公开(公告)号：PL321267A1

公开(公告)日：1997-11-24

申请号：PL32126795

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：FI972839A0

公开(公告)日：1997-07-02

申请号：FI972839

申请日：1997-07-02

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 ,  C07C

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：NO972503D0

公开(公告)日：1997-06-02

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.

公开(公告)号：DE50108247D1

公开(公告)日：2006-01-05

申请号：DE50108247

申请日：2001-06-13

Applicant: BASF AG

Inventor： LUYKEN HERMANN ,  OHLBACH DR ,  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：DE10256578A1

公开(公告)日：2004-06-17

申请号：DE10256578

申请日：2002-12-04

Applicant: BASF AG

Inventor： BASLER PETER ,  SIEGEL WOLFGANG ,  ACHHAMMER GUENTHER ,  NEGELE ANTON ,  MENIG HELMUTH ,  RUPPEL WILHELM ,  ZEHNER PETER ,  LUYKEN HERMANN ,  VOGT VOLKER

IPC: B01J12/00 ,  B01J15/00 ,  B01J19/02 ,  B01J19/24 ,  B01J23/86 ,  C01C3/02

公开(公告)号：PL186443B1

公开(公告)日：2004-01-30

申请号：PL32116295

申请日：1995-12-22

Applicant: BASF AG

Inventor： RITZ JOSEF ,  FISCHER ROLF ,  SCHNURR WERNER ,  ACHHAMMER GUENTHER ,  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：DE10138553A1

公开(公告)日：2003-05-28

申请号：DE10138553

申请日：2001-08-06

Applicant: BASF AG

Inventor： BASLER PETER ,  SIEGEL WOLFGANG ,  ACHHAMMER GUENTHER ,  NEGELE ANTON ,  MENIG HELMUTH ,  WINTER MANFRED ,  RUPPEL WILHELM ,  RESCH PETER ,  ZEHNER PETER ,  LUYKEN HERMANN ,  SCHINDLER GOETZ-PETER ,  VOGT VOLKER

IPC: B01J19/30 ,  B01J19/32 ,  B01J23/745 ,  C01C3/02

Abstract: Hydrogen cyanide (hydrocyanic acid) production by dehydration of gaseous formamide in presence of atmospheric oxygen is effected using a catalyst containing metallic iron or iron oxide. An Independent claim is also included for use of ordered packings of steel and iron oxide on an aluminum oxide carrier as catalyst in hydrogen cyanide production by dehydration of gaseous formamide containing atmospheric oxygen.

公开(公告)号：DE59506855D1

公开(公告)日：1999-10-21

申请号：DE59506855

申请日：1995-11-29

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：EA199800190A1

公开(公告)日：1998-10-29

申请号：EA199800190

申请日：1996-07-26

Applicant: BASF AG

Inventor： ROEPER MICHAEL ,  ACHHAMMER GUENTHER

IPC: C07C67/54 ,  C07C69/716

Abstract: Способполученияэфиров 5-формилвалериановойкислотыс выходомнеменеечем 90%, перегонкойсмесиэфировформилвалериановыхкислот, состоящейизэфиров 5-формилвалериановойкислотыи эфировили 3-, или 4-формилвалериановыхкислот, илисмеси, состоящейизэфиров 3- и 4-формилвалериановыхкислот, причемэфирныеостаткисоответствующихформилвалериановыхкислотидентичны, покоторомуэфиры 3- или 4-формилвалериановыхкислотилиихсмесиотделяютотэфиров 5-формилвалериановойкислотынаректификационнойколонкепридавлениив интервалеот 2 до 100 мбари температуреневыше 150°С (измереннойкактемпературав нижнейчастиколонки), ив качествеэфировиспользуютсоответствующиеметиловыеилиэтиловыеэфиры, иприэтомчистотаэфиров 5-формилвалериановойкислотысоставляетнеменее 98% иэфир 4-формилвалериановойкислотыприсутствуетв качествепримесив количественеболее 100 млн.долей.Международнаязаявкабылаопубликованавместес отчетомо международномпоиске.

公开(公告)号：BG101661A

公开(公告)日：1998-02-27

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 ofcaprolactam and hexamethylene diamine from adipodinitrile, by thefollowing steps: (a) the adipodinitrile is partially hydrogenated,producing a mixture substantially containing 6-aminocapronitrile,hexamethylene diamine, ammonia, adipodinitrile and hexamethyleneimine ( "the mixture"); (b) the mixture obtained in step (a) isdistilled, producing ammonia, as the forerunnings, and a residueI, in the presence of a compound A which is inert in thedistillation conditions, the ammonia not being separated totally;(c) the residue I, substantially containing 'the mixture", inertcompound A and ammonia, the ammonia content being less than thatof the mixture used in step (b), is subjected to a seconddistillation, producing a mixture of the inert compound A andammonia, as the forerunnings, and a residue II; (d) the base II,substantially containing "the mixture" and inert compound A, issubjected to distillation in a third column, producing the inertcompound A, as the forerunnings, and a residue III; (e) the baseIII, substantially containing "the mixture" and optionally aninert compound B, is subjected to distillation in a fourth column,producing forerunnings KP, which substantially containhexamethylene imine, optionally inert compound B and hexamethylenediamine, and a residue IV; (f) the forerunnings KP are subjectedin a fifth column to distillation, producing forerunnings KP2,which substantially contain hexamethylene imine and optionallyinert compound B, and a residue V, which substantially containshexamethylene diamine with a degree of purity of at least 95 %,the forerunnings KP2 being fed to the third column or optionallyonly partially fed to the third column, and the rest beingdiscarded; and (g) the residue IV, substantially containing6-aminocapronitrile and adipodinitrile, is subjected in a sixthcolumn to distillation, producing 6-aminocapronitrile with adegree of purity of at least 95 %, as forerunnings, andadiponitrile in the residue. The resultant 6-aminocapronitrile iscyclized to form caprolactam.