公开(公告)号：CA1203072A

公开(公告)日：1986-04-15

申请号：CA406859

申请日：1982-07-08

Applicant: BASF AG

Inventor： RAPP GUENTHER DR ,  GROSSKINSKY OTTO-ALFRED ,  FROMMER ELMAR ,  RAPP GUENTHER

IPC: C07C239/08 ,  B01J23/42 ,  C01B21/14 ,  C07C67/00 ,  C07C239/00

Abstract: Hydroxylammonium salts are prepared by an improved process, wherein nitric oxide is reduced catalytically with hydrogen in a dilute aqueous solution of a mineral acid in the presence of a suspended supported platinum catalyst and at elevated temperatures, and wherein the improvement comprises avoiding the formation of foam at the surface of the reaction mixture.

公开(公告)号：CA636629A

公开(公告)日：1962-02-13

申请号：CA636629D

Applicant: BASF AG

Inventor： RAPP GUENTHER

公开(公告)号：CA886799A

公开(公告)日：1971-11-23

申请号：CA886799D

Applicant: BASF AG

Inventor： RAPP GUENTHER ,  KAHR KURT

公开(公告)号：GB996322A

公开(公告)日：1965-06-23

申请号：GB1568962

申请日：1962-04-25

Applicant: BASF AG

Inventor： NIESWANDT WERNER ,  STREHLER HUGO ,  RAPP GUENTHER ,  KAHR KURT

IPC: C01C1/242 ,  C07D201/16

Abstract: A process for continuously recovering pure ammonium sulphate in the preparation of lactams (see Division C2) by Beckmann rearrangement of a cycloalkanone oxime having 6 to 10 ring carbon atoms with 98 to 100% wt. sulphuric acid or oleum containing up to 35% wt. of free sulphur trioxide, which reaction mixture contains 30 to 50% wt. lactam, followed by neutralizing said reaction mixture by contact with ammonia in the presence of 5 to 50 times the amount (with reference to the weight of reaction mixture) of 25 to 45% wt. ammonium sulphate solution, comprises separating the resulting lactam and ammonium sulphate phases, evaporating the ammonium sulphate phase until ammonium sulphate has been precipitated in an amount corresponding to the sulphuric acid in the rearrangement mixture, diluting the mother liquor with such an amount of water as is necessary to restore the ammonium sulphate solution to its original concentration, and returning the diluted mother liquor to the neutralization zone. Concentration of the ammonium sulphate fraction may be effected by evaporation under reduced pressure. Preferably 5 to 50 times the weight of mother liquor (with reference to the weight of rearrangement mixture) is returned to the neutralization zone.ALSO:A process for the recovery of pure lactams and pure ammonium sulphate from reaction mixtures obtained by Beckmann re-arrangement of a cycloalkanone oxime having 6 to 10 ring carbon atoms with 98 to 100% wt. sulphuric acid or oleum containing up to 35% wt. of free sulphur trioxide, which reaction mixture contains 30 to 50% wt. of lactam, comprises neutralizing said reaction mixtures by contact with ammonia in the presence of 5 to 50 times the amount (with reference to the weight of the reaction mixture) of 25 to 45% wt. ammonium sulphate solution, separating the resulting lactam and ammonium sulphate phases, evaporating the ammonium sulphate phase until ammonium sulphate has been precipitated in an amount corresponding to the sulphuric acid in the re-arrangement mixture, diluting the mother liquor with such an amount of water as is necessary to restore the ammonium sulphate solution to its original concentration, returning the diluted mother liquor to the neutralization zone, extracting the lactam phase with at least three times its weight of benzene, toluene or xylene, and distilling to obtain the lactam. Preferably 5 to 50 times the amount of mother liquor (with reference to the weight of re-arrangement mixture) is returned to the neutralization zone. Concentration of the ammonium sulphate solution may be effected by evaporation under reduced pressure. The lactam may be extracted by a countercurrent extraction in a one-stage or multi-stage process. In specific examples caprolactam and caprylolactam are produced from cyclohexanone oxine and cyclooctanone oxine respectively.

公开(公告)号：GB911806A

公开(公告)日：1962-11-28

申请号：GB1503761

申请日：1961-04-26

Applicant: BASF AG

Inventor： RAPP GUENTHER

Abstract: Caprylic lactam is obtained by rearrangement of cyclooctanone oxime, containing less than 1% by weight of water, with sulphuric acid containing from 80% to 81.7% by weight of sulphur trioxide at 108 DEG to 120 DEG C. Preferablly the cyclooctanone oxime contains 0.3% by weight of water and the temperature is from 111 DEG to 113 DEG C. In examples cyclooctanone oxime is reacted with sulphuric acid of various concentrations, the reaction mixture is neutralized with ammonia, and the caprylic lactam separated by extraction with benzene.