Methyl Ethyl Ketone → Adipic Acid

Participants

Reaction Steps

A 4-neck flask was fitted with a variable speed stirrer, thermocouples in combination with a controller, a condenser, a nitrogen in- and outlet, an addition funnel, and a heating mantle. In the flask were placed 77.03 g isophorone diisocyanate and 70 g dry 2-butanone. A mixture of 36.8 g Tegomer D3403 (available from Tego Chemie Service), 80.22 g dry 2-butanone, 23.82 g of Rucoflex S-107-210 (a polyesterdiol resulting from the reaction of adipic acid and neopentyl glycol, available from Ruco Polymers), 59.9 g of acetal-functional intermediate E, described above, 0.22 g tin(II)octanoate, and 21.14 g of acetal functional intermediate D, described above, was added during 1 hour. The mixture was further heated to 85° C. and kept at this temperature for 19 hours. After this time, the isocyanate content of the mixture was below 0.1%. The mixture was cooled to 45° C. and transferred to a 2 I round-bottom flask with baffles and the above-mentioned equipment. The stirring speed was set to 350 RPM and 435 g water were added at a rate of 2.7 ml/min. When the addition of water was complete, the emulsion was transferred to a 2 I flask fifted with the above-mentioned equipment and a distillation head. The temperature was maintained at 45° C. A vacuum pump was connected to the flask and the pressure was gradually lowered until substantially all 2-butanone was distilled off.

Provenance & Evidence