邻苯二甲酸二异丁酯

反应条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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. to form a uniform solution The uniform solution so obtained was cooled to room temperature kept at -20° C After the addition was elevated to 110° C. over the course of 4 hours reached 110° C. 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 again reacted at 110° C. for 2 hours After the reaction the solid portion was collected again by hot filtration washed fully with decane and hexane at 110° C. until no free titanium compound The solid titanium catalyst component (A) prepared by the above method a part of it was dried

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a stirred reactor 28.4 g of MgCl2, 49.5 g of anhydrous ethanol, 10 ml of vaseline oil ROL OB/30, 100 ml of silicone oil having a viscosity of 350 cs were added. The mixture was heated at 120° C. until MgCl2 was dissolved. The hot reaction mixture was then transferred to a 1.5 l reactor equipped with a Ultra Turrax T-45 N stirrer, containing 150 cm3 of vaseline oil and 150 cm3 of silicone oil. The temperature was maintained at 120° C. whilst stirring for 3 minutes at 3000 RPM. The mixture was then discharged in a 2 liter stirred tank containing 1 l of anhydrous n-heptane cooled to 0° C. whilst stirring at a speed of 6 m/sec for about 20 minutes, maintaining the temperature at 0° C. The particles so obtained, after washing with n-hexane, were subjected to a thermal treatment in a nitrogen stream, at temperatures ranging from 50° to 150° C. until spherical particles were obtained having a residual alcohol content of about 35% by weight. 25 g of this product were charged into a stirred reactor containing 625 ml of TlCl4 at 0° C. and under stirring. The mixture was then heated to 100° C. for one hour and then left to cool. When the temperature of 40° C. was reached, diisobutyl phthalate was added in quantities such to give a molar ratio of magnesium to phthalate of 8. The mixture was heated to 100° C. for 2 hours under stirring and then the solid was left to settle. The hot liquid was removed by syphoning. Then 500 ml of TiCl4 was added and the mixture was heated to 120° C. for 1 hour whilst stirring. After settling, the hot liquid was removed by syphoning and the solid was washed with n-hexane. was dissolved The hot reaction mixture was then transferred to a 1.5 l reactor equipped with a Ultra Turrax T-45 N stirrer stirred tank cooled to 0° C. whilst stirring at a speed of 6 m/sec for about 20 minutes maintaining the temperature at 0° C The particles so obtained after washing with n-hexane ranging from 50° to 150° C. until spherical particles were obtained under stirring The mixture was then heated to 100° C. for one hour left to cool the temperature of 40° C.

反应条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 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. to form a uniform solution The uniform solution so obtained was cooled to room temperature kept at -20° C After the addition was elevated to 110° C. over the course of 4 hours reached 110° C. 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 again reacted at 110° C. for 2 hours After the reaction the solid portion was collected again by hot filtration washed fully with decane and hexane at 110° C. until no free titanium compound The solid titanium catalyst component (A) prepared by the above method a part of it was dried

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a stirred reactor 28.4 g of MgCl2, 49.5 g of anhydrous ethanol, 10 ml of vaseline oil ROL OB/30, 100 ml of silicone oil having a viscosity of 350 cs were added. The mixture was heated at 120° C. until MgCl2 was dissolved. The hot reaction mixture was then transferred to a 1.5 l reactor equipped with a Ultra Turrax T-45 N stirrer, containing 150 cm3 of vaseline oil and 150 cm3 of silicone oil. The temperature was maintained at 120° C. whilst stirring for 3 minutes at 3000 RPM. The mixture was then discharged in a 2 liter stirred tank containing 1 l of anhydrous n-heptane cooled to 0° C. whilst stirring at a speed of 6 m/sec for about 20 minutes, maintaining the temperature at 0° C. The particles so obtained, after washing with n-hexane, were subjected to a thermal treatment in a nitrogen stream, at temperatures ranging from 50° to 150° C. until spherical particles were obtained having a residual alcohol content of about 35% by weight. 25 g of this product were charged into a stirred reactor containing 625 ml of TlCl4 at 0° C. and under stirring. The mixture was then heated to 100° C. for one hour and then left to cool. When the temperature of 40° C. was reached, diisobutyl phthalate was added in quantities such to give a molar ratio of magnesium to phthalate of 8. The mixture was heated to 100° C. for 2 hours under stirring and then the solid was left to settle. The hot liquid was removed by syphoning. Then 500 ml of TiCl4 was added and the mixture was heated to 120° C. for 1 hour whilst stirring. After settling, the hot liquid was removed by syphoning and the solid was washed with n-hexane. was dissolved The hot reaction mixture was then transferred to a 1.5 l reactor equipped with a Ultra Turrax T-45 N stirrer stirred tank cooled to 0° C. whilst stirring at a speed of 6 m/sec for about 20 minutes maintaining the temperature at 0° C The particles so obtained after washing with n-hexane ranging from 50° to 150° C. until spherical particles were obtained under stirring The mixture was then heated to 100° C. for one hour left to cool the temperature of 40° C.