Phenol → Phenol

Participants

Reaction Steps

The same procedure was selected as in Example 1. However, the reactor used was a 20-tray bubble-cap tray column 2 m in length and 5 cm in diameter. 500 g/h of phenol and 0.5 mol % of poly[oxy(butylhydroxystannylene)] were added at the head of the column, 500 g/h of gaseous dimethyl carbonate were added at the foot of the column. After one pass through the column, 554 g/h of a bottom product of composition 23.2% by weight of methyl phenyl carbonate, 2.1% by weight of diphenyl carbonate and 74.7% by weight of phenol were obtained, which still contained the catalyst. After a second pass of this product in the manner described in Example 1, 615 g/h of a bottom product of composition 36.8% by weight of methyl phenyl carbonate, 9.1% by weight of diphenyl carbonate and 54.1% by weight of phenol were obtained. After a third column pass, 670 g/h of a bottom product of composition 45.5% by weight of methyl phenyl carbonate, 14.3% by weight of diphenyl carbonate and 40.2% by weight of phenol were obtained. This corresponds to a space-time yield for the formation of methyl phenyl carbonate and diphenyl carbonate, based on three column passes, of 0.034 kg 1-1 h-1. After the fourth pass of the bottom product, in which no dimethyl carbonate was conducted in counter-current, the bottom product had the composition 13.5% by weight of methyl phenyl carbonate, 50.7% by weight of diphenyl carbonate and 35.8% by weight of phenol, which gives a space-time yield for the formation of methyl phenyl carbonate and diphenyl carbonate, based on 4 column passes, of 0.032 g 1-1 h-1. Here also, the catalyst was not removed at any stage, but recycled in all passes with the bottom product. The bottom compositions were determined by gas chromatographic analysis (GC) as % by weight compositions.

Provenance & Evidence