Nitric Acid → 1-Nitroanthraquinone

Participants

Reaction Steps

A mixture of 2.08 kg of anthraquinone and 9.545 kg of 99% nitric acid per hour (mole ratio 15:1) is cooled to 0° and continuously reacted in a flow tube reactor with a residence time of 13 minutes and a final temperature of 55°. The solution leaving the reactor is continuously cooled to -10° to stop the reaction and introduced into a crystallising apparatus together with 19.33 kg per hour of 66.2% nitric acid (crystallisation acid 76%, γHNO3 = 0.469). The precipitated product is continuously suction-filtered, washed with a little 76% nitric acid, freed from nitric acid adhering to it and subjected to continuous vacuum rectification (10 Torr, head temperature 281°). 1.740 kg of 98.9% pure 1-nitroanthraquinone are obtained per hour (68% of the theoretical amount).

Provenance & Evidence