公开(公告)号：CA2250745A1

公开(公告)日：1997-10-16

申请号：CA2250745

申请日：1997-04-01

Applicant: BASF AG

Inventor： THOME ALFRED ,  ACHHAMMER GUENTHER ,  SCHNEIDER HEINZ-WALTER ,  HEINEKE DANIEL

IPC: B01J23/42 ,  B01J37/20 ,  C01B21/14 ,  C01B21/087 ,  B01J23/96

Abstract: The invention concerns the manufacture of a hydrogenation catalyst by the reduction of platinum from an oxidation state of not less than two with a reducing agent in an aqueous medium in the presence of a carbon-containing support following partial poisoning, the method using a compound of general formula (I) in which X, Y and Z, which may be the same or different, are hydrogen, C1-C18 alkyl, C5-C10 cycloalkyl, halogen, hydroxyl, C1-C6 alkoxy orNR'R'', whereby R, R' and R'', which may by the same or different, are hydrogen, C1-C18 alkyl or C5-C10 cycloalkyl. The invention also concerns a hydrogenation catalyst manufactured by this method, its use in the production of hydroxylammonium salts, a method of producing hydroxylammonium salts and a method of regenerating platinum-based hydrogenation catalysts of this kind.

公开(公告)号：CA2237727A1

公开(公告)日：1997-07-03

申请号：CA2237727

申请日：1996-12-11

Applicant: BASF AG

Inventor： FISCHER ROLF ,  HILPRECHT LUTZ ,  SCHNURR WERNER ,  VOIT GUIDO ,  LUYKEN HERMANN ,  ACHHAMMER GUENTHER ,  BASSLER PETER ,  FUCHS EBERHARD

IPC: C07C209/48 ,  C07C209/86 ,  C07C211/12 ,  C07D201/08 ,  C07D223/10 ,  C07C255/24 ,  C07C253/34

Abstract: A process is disclosed for simultaneously preparing caprolactam and hexamethylene diamine starting from adipodinitrile.

公开(公告)号：CA2225649A1

公开(公告)日：1997-02-20

申请号：CA2225649

申请日：1996-07-26

Applicant: BASF AG

Inventor： R PER MICHAEL ,  ACHHAMMER GUENTHER

IPC: C07C67/54 ,  C07C69/716

Abstract: The production of 5-formyl valeric acid ester with a yield of not less than 90 % by the distillation of a mixture of 5-formyl valeric acid ester and either 3 or 4-formyl valeric acid ester or a mixture of 3 and 4-formyl valeric acid esters, in which the ester radicals of the formyl valeric acid esters are identical, by separating the 3 or 4-formyl valeric acid esters of their mixtures from the 5-formyl valeric acid ester at a pressure between 2 and 100 mbar and a temperature not exceeding 150 ~C (measured as the column well temperature) in a distillation column, and using the corresponding ethyl or ethyl ester as the esters, and in which the purity of the 5-formyl valeric ester is no lower than 98 % and 4-formyl valeric acid ester is present as an impurity in a quantity of no more than 100 ppm.

公开(公告)号：CA2207942A1

公开(公告)日：1996-06-13

申请号：CA2207942

申请日：1995-11-29

Applicant: BASF AG

Inventor： FUCHS EBERHARD ,  ACHHAMMER GUENTHER

IPC: C07D201/08 ,  C07D223/10

Abstract: Method for preparing caprolactam by heating 6-aminocapric acid nitrile in the presence of heterogeneous catalysts ans water under elevated pressure, wherein (a) 6-aminocapric acid nitrile or a mixture containing essentially 6aminocapric acid nitrile as well as water and a low-boiling or a high-boiling alcohol is heated in the presence of a heterogeneous catalyst in a reactor A to produce a mixture (I); then (b) mixture (I) is distilled, yielding a head fraction, caprolactam and a bottom product, with any ammonia in mixture (I) being removed prior to distillation; and then (c1) the head fraction is fed into the reactor of step (a), with the head fraction optionally being mixed with the alcohol and/or water and/or 6-aminocapric nitrile used in step (a) before being fed into reactor (A); or (c2) the head fraction, optionally with the bottom product from step (b), is fed into a reactor (B), the first fraction optionally being mixed with the alcohol and/or water and/or 6aminocapric acid nitrile before being fed into reactor (B), and then analogously to step (b) caprolactam is produced by distillation; and either (d1) the bottom product from step (b) is fed into reactor A of step (a); or (d2) optionally water and possibly a low-boiling or a high-boiling alcohol are added to the bottom product which then, analogously to step (a) is heated in a reactor (C) to give a reaction product which is distilled to yield caprolactam; or (d3) water is added to the bottom product which is heated in a reactor (D) without added catalyst to give a reaction product which is distilled to yield caprolactam; or (d4) water and a base are added to the bottom product which is heated in reactor (E) to give a reaction product which is distilled to yield caprolactam.

公开(公告)号：FI115907B

公开(公告)日：2005-08-15

申请号：FI972340

申请日：1997-06-02

Applicant: BASF AG

Inventor： FUCHS EBERHARD ,  ACHHAMMER GUENTHER

IPC: C07D201/08 ,  C07D223/10

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：DE59907216D1

公开(公告)日：2003-11-06

申请号：DE59907216

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：BR0111788A

公开(公告)日：2003-05-20

申请号：BR0111788

申请日：2001-06-13

Applicant: BASF AG

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

IPC: C07C209/48 ,  C07C253/34 ,  C07C255/03 ,  C07C255/24

Abstract: The invention relates to a method for removing, by distillation, 6-aminocapronitrile from mixtures that contain 6-aminocapronitrile, adipodinitrile and hexamethylenediamine, by a) removing the hexamethylenediamine from the mixture while obtaining a mixture (I) that has a hexamethylenediamine content of less than 1 wt. -%, b) removing completely or partially the 6-aminocapronitrile from mixture (I) while obtaining a mixture (II) whose content in substances that have a higher boiling point as 6-aminocapronitrile under distillation conditions and that cannot be formed by dimerization reactions when 6-aminocapronitrile is thermally treated is less than 1 wt. -%, and c) completely or partially removing from mixture (II) the hexamethylenediamine that might be present while obtaining a mixture (IV) whose hexamethylenediamine content is higher than that of mixture (II), and a mixture (V) whose hexamethylenediamine content is lower than that of mixture (II).

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：DE59605949D1

公开(公告)日：2000-11-02

申请号：DE59605949

申请日：1996-07-26

Applicant: BASF AG

Inventor： ACHHAMMER GUENTHER ,  ROEPER MICHAEL

IPC: C07C67/54 ,  C07C69/716

Abstract: PCT No. PCT/EP96/03290 Sec. 371 Date Jan. 27, 1998 Sec. 102(e) Date Jan. 27, 1998 PCT Filed Jul. 26, 1996 PCT Pub. No. WO97/06126 PCT Pub. Date Feb. 20, 19975-Formylvaleric esters are prepared in a yield of not less than 90% by distillation of a formylvaleric ester mixture of 5-formylvaleric ester and either 3- or 4-formylvaleric ester or a mixture of 3- and 4-formylvaleric esters, where the ester radicals of the respective formylvaleric esters are identical, wherein the 3- or 4-formylvaleric ester or a mixture thereof is separated from the 5-formylvaleric ester in a distillation column at a pressure in the range from 2 to 100 mbar and a temperature of not above 150 DEG C. (measured as the temperature at the bottom of the column) and the esters used are the corresponding methyl or ethyl esters, where the purity of the 5-formylvaleric ester is not less than 98% and, as impurity, 4-formylvaleric ester is present in an amount of not more than 100 ppm.

公开(公告)号：NO307374B1

公开(公告)日：2000-03-27

申请号：NO972503

申请日：1997-06-02

Applicant: BASF AG

Inventor： FUCHS EBERHARD ,  ACHHAMMER GUENTHER

IPC: C07D201/08 ,  C07D223/10

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.