HRID1158185

反应详情

EQUATION

反应方程式

HRID 1158185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
30 °C

PROCEDURE

实验过程

To 158.5 g of 2,4-toluene diisocyanate was added 240 g of methyl ethyl ketone as a solvent, and 107.5 g of 4,4′-diaminodiphenyl sulfone was added thereto in the form of powder at 30° C. with stirring at 400 rpm over a period of 8 hours. After 1 hour, 26 g of methyl ethyl ketone was added thereto and stirred for another 15 hours to obtain a white viscous slurry reaction mixture. Then, a solution of 89.5 g of phenol in 15.8 g of methyl ethyl ketone was poured into the reaction mixture to be dissolved therein, after which 9.3 g of a 1 wt % solution of triethylamine in methyl ethyl ketone was added thereto as a catalyst over a period of 2 hours, and the reaction was uninterruptedly carried out for 1 hour. Thereafter, the reaction mixture was cooled to 20° C. and continuously stirred for 3 hours to obtain a slurry containing slightly yellow crystals precipitated therein. The slurry was freed of the solvent and concentrated under reduced pressure to be solidified, after which the resulting solid was ground and then dried overnight in a vacuum to obtain 355 g of a urea-urethane composition as slightly yellow powder.

WORKUP

后处理

  1. waitAfter 1 hour
  2. stirringstirred for another 15 hours
  3. customto obtain
  4. customa white viscous slurry reaction mixture
  5. dissolutionto be dissolved
  6. waitas a catalyst over a period of 2 hours
  7. waitthe reaction was uninterruptedly carried out for 1 hour
  8. temperatureThereafter, the reaction mixture was cooled to 20° C.
  9. stirringcontinuously stirred for 3 hours
  10. customto obtain a slurry
  11. additioncontaining slightly yellow crystals
  12. customprecipitated
  13. concentrationconcentrated under reduced pressure
  14. customdried overnight in a vacuum