Ethanol → Phthalate

Participants

Reaction Conditions

Reaction Steps

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.

Provenance & Evidence