HRID370382

反应详情

EQUATION

反应方程式

HRID 370382 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
210 °C

PROCEDURE

实验过程

A standard 1-liter esterification system was charged with 111 g of phthalic anhydride, 284 g of isodecyl alcohol and 0.5 g of catalyst ATC-II. The system was heated to reflux and the temperature was maintained at 210° C. at reduced pressure. At the end of 1.25 hours the water of reaction was collected and the acid number of the residue was measured to be 0.03 mg KOH/g. Heating was discontinued and excess alcohol removed as the pressure was reduced to 100 torr. Adjusting the temperature to 150° C., hydrolysis of the catalyst and removal of remaining alcohol was accomplished by steam distillation using 40 ml water during 35 minutes at 150° C. and 100 torr. After drying for 15 minutes at these conditions the cloudy crude product was cooled to 90° C. and filtered through a No. 1 Whatman paper to yield a clear residue product diisodecyl phthalate (DIDP) (nD25 =1.4850) having an acid number of 0.04 mg KOH/g and a color of 15 APHA.

WORKUP

后处理

  1. temperatureThe system was heated
  2. temperatureto reflux
  3. customwas collected
  4. temperatureHeating
  5. customexcess alcohol removed as the pressure
  6. customto 150° C.
  7. customhydrolysis of the catalyst and removal of remaining alcohol
  8. distillationwas accomplished by steam distillation
  9. customduring 35 minutes
  10. customat 150° C.
  11. dry with materialAfter drying for 15 minutes at these conditions the cloudy crude product
  12. temperaturewas cooled to 90° C.
  13. filtrationfiltered through a No