Diisobutyl phthalate → Diisobutyl phthalate

Temperatur

130 °C

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.

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

ORD-Eintrag

ord-d14d7daef79448959800781d8504d1ca

Quelldatensatz

uspto-grants-1996_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05583188