 10 g of magnesium sulfate was added while stirring to remove any remaining water, then the contents filtered to remove the magnesium sulfate. 100 parts per million of methylethyl hydroquinone based on the final product was added and the contents were then stripped of solvent. A 60 to 70% yield was obtained. The product had a viscosity of 250 centipoise.

1. customwas equipped with a stirrer
2. temperaturethermometer and condenser, Dean-Stock trap air inlet and heating mantle
3. temperaturemaintained
4. customwas produced (about 4.5 hours)
5. customDuring the reaction, air
6. customwas continually bubbled through the reaction
7. temperatureThe reaction mixture was cooled to about 60° C. in a separatory funnel
8. additionabout 50 ml of benzene added
9. additionA second aliquot of 200 g of a 15 percent aqueous sodium hydroxide solution was added
10. washExcess acid and hydroquinone inhibitor were washed out
11. stirringby shaking the solution three times with 50 g of a 15 percent aqueous sodium hydroxide solution
12. addition10 g of magnesium sulfate was added
13. stirringwhile stirring
14. customto remove any remaining water
15. filtrationthe contents filtered
16. customto remove the magnesium sulfate
17. additionwas added
18. customA 60 to 70% yield was obtained