Hexane → 2,3-Dibutyl-4-methylphenol

Participants

Reaction Conditions

Reaction Steps

Five gallons of the block copolymer cement product from Example VI containing about 2500 gms. of polymer is charged to a hydrogenation reactor together with an additional 40 lbs. of dry hexane. The reactor is flushed 6 times by pressuring to 50 psig with hydrogen and then releasing the pressure to about 5 psig. Then the hydrogenation catalyst is added which comprises 25 millimoles of Ni in nickel octoate-cyclohexene-triethyl aluminum in proportions of 1/1/3 respectively. The temperature is raised to 130°F and hydrogen introduced to a pressure of 150 psig. Periodically the system is repressured to 150 psig and samples are removed three times at several hours intervals. The temperature is maintained at 130°-160°F over a period of about 7 hours after which the reaction mixture is cooled to 120°F and vented several times. The product is dropped into a 55 gallon drum containing methanol and a small amount of antioxidant (dibutyl-p-cresol) to provide about 0.5 gm. of A.O. per 100 gms. of polymer. The product is filtered and rinsed several times with hexane. The copolymer is found to be about 100% hydrogenated and to have a glass transition temperature of -59°C and a melting point of 97°C. This product shows excellent impact strength and is used in the tests of Example VIII.

Provenance & Evidence