公开(公告)号：DE19839338A1

公开(公告)日：2000-03-02

申请号：DE19839338

申请日：1998-08-28

Applicant: BASF AG

Inventor： LUYKEN HERMANN ,  OHLBACH FRANK ,  ANSMANN ANDREAS ,  BASLER PETER ,  FISCHER ROLF ,  MELDER JOHANN-PETER ,  MERGER MARTIN ,  REHFINGER ALWIN ,  VOIT GUIDO ,  ACHHAMMER GUENTHER

IPC: C07B61/00 ,  C07C209/48 ,  C07C209/84 ,  C07C211/12 ,  C07C253/30 ,  C07C253/34 ,  C07C255/24

Abstract: The invention relates to a method for simultaneous preparation of 6-aminocapronitrile and hexamethylene diamine from adipodinitrile, comprising the following steps: a) hydrogenating adipodinitrile in the presence of a catalyst containing an element of the eight subgroup as catalytically active component to obtain a mixture containing 6-aminocapronitrile, hexamethylene diamine, adipodinitrile and high boilers; b) separating by distillation hexamethylene diamine from the mixture containing 6-aminocapronitrile, hexamethylene diamine, adipodinitrile and high boilers and c1) separating by distillation 6-aminocapronitrile and subsequently d1) separating by distillation adipodinitrile or c2) simultaneously separating by distillation 6-aminocapronitrile and adipodinitrile into separate fractions. The method is characterized in that the temperature of the bottom in steps d1) or c2) is below 185 DEG C.

公开(公告)号：BG101672A

公开(公告)日：1998-02-27

申请号：BG10167297

申请日：1997-06-25

Applicant: BASF AG

Inventor： RITZ JOSEF ,  FISCHER ROLF ,  SCHNURR WERNER ,  ACHHAMMER GUENTHER ,  LUYKEN HERMANN ,  FUCHS EBERHARD

IPC: C07D201/08 ,  C07B63/02 ,  C07D201/16

Abstract: The invention relates to a method where the raw caprolactamis purified by hydrogenation after which it is treated in acidicmedium and is distilled in alkaline medium, when: (a)6-aminiocapronitrile is converted in raw caprolactam by reactionwith water, (b) the high-boiling and low-boiling components areseparated from the raw caprolactam from stage (a), (c) the rawcaprilactam of stage (b) is treated with hydrogen at temperaturesranging from 50 to 150°C and from 1.5 to 250 bar in the presenceof hydrogenation catalyst and optionally of solvent, thusproducing mixtire A, (d1) mixture A in a solvent is passed at 30to 80°C and from 1 to 5 bar through ion-exchange resin having andacidic groups, thus producing mixture B1, or (d2) mixture A isdistilled in the presence of sulphuric acid and any amount ofsolvent is eliminated before the addition of the sulphuric acid,thus producing mixture B2, and mixture B1 or B2 is distilled inthe presence of a base, thus producing pure caprolactam.

公开(公告)号：PL320367A1

公开(公告)日：1997-09-29

申请号：PL32036795

申请日：1995-11-14

Applicant: BASF AG

Inventor： ACHHAMMER GUENTHER ,  FUCHS EBERHARD

IPC: C07D201/08 ,  C07D223/10

Abstract: Caprolactam is prepared by reacting a solution of 6-aminocapronitrile with water in the liquid phase at elevated temperatures by a process in which (a) an aqueous solution of 6-aminocapronitrile in the liquid phase is heated without the addition of a catalyst in a reactor A to give a mixture I consisting essentially of water, caprolactam and a high-boiling fraction (high boiler), then (b) the water is removed from the resulting mixture I to give a mixture II consisting essentially of caprolactam and the high boilers, then (c) the caprolactam and the high boilers from mixture II are separated from one another by distillation, and then either (d1) the high boilers from stage (c) are fed into the reactor A of stage (a) or (d2) the high boilers are heated similarly to stage (a) in a further reactor B and then worked up similarly to stages (b) and (c) to give further caprolactam, or (d3) the high boilers are heated under reduced pressure in the presence of a base in a reactor C and the reacted mixture is worked up by distillation to give caprolactam.

公开(公告)号：NO972503A

公开(公告)日：1997-08-01

申请号：NO972503

申请日：1997-06-02

Applicant: BASF AG

Inventor： FUCHS EBERHARD ,  ACHHAMMER GUENTHER

IPC: C07D201/08 ,  C07D223/10

CPC classification number: C07D201/08 ,  Y02P20/52 ,  Y10S203/17 ,  Y10S203/90

公开(公告)号：FI972340A

公开(公告)日：1997-06-02

申请号：FI972340

申请日：1997-06-02

Applicant: BASF AG

Inventor： FUCHS EBERHARD ,  ACHHAMMER GUENTHER

IPC: C07D201/08 ,  C07D223/10 ,  C07D

Abstract: An improved process for the preparation of caprolactam by heating 6-aminocapronitrile in the presence of a heterogenous catalyst and water under superatmospheric pressure without rapid deactivation of the catalysts used. The process further includes the addition of a low or high boiling alcohol in the heating phase, after which the products are obtained by distillation. The process further includes a method of working up the top and bottom products of the reactors to achieve higher yields.

公开(公告)号：CA2231536A1

公开(公告)日：1997-04-10

申请号：CA2231536

申请日：1996-09-26

Applicant: BASF AG

Inventor： HEINEKE DANIEL ,  SCHNEIDER HEINZ-WALTER ,  RIEKER CHRISTOPHER WILLIAM ,  OOSTVOGELS JOZEF ,  POSTELMANS DANY ,  THOME ALFRED ,  ACHHAMMER GUENTHER

IPC: B01J23/42 ,  B01J23/96 ,  B01J37/16 ,  B01J38/48 ,  C01B21/14

Abstract: The invention relates to a hydrogenation catalyst by the reduction from platinum in the stage of oxidation of +4 (Pt (IV)) with a selective reducing agent in an acidic aqueous medium in the presence of a carbon-containing carrier to platinum in the stage of oxidation +2 (Pt (II)), subsequent poisoning of the platinum thus obtained with a sulphur-containing selective reducing agent, and subsequent reduction of the platinum thus partially poisoned to form metallic platinum (Pt(0)) and subsequent processing as known per se in that (a) Pt (II) is partially poisoned with a sulphur-containing selective reducing agent, wherein the sulphur-containing selective reduction agent is used in an amount which corresponds to from 15 to 70 mol % of the amount of the sulphur-containing selective reducing agent which might be needed to reduce Pt(IV) to Pt (II), provided that the amount of Pt (IV) corresponds to the amount of Pt (II) used and to be poisoned, and subsequently the partially poisoned Pt (II) is reduced with an alkali metal formate to Pt (0); or (b) platinum in the stage of oxidation of greater than +2 is partially poisoned and subsequently or simultaneously reduced with an alkali metal formate to Pt (0). The invention also relates to a hydrogenation catalyst, use of the hydrogenation catalyst for preparing hydroxylammonium salts, a process for the preparation of hydroxylammonium salts, and a process for regenerating platinum-containing hydrogenation catalysts.

公开(公告)号：AT251112T

公开(公告)日：2003-10-15

申请号：AT99934555

申请日：1999-07-02

Applicant: BASF AG

Inventor： LUYKEN HERMANN ,  OHLBACH FRANK ,  ANSMANN ANDREAS ,  BASSLER PETER ,  FISCHER ROLF ,  MELDER JOHANN-PETER ,  MERGER MARTIN ,  REHFINGER ALWIN ,  VOIT GUIDO ,  ACHHAMMER GUENTHER

IPC: C07B61/00 ,  C07C209/48 ,  C07C209/84 ,  C07C209/86 ,  C07C211/12 ,  C07C253/30 ,  C07C253/34 ,  C07C255/24

Abstract: The invention relates to a method for simultaneous production of 6-aminocapronitrile and hexamethylenediamine from adipodinitrile, comprising the following steps: a) hydrogenating adipodinitrile in the presence of a catalyst containing an element of the VIII subgroup thereby obtaining a mixture containing 6-aminocapronitrile, hexamethylenediamine, adipodinitrile and high boilers; b) distillative separation of hexamethylenediamine from the mixture containing 6-aminocapronitrile, hexamethylenediamine, adipodinitrile and high boilers or c1) distillative separating 6-aminocapronitrile and subsequently d1) distillative separation of adipodinitrile or c2) simultaneous distillative separation of 6-aminocapronitrile and adipodinitrile into separate fractions. The invention is characterized in that temperatures in the bottoms of the column in steps d1) or c2) are under 185 DEG C. The adipodinitrile thus obtained contains less impurities than for instance 1-amino-2-cyanocyclopentenes.

公开(公告)号：DE59510263D1

公开(公告)日：2002-08-08

申请号：DE59510263

申请日：1995-11-14

Applicant: BASF AG

Inventor： ACHHAMMER GUENTHER ,  FUCHS EBERHARD

IPC: C07D201/08 ,  C07D223/10

Abstract: Caprolactam is prepared by reacting a solution of 6-aminocapronitrile with water in the liquid phase at elevated temperatures by a process in which (a) an aqueous solution of 6-aminocapronitrile in the liquid phase is heated without the addition of a catalyst in a reactor A to give a mixture I consisting essentially of water, caprolactam and a high-boiling fraction (high boiler), then (b) the water is removed from the resulting mixture I to give a mixture II consisting essentially of caprolactam and the high boilers, then (c) the caprolactam and the high boilers from mixture II are separated from one another by distillation, and then either (d1) the high boilers from stage (c) are fed into the reactor A of stage (a) or (d2) the high boilers are heated similarly to stage (a) in a further reactor B and then worked up similarly to stages (b) and (c) to give further caprolactam, or (d3) the high boilers are heated under reduced pressure in the presence of a base in a reactor C and the reacted mixture is worked up by distillation to give caprolactam.

公开(公告)号：DE59509451D1

公开(公告)日：2001-08-30

申请号：DE59509451

申请日：1995-12-22

Applicant: BASF AG

Inventor： RITZ JOSEF ,  FISCHER ROLF ,  SCHNURR WERNER ,  ACHHAMMER GUENTHER ,  LUYKEN HERMANN ,  FUCHS EBERHARD

IPC: C07D201/08 ,  C07B63/02 ,  C07D201/16

Abstract: Crude capronitrile is purified by hydrogenation, subsequent treatment in an acidic medium and subsequent distillation in an alkaline medium, by a process in which (a) 6-aminocapronitrile is converted into crude caprolactam by reaction with water, (b) high boilers and low boilers are separated off from the crude caprolactam from step (a), (c) the crude caprolactam from step (b) is treated with hydrogen at from 50 DEG to 150 DEG C. and from 1.5 to 250 bar in the presence of a hydrogenation catalyst and, if desired, of a solvent to give a mixture A, (d1) mixture A in a solvent is passed, at from 30 DEG to 80 DEG C. and from 1 to 5 bar, over an ion exchanger containing terminal acid groups to give a mixture B1, or (d2) mixture A is distilled in the presence of sulfuric acid, any solvent present being removed before the addition of the sulfuric acid, to give a mixture B2, and (e) mixture B1 or mixture B2 is distilled in the presence of a base to give pure caprolactam.

公开(公告)号：DE19832529A1

公开(公告)日：2000-01-27

申请号：DE19832529

申请日：1998-07-20

Applicant: BASF AG

Inventor： LUYKEN HERMANN ,  OHLBACH FRANK ,  ANSMANN ANDREAS ,  BASLER PETER ,  FISCHER ROLF ,  MELDER JOHANN-PETER ,  MERGER MARTIN ,  REHFINGER ALWIN ,  VOIT GUIDO ,  ACHHAMMER GUENTHER

IPC: C07B61/00 ,  C07C209/48 ,  C07C209/84 ,  C07C209/86 ,  C07C211/12 ,  C07C253/30 ,  C07C253/34 ,  C07C255/24 ,  C07C209/82

Abstract: A process for the simultaneous production of 6-amino-capronitrile (ACN) and hexamethylenediamine (HDA) by hydrogenation of adiponitrile (ADN) in which, after separation of HDA by distillation, the ACN and ADN are separated in succession or simultaneously (in separate fractions) with a bottom temperature below 185 deg C. A process for the simultaneous production of ACN and HDA from ADN comprises (a) hydrogenation of ADN in presence of a catalyst based on a Subgroup VIII element to give a mixture containing ACN, HDA, ADN and high-boiling products, (b) separation of HDA from the mixture by distillation, (c1) separation of ACN by distillation and then (d1) separation of ADN by distillation or (c2) simultaneous separation of ACN and ADN in separate fractions. Distillation stage (d1) or (c2) is carried out with a bottom temperature below 185 deg C.