公开(公告)号：DE59409678D1

公开(公告)日：2001-04-19

申请号：DE59409678

申请日：1994-06-28

Applicant: BASF AG

Inventor： FUCHS DR ,  RITZ DR ,  WILFINGER DR ,  WEATHERFORD DR

IPC: C07D201/12 ,  C07D201/16

Abstract: Recovery of caprolactam and of an alkali metal carbonate from distillation residues which are obtained in the purification of caprolactam and contain caprolactam and/or oligomers and/or polymers of caprolactam, and alkali metal hydroxides, by (a) melting the distillation residues, which contain caprolactam and/or oligomers and/or polymers of caprolactam, and alkali metal hydroxides, (b) continuously removing caprolactam from the melt, (c) cooling the melt after removing caprolactam with obtainment of a residue, (d) dissolving the residue thus obtained in water and (e) subjecting the aqueous solution thus obtained to incineration with the formation of an alkali metal carbonate.

公开(公告)号：DE59808566D1

公开(公告)日：2003-07-10

申请号：DE59808566

申请日：1998-03-27

Applicant: BASF AG

Inventor： FUCHS DR ,  BREITSCHEIDEL DR ,  BECKER DR ,  NEUHAUSER DR

IPC: B01J23/44 ,  C07B61/00 ,  C07C209/48 ,  C07C211/09 ,  C07C211/12 ,  C07C213/02 ,  C07C215/08

Abstract: Preparation of mono- or polyfunctional tertiary amines of formula X(CH2NR1R2)n (I) involves reacting a nitrile of formula (R1R2NCH2)n-mX(CN)m (II) with a secondary amine of formula NHR1R2 (III) and hydrogen. The reaction is at 50-250 degrees C and 5-350 bars, in presence of a palladium-based catalyst (IV), comprising (based on total catalyst) 0.1-10 wt.% palladium and 0.01-10 wt.% of at least one other metal, selected from Group IB and VIII elements, cerium and lanthanum, on a carrier. In (I)-(III), R1, R2 = 1-20C alkyl, 3-8C cycloalkyl, 4-20C alkylcycloalkyl, 4-20C cycloalkylalkyl, aryl, 7-20C alkaryl, 7-20C aralkyl, 2-8C hydroxyalkyl, 2-8C mercaptoalkyl or 8-20C aryloxyalkyl; or R1 + R2 = optionally unsaturated 2-6C alkylene chain (optionally substituted by 1-3 1-4C alkyl and optionally interrupted by O); X = n-valent 1-20C alkyl, 2-20C alkenyl or 3-8C cycloalkyl group (optionally substituted by 1-20C alkyl, 3-8C cycloalkyl, 4-20C alkylcycloalkyl, 4-20C cycloalkylalkyl, 2-20C alkoxyalkyl, aryl, 7-20C alkaryl, 7-20C aralkyl, 1-20C alkoxy, OH, 1-20C hydroxyalkyl, 1-20C alkylamino, 2-20C dialkylamino, 2-12C alkenylamino, 3-8C cycloalkylamino, arylamino, diarylamino, aryl-(1-8C)alkylamino, halo, SH, 2-20C alkenyloxy, 3-8C cycloalkoxy, aryloxy or 2-8C alkoxycarbonyl); n = 1-4; and m = 1 to n. Also claimed is the use of (IV) as catalyst for the reaction of secondary amines with nitriles and hydrogen to give tertiary amines in general.