Continuous preparation of .epsilon.-caprolactam by Beckmann rear

Chemistry of carbon compounds – Miscellaneous organic carbon compounds – C-metal

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C07D20104

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042579503

ABSTRACT:
A process for the continuous preparation of .epsilon.-caprolactam by Beckmann rearrangement of cyclohexanone-oxime, dissolved in a solvent which is inert toward oleum and is immiscible with oleum and water, at an elevated temperature, with removal of the heat of rearrangement by evaporation of the solvent, wherein oleum containing caprolactam is circulated successively through a conveying zone, a mixing zone, a boiling zone and a separating zone, upstream of the conveying zone oleum is added at the rate at which it is consumed, in the mixing zone cyclohexanone-oxime dissolved in solvent is added under turbulent conditions, in the boiling zone the heat of rearrangement is removed in a conventional manner by evaporating the solvent and recycling the condensate, and in the separating zone the reaction mixture is separated into a solvent phase, from which solvent is withdrawn at the rate at which the phase is formed, and a caprolactam-containing oleum phase, which is removed at the rate at which it is formed.

REFERENCES:
patent: 2249177 (1941-07-01), Schlack
patent: 2573374 (1951-10-01), Wichterle

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