公开(公告)号：DE2960317D1

公开(公告)日：1981-08-06

申请号：DE2960317

申请日：1979-10-12

Applicant: BASF AG

Inventor： HORN PETER DR DIPL CHEM ,  GROSSKINSKY OTTO-ALFRED DR DIP ,  THOMA RICHARD DR ,  FUCHS HUGO DR DIPL CHEM

IPC: C07D201/04 ,  C07D223/10

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condensate, and in the separating zone the reaction mixture is separated into a solvent phase, from which solvent is withdrawn at the rate at which the phase is formed, and a caprolactam-containing oleum phase, which is removed at the rate at which it is formed.

公开(公告)号：DE2962465D1

公开(公告)日：1982-05-19

申请号：DE2962465

申请日：1979-10-12

Applicant: BASF AG

Inventor： HORN PETER DR DIPL CHEM ,  FUCHS HUGO DR DIPL CHEM

IPC: C07D201/16 ,  C07D223/10

Abstract: A process for purifying crude caprolactam which has been obtained by rearrangement of cyclohexanone-oxime in the gas phase over a catalyst containing boron trioxide, wherein caprolactam is crystallized out, by cooling, from a melt which contains, per 100 parts by weight of crude caprolactam, from 5 to 30 parts by weight of primary alkanols or fatty acids which have a carbon chain of 6 to 10 carbon atoms and are substituted by alkyl radicals of 1 to 5 carbon atoms, and from 0 to 5 parts by weight of water, and is separated from the mother liquor.