公开(公告)号：BG63431B1

公开(公告)日：2002-01-31

申请号：BG10166197

申请日：1997-06-24

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 KP, which substantially contain hexamethylene imine, optionally inert compound B and hexamethylene diamine, and a residue IV; (f) the forerunnings KP 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. 7 claims, 1 figure

公开(公告)号：ES2160729T3

公开(公告)日：2001-11-16

申请号：ES95942729

申请日：1995-12-22

Applicant: BASF AG

Inventor： RITZ JOSEF ,  FISCHER ROLF ,  SCHNURR WERNER ,  ACHHAMMER GUNTHER ,  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：BG63299B1

公开(公告)日：2001-09-28

申请号：BG10163197

申请日：1997-06-17

Applicant: BASF AG

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

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

Abstract: The invention relates to the preparation of aliphatic -aminonitriles by partial hydrogenation of aliphatic dinitriles at elevated temperature and higher pressure, in the presence of a solvent and catalyst. Catalyst, containing the following is used: (a) compound based on metal, e.g. nickel, cobalt, iron, ruthenium and rhodium; (b) from 0.01 to 25 wt.% promotor to component (a) based on metal such as palladium, platinum, iridium, osmium, copper, silver, gold, chromium, molybdenum, tungsten, manganese, rhenium, zinc, cadmium, lead, aluminium, tin, phosphorus, arsenic, antimony, bismith, silicon, titanium, zirconium and the rare earth elements, and (c) from 0 to 5 wt.% compound to component (a) based on alkali or alkaliearth metal, provided that component (a) is different from an iron-based compound or from iron, as well as from the metals cobalt, ruthenium or rhodium when component (b) is promotor based on a metal from the group containing titanium, managanese, chromium and molybdenum. An additional condition is that when component (a) is a compound based on ruthenium or rhodium separately, or of ruthenium and rhodium, or of nickel and rhodium, promotor (b) can optionally be dropped. 8 claims

公开(公告)号：DE59704129D1

公开(公告)日：2001-09-13

申请号：DE59704129

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：PL181529B1

公开(公告)日：2001-08-31

申请号：PL32099395

申请日：1995-12-16

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 partial hydrogenation of aliphatic alpha,omega-dinitriles at elevated temperatures and superatmospheric pressure in the presence of a base and of a hydrogenation catalyst, by carrying out the hydrogenation in the presence of ammonia and lithium hydroxide or of a compound which gives lithium hydroxide during the hydrogenation.

公开(公告)号：NO310352B1

公开(公告)日：2001-06-25

申请号：NO990432

申请日：1999-01-29

Applicant: BASF AG

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

IPC: B01J23/78 ,  B01J23/94 ,  B01J27/187 ,  B01J27/28 ,  B01J38/10 ,  C07B43/04 ,  C07B61/00 ,  C07C20060101 ,  C07C209/48 ,  C07C209/52 ,  C07C211/12 ,  C07C211/35 ,  C07C253/30 ,  C07C255/24

Abstract: A process for preparing an NH2-containing compound by hydrogenating a compound containing at least one unsaturated carbon-nitrogen bond with hydrogen in the presence of a catalyst at temperatures not below room temperature and elevated hydrogen partial pressure in the presence or absence of a solvent which process includes the following steps: a) using a catalyst comprising a cobalt- and/or iron-containing catalyst, and b) after the conversion based on the compound to be hydrogenated and/or the selectivity based on the desired product has or have dropped below a defined value or the amount of an unwanted by-product has risen beyond a defined value, interrupting the hydrogenation by stopping the feed of the compound to be hydrogenated and of the solvent, if used, c) 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 d) subsequently continuing the hydrogenation of the compound containing at least one unsaturated carbon-nitrogen bond.

公开(公告)号：ES2156400T3

公开(公告)日：2001-06-16

申请号：ES97941902

申请日：1997-07-29

Applicant: BASF AG

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

IPC: B01J23/78 ,  B01J23/94 ,  B01J27/187 ,  B01J27/28 ,  B01J38/10 ,  C07B43/04 ,  C07B61/00 ,  C07C20060101 ,  C07C209/48 ,  C07C209/52 ,  C07C211/12 ,  C07C211/35 ,  C07C253/30 ,  C07C255/24

Abstract: A process for preparing an NH2-containing compound by hydrogenating a compound containing at least one unsaturated carbon-nitrogen bond with hydrogen in the presence of a catalyst at temperatures not below room temperature and elevated hydrogen partial pressure in the presence or absence of a solvent which process includes the following steps: a) using a catalyst comprising a cobalt- and/or iron-containing catalyst, and b) after the conversion based on the compound to be hydrogenated and/or the selectivity based on the desired product has or have dropped below a defined value or the amount of an unwanted by-product has risen beyond a defined value, interrupting the hydrogenation by stopping the feed of the compound to be hydrogenated and of the solvent, if used, c) 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 d) subsequently continuing the hydrogenation of the compound containing at least one unsaturated carbon-nitrogen bond.

公开(公告)号：ES2151259T3

公开(公告)日：2000-12-16

申请号：ES97918103

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：DK0800508T3

公开(公告)日：2000-07-17

申请号：DK95941718

申请日：1995-12-16

Applicant: BASF AG

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

IPC: B01J23/76 ,  B01J23/889 ,  B01J23/89 ,  B01J27/18 ,  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.

公开(公告)号：CZ9900768A3

公开(公告)日：2000-01-12

申请号：CZ76899

申请日：1997-08-21

Applicant: BASF AG

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

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

CPC classification number: C07C253/30