公开(公告)号：BR0316178A

公开(公告)日：2005-09-27

申请号：BR0316178

申请日：2003-11-11

Applicant: BASF AG

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

IPC: C07D201/08 ,  C07D201/16

Abstract: A process for removing high boilers from crude caprolactam which comprises high boilers, caprolactam and in some cases low boilers, and which has been obtained by a) reacting 6-aminocapronitrile with water to give a reaction mixture b) removing ammonia and unconverted water from the reaction mixture to obtain crude caprolactam, which comprises c) feeding the crude caprolactam to a distillation apparatus to obtain a first substream via the top as a product and a second substream via the bottom, by setting the pressure in the distillation in such a way that the bottom temperature does not go below 170° C., and adjusting the second substream in such a way that the caprolactam content of the second substream is not less than 10% by weight, based on the entire second substream.

公开(公告)号：DE50104042D1

公开(公告)日：2004-11-11

申请号：DE50104042

申请日：2001-11-29

Applicant: BASF AG

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

IPC: C07C209/84 ,  C07C211/09 ,  C07C253/34 ,  C07C255/24

Abstract: A process is provided for reducing the content of a monounsaturated aliphatic amine (III) in a mixture (IV) containing an aminonitrile (I) or a diamine (II), or mixtures thereof, and the amine (III), whereina) the mixture (IV) is reacted with an anionic nucleophile (V),which contains a nucleophilic atom selected from the group comprising oxygen, nitrogen and sulfur,which is capable of taking up an H ion to form an acid with a pKa ranging from 7 to 11, measured in water at 25° C., andwhich has a relative nucleophilicity, measured in methyl perchlorate/methanol at 25° C.,ranging from 3.4 to 4.7 when oxygen is the nucleophilic atom,ranging from 4.5 to 5.8 when nitrogen is the nucleophilic atom, andranging from 5.5 to 6.8 when sulfur is the nucleophilic atom,in an amount ranging from 0.01 to 10 mol per mole of amine (III) in the mixture (IV), to give a mixture (VI), andb) the aminonitrile (I) or the diamine (II), or mixtures thereof, are distilled from the mixture (VI) at a temperature ranging from 50 to 170° C. and a pressure ranging from 0.5 to 100 kPa.

公开(公告)号：AT278662T

公开(公告)日：2004-10-15

申请号：AT01984785

申请日：2001-11-29

Applicant: BASF AG

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

IPC: C07C209/84 ,  C07C211/09 ,  C07C253/34 ,  C07C255/24

Abstract: A process is provided for reducing the content of a monounsaturated aliphatic amine (III) in a mixture (IV) containing an aminonitrile (I) or a diamine (II), or mixtures thereof, and the amine (III), whereina) the mixture (IV) is reacted with an anionic nucleophile (V),which contains a nucleophilic atom selected from the group comprising oxygen, nitrogen and sulfur,which is capable of taking up an H ion to form an acid with a pKa ranging from 7 to 11, measured in water at 25° C., andwhich has a relative nucleophilicity, measured in methyl perchlorate/methanol at 25° C.,ranging from 3.4 to 4.7 when oxygen is the nucleophilic atom,ranging from 4.5 to 5.8 when nitrogen is the nucleophilic atom, andranging from 5.5 to 6.8 when sulfur is the nucleophilic atom,in an amount ranging from 0.01 to 10 mol per mole of amine (III) in the mixture (IV), to give a mixture (VI), andb) the aminonitrile (I) or the diamine (II), or mixtures thereof, are distilled from the mixture (VI) at a temperature ranging from 50 to 170° C. and a pressure ranging from 0.5 to 100 kPa.

公开(公告)号：AU2003293671A1

公开(公告)日：2004-06-03

申请号：AU2003293671

申请日：2003-11-11

Applicant: BASF AG

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

IPC: C07D201/16 ,  C07D201/08

Abstract: A process for the purification of crude caprolactam, prepared by reaction of a mixture comprising 6-aminocapronitrile and water, comprises a three stage distillation process with feeding of the crude caprolactam and an inorganic acid having a b. pt. above the b. pt. of the caprolactam to a first distillation column. A process for the purification of crude caprolactam, prepared by reaction of a mixture comprising 6-aminocapronitrile and water in the presence of a catalyst to form a mixture comprising caprolactam, ammonia, water and high and low b. pt. byproducts followed by removal of ammonia to yield a mixture of caprolactam, water and high and low b. pt. byproducts followed by at least partial removal of water to yield a crude caprolactam containing caprolactam and high and low b. pt. byproducts, comprises: (a) feeding of the crude caprolactam and an inorganic acid having a b. pt. above the b. pt. of the caprolactam to a first distillation column; (b) distillation of the crude caprolactam and inorganic acid to form a sump stream and an overhead stream; (c) feeding of the overhead stream to a second distillation column; (d) distillation of the stream to form a sump stream and overhead stream; (e) feeding of the overhead stream to a third distillation column; (f) distillation of the overhead stream to form a sump stream and purified caprolactam in the overhead stream; and (g) feeding of the sump stream to the first distillation column.

公开(公告)号：AU2003282093A1

公开(公告)日：2004-06-03

申请号：AU2003282093

申请日：2003-11-11

Applicant: BASF AG

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

IPC: C07D201/08 ,  C07D201/16

Abstract: A process for removing high boilers from crude caprolactam which comprises high boilers, caprolactam and in some cases low boilers, and which has been obtained by a) reacting 6-aminocapronitrile with water to give a reaction mixture b) removing ammonia and unconverted water from the reaction mixture to obtain crude caprolactam, which comprises c) feeding the crude caprolactam to a distillation apparatus to obtain a first substream via the top as a product and a second substream via the bottom, by setting the pressure in the distillation in such a way that the bottom temperature does not go below 170° C., and adjusting the second substream in such a way that the caprolactam content of the second substream is not less than 10% by weight, based on the entire second substream.

公开(公告)号：CA2505359A1

公开(公告)日：2004-05-27

申请号：CA2505359

申请日：2003-11-11

Applicant: BASF AG

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

IPC: C07D201/16 ,  C07D201/08

Abstract: The invention relates to a method for purifying crude caprolactam that has been obtained by: 1) reacting a mixture (I) containing 6-aminocapronitrile a nd water to form a mixture (II) containing caprolactam, ammonia, water, high boilers and low boilers in the presence of a catalyst followed by; 2) removi ng ammonia from mixture (II) while obtaining a mixture (III) that contains caprolactam, water, high boilers and low boilers, after which; 3) water is entirely or partially removed from mixture (III) while obtaining a crude caprolactam (IV) that contains caprolactam, high boilers and low boilers. Th e inventive method is characterized in that: a) the crude caprolactam and an inorganic acid, which has a boiling point higher that that of caprolactam under distillation conditions in accordance with subsequent steps b) to h), are fed to a first distillation device K1; b) the crude caprolactam and the inorganic acid are distilled in the first distillation device K1 during whic h a first partial flow in the bottom area and a second partial flow in the top area are withdrawn from the distillation device K1; c) the second partial fl ow from step b) is fed to a second distillation device K2; d) the second partia l flow from step b) is distilled in the second distillation device K2 during which a first partial flow in the bottom area and a second partial flow in t he top area are withdrawn from the distillation device K2; e) a first partial flow from step d) is fed to a third distillation device K3; f) the first partial flow from step d) is distilled in the third distillation device K3 during which a first partial flow in the bottom area and purified caprolacta m in the top area are withdrawn from the distillation device K3, and; g) the first partial flow from step f) is fed to the first distillation device K1.

公开(公告)号：CA2505356A1

公开(公告)日：2004-05-27

申请号：CA2505356

申请日：2003-11-11

Applicant: BASF AG

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

IPC: C07D201/08 ,  C07D201/16

Abstract: The invention relates to a method for separating high boilers out from a cru de caprolactam, which contains high boilers, caprolactam and, optionally, light boilers, and which has been obtained by: a) reacting 6-aminocapronitrile wit h water to form a reaction mixture, and; b) separating ammonia and unreacted water out from the reaction mixture while obtaining a crude caprolactam. The invention is characterized in that: c) the crude caprolactam is fed to a distillation device while obtaining, as a product, a first partial flow via the top, and obtaining a second partial flow via the bottom. During distillation, the pressure is set so that a bottom temperature of 170 ~C is not fallen below, and the second partial flow is set so that the caprolactam content of the second partial flow is no less than 10 % by weight with regar d to the entire second partial flow.

公开(公告)号：CA2485077A1

公开(公告)日：2003-12-04

申请号：CA2485077

申请日：2003-05-21

Applicant: BASF AG

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

IPC: C07C209/84 ,  C07C211/09 ,  C07C211/12 ,  C07C253/34 ,  C07C255/09 ,  C07C255/24

Abstract: The invention relates to a method for reducing the content of an aliphatic, monounsaturated amine (IV) in a mixture (V) containing an aminonitrile (I) o r a diamine (II) or a dinitrile (III) or mixtures thereof and amine (IV), whereby: a) mixture (V) is reacted with an anionic nucleophile (VI) in a quantity ranging from 0.01 to 10 mols per mol of amine (IV) in mixture (V) a t a temperature ranging from 50 to 200 ~C while obtaining mixture (VII), and; b) amino nitrile (I) or diamine (II) or dinitrile (III) or mixtures thereof are removed by distillation from mixture (VII) at a temperature ranging from 50 to 200 ~C and under a pressure ranging from 0.1 to 100 kPa while obtaining a bottom product (VIII). The inventive method is characterized in that: c) an amino nitrile (I) or diamine (II) or dinitrile (III) or mixtures thereof are removed by distillation from bottom product (VIII) at a temperature which is lower than that selected in step b).

公开(公告)号：BR0115648A

公开(公告)日：2003-09-02

申请号：BR0115648

申请日：2001-11-29

Applicant: BASF AG

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

IPC: C07C209/84 ,  C07C211/09 ,  C07C253/34 ,  C07C255/24

Abstract: A process is provided for reducing the content of a monounsaturated aliphatic amine (III) in a mixture (IV) containing an aminonitrile (I) or a diamine (II), or mixtures thereof, and the amine (III), whereina) the mixture (IV) is reacted with an anionic nucleophile (V),which contains a nucleophilic atom selected from the group comprising oxygen, nitrogen and sulfur,which is capable of taking up an H ion to form an acid with a pKa ranging from 7 to 11, measured in water at 25° C., andwhich has a relative nucleophilicity, measured in methyl perchlorate/methanol at 25° C.,ranging from 3.4 to 4.7 when oxygen is the nucleophilic atom,ranging from 4.5 to 5.8 when nitrogen is the nucleophilic atom, andranging from 5.5 to 6.8 when sulfur is the nucleophilic atom,in an amount ranging from 0.01 to 10 mol per mole of amine (III) in the mixture (IV), to give a mixture (VI), andb) the aminonitrile (I) or the diamine (II), or mixtures thereof, are distilled from the mixture (VI) at a temperature ranging from 50 to 170° C. and a pressure ranging from 0.5 to 100 kPa.

公开(公告)号：AR029914A1

公开(公告)日：2003-07-23

申请号：ARP010101992

申请日：2001-04-27

Applicant: BASF AG

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

IPC: C08J5/18 ,  C08G69/04 ,  C08G69/14 ,  C08G69/16

Abstract: Procedimientos para la obtencion de caprolactama, así como procedimientos para la obtencion de polímeros usando caprolactama son generalmente conocidos. Los procedimientos de purificacion del producto citado obtenido tienen la desventaja, que son técnicamente complicados y requieren mucha energía, especialmente, por las numerosas etapas de separacion. Se provee un procedimiento que permite obtener polímeros a base de caprolactama de manera técnicamente sencilla y con ahorro de energía, obteniéndose polímeros con índices característicos de producto comparables con polímeros a base de caprolactama purificados mediante procedimientos técnicamente más complicados y con mayor consumo de energía. Procedimiento para la obtencion de un polímero usando caprolactama en donde: a) se hace reaccionar una mezcla (I) que contiene 6-aminocapronitrilo y agua, dando una mezcla (II) que contiene caprolactama, amoníaco, agua componentes de alto punto de ebullicion y componentes de bajo punto de ebullicion, en presencia de un solido que fomenta catalíticamente la reaccion, luego b) se elimina el amoníaco de la mezcla (II), obteniéndose una mezcla (III) que contienen caprolactama, agua, componentes de alto punto de ebullicion y componentes de bajo punto de ebullicion, luego c) se elimina el agua parcial o completamente de la mezcla (III), obteniéndose una mezcla (IV) que contienen caprolactama, componentes de alto punto de ebullicion y componentes de bajo punto de ebullicion, y luego d) se polimeriza la mezcla (IV), así como un polímero obtenido segun este procedimiento, a su uso para la fabricacion de fibras, materiales de estructura plana y cuerpos moldeados, así como a fibras, materiales de estructura plana y cuerpos moldeados obtenidos usando tal polímero.