反应详情

A quartz tube 40 cm×16 mm, inside diameter, with Vigreux indentations 1" above the top of the bottom joint was packed with 3 cm of quartz rings, 28 cm (equivalent to 44.16 grams) of the calcium-nickel phosphate catalyst of formula I, which had previously been calcined at about 800° for a period of about 17 hours and then filled with additional quartz rings (for heat transfer). Thermocouples were placed on the side of the tube and the tube placed in a vertical furnace. At the top of the tube was placed a manifold from which the air and liquid feeds were added. At the bottom of the tube were placed in series three three-necked flasks, the first two being immersed in ice/water baths. The catalyst bed was heated to a temperature between 300°-500° with an air flow of 0.15 ft3 /hr. Then the liquid feed composed of phenol, water, and isopropylphenol in the molar ratio of 2.8:2.0:1.0 was introduced to provide an addition rate of 0.15 ml/min. After specified volumes of feed had been introduced, the products (phenol, water, the propylphenol and propenylphenol) were collected from the receiver and analyzed for para-isopropenylphenol content by NHMR spectroscopy (proton nuclear magnetic resonance). Table I shows the results of para-isopropenylphenol formation as a function of the moles of para-isopropylphenol used.

1. additionfilled with additional quartz rings (for heat transfer)
2. additionfeeds were added
3. temperatureThe catalyst bed was heated to a temperature between 300°-500° with an air flow of 0.15 ft3 /hr
4. additionwas introduced
5. customto provide an addition rate of 0.15 ml/min
6. additionhad been introduced
7. customthe products (phenol, water, the propylphenol and propenylphenol) were collected from the receiver