HRID1080853

反应详情

EQUATION

反应方程式

HRID 1080853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

Anhydrous magnesium chloride (4.76 g; 50 millimoles), 25 ml of decane and 23.4 ml (150 mmoles) of 2-ethylhexyl alcohol were heated at 130° C. for 2 hours to form a uniform solution. Phthalic anhydride (1.11 g; 7.5 mmoles) was added to the solution, and the mixture was further stirred at 130° C. for 1 hour to dissolve phthalic anhydride in the aforesaid uniform solution. The uniform solution so obtained was cooled to room temperature, and added dropwise over the course of 1 hour to 200 ml (1.8 moles of titanium tetrachloride kept at -20° C. After the addition, the temperature of the mixed solution was elevated to 110° C. over the course of 4 hours. When the temperature reached 110° C., 2.68 ml (12.5 mmoles) of diisobutyl phthalate was added. The mixture was maintained at the same temperature for 2 hours with stirring. After the 2-hour reaction, the solid portion was collected by hot filtration. The solid portion was re-suspended in 200 ml of titanium tetrachloride, and again reacted at 110° C. for 2 hours. After the reaction, the solid portion was collected again by hot filtration and washed fully with decane and hexane at 110° C. until no free titanium compound was detected from the washing. The solid titanium catalyst component (A) prepared by the above method was stored as a hexane slurry, but a part of it was dried to examine its composition. The solid titanium catalyst component (A) obtained in this way comprised 3.1% by weight of titanium, 56.0% by weight of chlorine, 17.0% by weight of magnesium and 20.9% by weight of diisobutyl phthalate.

WORKUP

后处理

  1. customto form a uniform solution
  2. customThe uniform solution so obtained
  3. temperaturewas cooled to room temperature
  4. customkept at -20° C
  5. additionAfter the addition
  6. customwas elevated to 110° C. over the course of 4 hours
  7. customreached 110° C.
  8. temperatureThe mixture was maintained at the same temperature for 2 hours
  9. stirringwith stirring
  10. customAfter the 2-hour reaction
  11. filtrationthe solid portion was collected by hot filtration
  12. customagain reacted at 110° C. for 2 hours
  13. customAfter the reaction
  14. filtrationthe solid portion was collected again by hot filtration
  15. washwashed fully with decane and hexane at 110° C. until no free titanium compound
  16. customThe solid titanium catalyst component (A) prepared by the above method
  17. customa part of it was dried