Neutralization of reaction mixtures obtained by Beckman rearrangement of cyclohexanone oxime

摘要

Reaction mixtures obtained by Beckmann rearrangement of cyclohexanone oxime with sulfuric acid or oleum are neutralized by a process which comprises the following steps: (a) mixing the reaction mixture with recycled ammonium sulfate mother liquor whose concentration is chosen so that no solid ammonium sulfate is precipitated during the neutralization, (b) neutralization by feeding gaseous ammonia which contains water or an aqueous ammonium sulfate solution in finely divided liquid form through a plurality of nozzle orifices into the solution of the reaction mixture in the ammonium sulfate mother liquor at elevated temperatures, (c) separation of crude lactam from the aqueous ammonium sulfate solution, (d) evaporation of the ammonium sulfate solution under reduced pressure and with separation of the crystalline ammonium sulfate from the ammonium sulfate mother liquor and (e) recycling of the ammonium sulfate mother liquor to stage a).