公开(公告)号：DE50113838D1

公开(公告)日：2008-05-21

申请号：DE50113838

申请日：2001-09-20

Applicant: BASF SE

Inventor： OHLBACH FRANK ,  LUYKEN HERMANN ,  ANSMANN ANDREAS ,  FISCHER ROLF-HARTMUTH ,  MELDER JOHANN-PETER ,  BASSLER PETER

IPC: B01J38/52 ,  B01J23/86 ,  B01J23/94 ,  C07B61/00 ,  C07C209/48 ,  C07C211/12

Abstract: A process is provided for the regeneration of a heterogeneous catalyst used for the preparation of compounds containing NH 2 groups by the hydrogenation, with hydrogen, of compounds containing at least one unsaturated carbon-nitrogen bond, wherein a) the feed of the compound to be hydrogenated is stopped and b) the heterogeneous catalyst is treated with a compound of the formula R 1 R 2 N-CO-R 3 (I), in which R 1 is hydrogen or C 1 -C 4 alkyl and R 2 , R 3 independently of one another are each hydrogen or C 1 -C 4 alkyl or together are a C 3 -C 6 alkylene group, or mixtures of such compounds, at a pressure ranging from 0.1 to 30 MPa and a temperature ranging from 100 to 300° C., with the proviso that the compound of formula (I) is in liquid form during the treatment.

公开(公告)号：DE50114970D1

公开(公告)日：2009-08-20

申请号：DE50114970

申请日：2001-04-30

Applicant: BASF SE

Inventor： OHLBACH FRANK ,  ANSMANN ANDREAS ,  BASSLER PETER ,  FISCHER ROLF-HARTMUTH ,  LUYKEN HERMANN ,  MAIXNER STEFAN ,  MELDER JOHANN-PETER

IPC: C07D201/08 ,  C07D223/10 ,  C07B61/00 ,  C07D207/263 ,  C07D211/76 ,  C07D225/02

Abstract: The invention relates to a method for producing cyclic lactams of the formula (II), wherein n and m may each represent 0, 1, 2, 3, 4, 5, 6, 7, 8 and 9 and the sum of n + m is at least 3, preferably at least 4, R and R represent C1-C6 alkyl, C5-C7 cycloalkyl or C6-C12 aryl groups, by reacting a compound of the formula (I), wherein R , R , m and n have the meaning indicated above, and R represents nitrile groups, carboxylic acid amide groups and carboxylic acid groups, with water vapor in the gaseous phase. The inventive method is further characterized in that a) the compound (I) is reacted with water vapor in the gaseous phase, adding an organic diluent (III) before or after the reaction, which diluent has a miscibility gap under certain quantitative, pressure and temperature conditions, said reaction resulting in a mixture (IV) that contains a lactam (II), b) adjusting the mixture (IV) before or after the removal of ammonia to quantitative, pressure and temperature conditions under which the diluent (III) and water are present in a liquid form and have a miscibility gap, and obtaining a two-phase system consisting of a phase (V) that has a higher proportion of diluent (III) than water, and a phase (VI) that has a higher proportion of water than diluent (III), c) separating phase (V) from phase (VI) and, d) removing from phase (V) the diluent (III) and optionally by-products selected from the group of the low-boilers, high-boilers and unreacted compound (I), and obtaining a lactam (II).

公开(公告)号：AT435851T

公开(公告)日：2009-07-15

申请号：AT01927931

申请日：2001-04-30

Applicant: BASF SE

Inventor： OHLBACH FRANK ,  ANSMANN ANDREAS ,  BASSLER PETER ,  FISCHER ROLF-HARTMUTH ,  LUYKEN HERMANN ,  MAIXNER STEFAN ,  MELDER JOHANN-PETER

IPC: C07D201/08 ,  C07D223/10 ,  C07B61/00 ,  C07D207/263 ,  C07D211/76 ,  C07D225/02

Abstract: The invention relates to a method for producing cyclic lactams of the formula (II), wherein n and m may each represent 0, 1, 2, 3, 4, 5, 6, 7, 8 and 9 and the sum of n + m is at least 3, preferably at least 4, R and R represent C1-C6 alkyl, C5-C7 cycloalkyl or C6-C12 aryl groups, by reacting a compound of the formula (I), wherein R , R , m and n have the meaning indicated above, and R represents nitrile groups, carboxylic acid amide groups and carboxylic acid groups, with water vapor in the gaseous phase. The inventive method is further characterized in that a) the compound (I) is reacted with water vapor in the gaseous phase, adding an organic diluent (III) before or after the reaction, which diluent has a miscibility gap under certain quantitative, pressure and temperature conditions, said reaction resulting in a mixture (IV) that contains a lactam (II), b) adjusting the mixture (IV) before or after the removal of ammonia to quantitative, pressure and temperature conditions under which the diluent (III) and water are present in a liquid form and have a miscibility gap, and obtaining a two-phase system consisting of a phase (V) that has a higher proportion of diluent (III) than water, and a phase (VI) that has a higher proportion of water than diluent (III), c) separating phase (V) from phase (VI) and, d) removing from phase (V) the diluent (III) and optionally by-products selected from the group of the low-boilers, high-boilers and unreacted compound (I), and obtaining a lactam (II).

公开(公告)号：AT391554T

公开(公告)日：2008-04-15

申请号：AT01978378

申请日：2001-09-20

Applicant: BASF SE

Inventor： OHLBACH FRANK ,  LUYKEN HERMANN ,  ANSMANN ANDREAS ,  FISCHER ROLF-HARTMUTH ,  MELDER JOHANN-PETER ,  BASSLER PETER

IPC: B01J38/52 ,  B01J23/86 ,  B01J23/94 ,  C07B61/00 ,  C07C209/48 ,  C07C211/12

Abstract: A process is provided for the regeneration of a heterogeneous catalyst used for the preparation of compounds containing NH 2 groups by the hydrogenation, with hydrogen, of compounds containing at least one unsaturated carbon-nitrogen bond, wherein a) the feed of the compound to be hydrogenated is stopped and b) the heterogeneous catalyst is treated with a compound of the formula R 1 R 2 N-CO-R 3 (I), in which R 1 is hydrogen or C 1 -C 4 alkyl and R 2 , R 3 independently of one another are each hydrogen or C 1 -C 4 alkyl or together are a C 3 -C 6 alkylene group, or mixtures of such compounds, at a pressure ranging from 0.1 to 30 MPa and a temperature ranging from 100 to 300° C., with the proviso that the compound of formula (I) is in liquid form during the treatment.

公开(公告)号：DE50115253D1

公开(公告)日：2010-01-21

申请号：DE50115253

申请日：2001-04-30

Applicant: BASF SE

Inventor： BASSLER PETER ,  BAUMANN DIETER ,  FISCHER ROLF-HARTMUTH ,  FUCHS EBERHARD ,  MELDER JOHANN-PETER ,  OHLBACH FRANK

IPC: C07D201/08 ,  C07D223/10 ,  C07B61/00 ,  C07D201/16

Abstract: A process for the preparation of caprolactam is provided, whereina) a mixture (I) containing 6-aminocapronitrile and water is reacted in the liquid phase, in the presence of a catalyst, to give a mixture (II) containing caprolactam, ammonia, water, high-boiling components and low-boiling components,b) ammonia is then removed from the mixture (II) to give a mixture (III) containing caprolactam, water, high-boiling components and low-boiling components,c) water is then removed from the mixture (III) to give a mixture (IV) containing caprolactam, high-boiling components and low-boiling components, andd) a solid (V) containing caprolactam is then obtained from the mixture (IV) by crystallization, the proportion by weight of caprolactam in the solid (V) being greater than in the mixture (IV).

公开(公告)号：AT451353T

公开(公告)日：2009-12-15

申请号：AT01951465

申请日：2001-04-30

Applicant: BASF SE

Inventor： BASSLER PETER ,  BAUMANN DIETER ,  FISCHER ROLF-HARTMUTH ,  FUCHS EBERHARD ,  MELDER JOHANN-PETER ,  OHLBACH FRANK

IPC: C07D201/08 ,  C07D223/10 ,  C07B61/00 ,  C07D201/16

Abstract: A process for the preparation of caprolactam is provided, whereina) a mixture (I) containing 6-aminocapronitrile and water is reacted in the liquid phase, in the presence of a catalyst, to give a mixture (II) containing caprolactam, ammonia, water, high-boiling components and low-boiling components,b) ammonia is then removed from the mixture (II) to give a mixture (III) containing caprolactam, water, high-boiling components and low-boiling components,c) water is then removed from the mixture (III) to give a mixture (IV) containing caprolactam, high-boiling components and low-boiling components, andd) a solid (V) containing caprolactam is then obtained from the mixture (IV) by crystallization, the proportion by weight of caprolactam in the solid (V) being greater than in the mixture (IV).