公开(公告)号：DE59510717D1

公开(公告)日：2003-07-10

申请号：DE59510717

申请日：1995-12-22

Applicant: BASF AG

Inventor： ACHHAMMER GUENTHER ,  BASSLER PETER ,  FISCHER ROLF ,  FUCHS EBERHARD ,  LUYKEN HERMANN ,  SCHNURR WERNER ,  WITZEL TOM

IPC: C07D201/02 ,  C07C209/48 ,  C07C211/12 ,  C07D201/08 ,  C07D223/10

Abstract: The invention concerns the simultaneous preparation of caprolactam and hexamethylene diamine from adipodinitrile, by the following steps: (a) the adipodinitrile is partially hydrogenated, producing a mixture substantially containing 6-aminocapronitrile, hexamethylene diamine, ammonia, adipodinitrile and hexamethylene imine (= "the mixture"); (b) the mixture obtained in step (a) is distilled, producing ammonia, as the forerunnings, and a residue I, in the presence of a compound A which is inert in the distillation conditions, the ammonia not being separated totally; (c) the residue I, substantially containing "the mixture", inert compound A and ammonia, the ammonia content being less than that of the mixture used in step (b), is subjected to a second distillation, producing a mixture of the inert compound A and ammonia, as the forerunnings, and a residue II; (d) the base II, substantially containing "the mixture" and inert compound A, is subjected to distillation in a third column, producing the inert compound A, as the forerunnings, and a residue III; (e) the base III, substantially containing "the mixture" and optionally an inert compound B, is subjected to distillation in a fourth column, producing forerunnings KP1, which substantially contain hexamethylene imine, optionally inert compound B and hexamethylene diamine, and a residue IV; (f) the forerunnings KP1 are subjected in a fifth column to distillation, producing forerunnings KP2, which substantially contain hexamethylene imine and optionally inert compound B, and a residue V, which substantially contains hexamethylene diamine with a degree of purity of at least 95 %, the forerunnings KP2 being fed to the third column or optionally only partially fed to the third column, and the rest being discarded; and (g) the residue IV, substantially containing 6-aminocapronitrile and adipodinitrile, is subjected in a sixth column to distillation, producing 6-aminocapronitrile with a degree of purity of at least 95 %, as forerunnings, and adiponitrile in the residue. The resultant 6-aminocapronitrile is cyclized to form caprolactam.

公开(公告)号：AT242217T

公开(公告)日：2003-06-15

申请号：AT95942198

申请日：1995-12-22

Applicant: BASF AG

Inventor： ACHHAMMER GUENTHER ,  BASSLER PETER ,  FISCHER ROLF ,  FUCHS EBERHARD ,  LUYKEN HERMANN ,  SCHNURR WERNER ,  WITZEL TOM

IPC: C07D201/02 ,  C07C209/48 ,  C07C211/12 ,  C07D201/08 ,  C07D223/10

Abstract: The invention concerns the simultaneous preparation of caprolactam and hexamethylene diamine from adipodinitrile, by the following steps: (a) the adipodinitrile is partially hydrogenated, producing a mixture substantially containing 6-aminocapronitrile, hexamethylene diamine, ammonia, adipodinitrile and hexamethylene imine (= "the mixture"); (b) the mixture obtained in step (a) is distilled, producing ammonia, as the forerunnings, and a residue I, in the presence of a compound A which is inert in the distillation conditions, the ammonia not being separated totally; (c) the residue I, substantially containing "the mixture", inert compound A and ammonia, the ammonia content being less than that of the mixture used in step (b), is subjected to a second distillation, producing a mixture of the inert compound A and ammonia, as the forerunnings, and a residue II; (d) the base II, substantially containing "the mixture" and inert compound A, is subjected to distillation in a third column, producing the inert compound A, as the forerunnings, and a residue III; (e) the base III, substantially containing "the mixture" and optionally an inert compound B, is subjected to distillation in a fourth column, producing forerunnings KP1, which substantially contain hexamethylene imine, optionally inert compound B and hexamethylene diamine, and a residue IV; (f) the forerunnings KP1 are subjected in a fifth column to distillation, producing forerunnings KP2, which substantially contain hexamethylene imine and optionally inert compound B, and a residue V, which substantially contains hexamethylene diamine with a degree of purity of at least 95 %, the forerunnings KP2 being fed to the third column or optionally only partially fed to the third column, and the rest being discarded; and (g) the residue IV, substantially containing 6-aminocapronitrile and adipodinitrile, is subjected in a sixth column to distillation, producing 6-aminocapronitrile with a degree of purity of at least 95 %, as forerunnings, and adiponitrile in the residue. The resultant 6-aminocapronitrile is cyclized to form caprolactam.

公开(公告)号：ES2165087T3

公开(公告)日：2002-03-01

申请号：ES97941891

申请日：1997-07-23

Applicant: BASF AG

Inventor： FISCHER ROLF ,  PACIELLO ROCCO ,  ROPER MICHAEL ,  SCHNURR WERNER

IPC: B01J31/18 ,  B01J31/24 ,  C07C209/26 ,  C07C253/30 ,  C07C255/24 ,  C07F9/6574

Abstract: PCT No. PCT/EP97/03988 Sec. 371 Date Feb. 1, 1999 Sec. 102(e) Date Feb. 1, 1999 PCT Filed Jul. 23, 1997 PCT Pub. No. WO98/05632 PCT Pub. Date Feb. 12, 1998Manufacture of 6-aminocapronitrile or 6-aminocapronitrile/hexamethylene diamine mixtures, involving a) the reaction of at least one pentennitrile, selected from the group consisting of 2,3 and 4-pentennitrile with carbon monoxide and hydrogen in the presence of catalysts, which contain at least one element of the eighth subgroup as active components, obtaining a hydrogenation formylating discharge (I), b) the optional separation of carbon monoxide, hydrogen and the catalyst from the hydrogenation formylating discharge (I), obtaining a hydrogenation formylating discharge (II), c) the separation of 5-formyl valeronitrile from the hydrogenation formylating discharge (I) or (II), d) the reaction of separated 5-formyl valeronitrile with ammonia and hydrogen in the presence of hydrogenating catalysts, selected from the group consisting of rhenium, copper and its compounds as well as metals and metallic compounds of the eighth group, obtaining a hydrogenation discharge, and e) obtaining 6-aminocapronitrile and if necessary hexamethylene diamine.

公开(公告)号：ES2160943T3

公开(公告)日：2001-11-16

申请号：ES97918107

申请日：1997-04-04

Applicant: BASF AG

Inventor： SCHNURR WERNER ,  VOIT GUIDO ,  FLICK KLEMENS ,  MELDER JOHANN-PETER ,  FISCHER ROLF ,  HARDER WOLFGANG

IPC: C07B61/00 ,  C07C209/48 ,  C07C211/12 ,  C07C253/30 ,  B01J25/02 ,  C07C255/24

Abstract: A process for the coproduction of 6-aminocapronitrile (ACN) and hexamethylenediamine (HMD) by treatment of adiponitrile (ADN) with hydrogen in the presence of a nickel-containing catalyst at temperatures not below room temperature and elevated hydrogen partial pressure in the presence or absence of a solvent comprises, after the conversion based on ADN and/or the selectivity based on ACN has or have dropped below a defined value (a) interrupting the treatment of ADN with hydrogen by stopping the feed of ADN and of the solvent, if used, (b) treating the catalyst at from 150 DEG to 400 DEG C. with hydrogen using a hydrogen pressure within the range from 0.1 to 30 MPa and a treatment time within the range from 2 to 48 h, and (c) then continuing the hydrogenation of ADN with the treated catalyst of stage (b).

公开(公告)号：DE59704683D1

公开(公告)日：2001-10-25

申请号：DE59704683

申请日：1997-07-23

Applicant: BASF AG

Inventor： FISCHER ROLF ,  PACIELLO ROCCO ,  ROEPER MICHAEL ,  SCHNURR WERNER

IPC: B01J31/18 ,  B01J31/24 ,  C07C209/26 ,  C07C253/30 ,  C07C255/24 ,  C07F9/6574

Abstract: PCT No. PCT/EP97/03988 Sec. 371 Date Feb. 1, 1999 Sec. 102(e) Date Feb. 1, 1999 PCT Filed Jul. 23, 1997 PCT Pub. No. WO98/05632 PCT Pub. Date Feb. 12, 1998Manufacture of 6-aminocapronitrile or 6-aminocapronitrile/hexamethylene diamine mixtures, involving a) the reaction of at least one pentennitrile, selected from the group consisting of 2,3 and 4-pentennitrile with carbon monoxide and hydrogen in the presence of catalysts, which contain at least one element of the eighth subgroup as active components, obtaining a hydrogenation formylating discharge (I), b) the optional separation of carbon monoxide, hydrogen and the catalyst from the hydrogenation formylating discharge (I), obtaining a hydrogenation formylating discharge (II), c) the separation of 5-formyl valeronitrile from the hydrogenation formylating discharge (I) or (II), d) the reaction of separated 5-formyl valeronitrile with ammonia and hydrogen in the presence of hydrogenating catalysts, selected from the group consisting of rhenium, copper and its compounds as well as metals and metallic compounds of the eighth group, obtaining a hydrogenation discharge, and e) obtaining 6-aminocapronitrile and if necessary hexamethylene diamine.

公开(公告)号：BG63300B1

公开(公告)日：2001-09-28

申请号：BG10163297

申请日：1997-06-17

Applicant: BASF AG

Inventor： SCHNURR WERNER ,  FISCHER ROLF ,  BASSLER PETER ,  HARDER WOLFGANG

IPC: C07B61/00 ,  C07C253/30 ,  C07C255/24

Abstract: Aliphatic alpha, omega-aminonitriles are prepared by partially hydrogenating aliphatic alpha, omega-dinitriles at an increased temperature and pressure in the presence of a base and an hydrogenation catalyst. Hydrogenation is carried out in the presence of ammonia and lithium hydroxide or a compound that releases lithium hydroxide during the hydrogenation process. 4 claims

公开(公告)号：TR199900222T2

公开(公告)日：2000-09-21

申请号：TR9900222

申请日：1997-07-23

Applicant: BASF AG

Inventor： FISCHER ROLF ,  PACIELLO ROCCO ,  ROPER MICHAEL ,  SCHNURR WERNER

IPC: B01J31/18 ,  B01J31/24 ,  C07C209/26 ,  C07C253/30 ,  C07C255/24 ,  C07F9/6574

Abstract: PCT No. PCT/EP97/03988 Sec. 371 Date Feb. 1, 1999 Sec. 102(e) Date Feb. 1, 1999 PCT Filed Jul. 23, 1997 PCT Pub. No. WO98/05632 PCT Pub. Date Feb. 12, 1998Manufacture of 6-aminocapronitrile or 6-aminocapronitrile/hexamethylene diamine mixtures, involving a) the reaction of at least one pentennitrile, selected from the group consisting of 2,3 and 4-pentennitrile with carbon monoxide and hydrogen in the presence of catalysts, which contain at least one element of the eighth subgroup as active components, obtaining a hydrogenation formylating discharge (I), b) the optional separation of carbon monoxide, hydrogen and the catalyst from the hydrogenation formylating discharge (I), obtaining a hydrogenation formylating discharge (II), c) the separation of 5-formyl valeronitrile from the hydrogenation formylating discharge (I) or (II), d) the reaction of separated 5-formyl valeronitrile with ammonia and hydrogen in the presence of hydrogenating catalysts, selected from the group consisting of rhenium, copper and its compounds as well as metals and metallic compounds of the eighth group, obtaining a hydrogenation discharge, and e) obtaining 6-aminocapronitrile and if necessary hexamethylene diamine.

公开(公告)号：TR199802028T2

公开(公告)日：2000-09-21

申请号：TR9802028

申请日：1997-04-03

Applicant: BASF AG

Inventor： SCHNURR WERNER ,  VOIT GUIDO ,  FLICK KLEMENS ,  FISCHER ROLF-HARTMUTH

IPC: B01J23/78 ,  B01J23/94 ,  B01J27/187 ,  B01J27/28 ,  B01J38/10 ,  C07B61/00 ,  C07C209/48 ,  C07C211/12 ,  C07C253/30 ,  C07C255/24

Abstract: A process for the coproduction of 6-aminocapronitrile (ACN) and hexamethylenediamine (HMD) by treatment of adiponitrile (ADN) with hydrogen in the presence of a nickel-containing catalyst at temperatures not below room temperature and elevated hydrogen partial pressure in the presence or absence of a solvent comprises, after the conversion based on ADN and/or the selectivity based on ACN has or have dropped below a defined value (a) interrupting the treatment of ADN with hydrogen by stopping the feed of ADN and of the solvent, if used, (b) treating the catalyst at from 150 DEG to 400 DEG C. with hydrogen using a hydrogen pressure within the range from 0.1 to 30 MPa and a treatment time within the range from 2 to 48 h, and (c) then continuing the hydrogenation of ADN with the treated catalyst of stage (b).

公开(公告)号：ES2146118T3

公开(公告)日：2000-07-16

申请号：ES97943816

申请日：1997-08-21

Applicant: BASF AG

Inventor： FLICK KLEMENS ,  FISCHER ROLF ,  EBEL KLAUS ,  SCHNURR WERNER ,  VOIT GUIDO

IPC: B01J23/74 ,  B01J23/76 ,  B01J25/00 ,  C07B61/00 ,  C07C253/30 ,  B01J23/75 ,  C07C255/24 ,  C07C255/25

Abstract: PCT No. PCT/EP97/04547 Sec. 371 Date Jan. 7, 1999 Sec. 102(e) Date Jan. 7, 1999 PCT Filed Aug. 21, 1997 PCT Pub. No. WO98/11058 PCT Pub. Date Mar. 19, 1998A catalyst suitable for preparing aliphatic alpha, omega-aminonitriles by partial hydrogenation of aliphatic dinitriles comprises (a) metallic cobalt, a cobalt compound or a mixture thereof, the proportion of metallic cobalt based on (a) being from 20 to 100% by weight, (b) from 10 to 70% by weight, based on (a), of metallic iron, iron oxide, a further iron compound or a mixture thereof, the proportion of iron oxide based on (b) being from 20 to 100% by weight, (c) from 0 to 1% by weight, based on (a), of a compound based on an alkali metal, an alkaline earth metal or zinc.

公开(公告)号：NO307781B1

公开(公告)日：2000-05-29

申请号：NO972997

申请日：1997-06-26

Applicant: BASF AG

Inventor： MELDER JOHANN-PETER ,  SCHNURR WERNER ,  FLICK KLEMENS ,  EBEL KLAUS ,  WITZEL TOM ,  FISCHER ROLF ,  HARDER WOLFGANG ,  REHFINGER ALWIN

IPC: B01J23/76 ,  B01J23/889 ,  B01J27/18 ,  B01J23/89 ,  B01J37/02 ,  C07B61/00 ,  C07C253/30 ,  C07C255/24

Abstract: Aliphatic alpha,omega-aminonitriles are prepared by partial hydrogenation of aliphatic alpha,omega-dinitriles at elevated temperatures and superatmospheric pressure in the presence of a solvent and of a catalyst by a process which comprises using a catalyst which (a) contains a compound based on a metal selected from the group consisting of nickel, cobalt, iron, ruthenium and rhodium and (b) contains from 0.01 to 25% by weight, based on (a), of a promoter based on a metal selected from the group consisting of palladium, platinum, iridium, osmium, copper, silver, gold, chromium, molybdenum, tungsten, manganese, rhenium, zinc, cadmium, lead, aluminum, tin, phosphorus, arsenic, antimony, bismuth and rare earth metals and (c) from 0 to 5% by weight, based on (a), of a compound based on an alkali metal or on an alkaline earth metal. with the proviso that the component (a) is not based on iron or iron and one of the metals selected from the group consisting of cobalt, ruthenium and rhodium when (b) is a promoter based on a metal selected from the group consisting of titanium, manganese, chromium and molybdenum, and with the further proviso that, when a compound based on only ruthenium or rhodium or ruthenium and rhodium or nickel and rhodium is selected as component (a), the promoter (b) may be dispensed with.