公开(公告)号：BR9710470A

公开(公告)日：1999-08-17

申请号：BR9710470

申请日：1997-07-07

Applicant: BASF AG

Inventor： RITZ JOSEF ,  ACHHAMMER GUENTHER ,  FISCHER ROLF ,  FUCHS EBERHARD ,  VOIT GUIDO

IPC: C07C231/06 ,  C07C237/06 ,  C07C253/00 ,  C07C255/24 ,  C07D201/08 ,  C07D201/12 ,  C07D201/16

Abstract: A process for preparing caprolactam by cyclization of 6-aminocapronitrile in the presence of water at elevated temperature and in the presence or absence of a catalyst and a solvent, comprises a) removing from the cyclization reaction effluent ("reaction effluent I") caprolactam and all components boiling higher than caprolactam ("high boilers"), b) treating the high boilers of stage a) with phosphoric acid and/or polyphosphoric acid at from 200 to 350 DEG C. to obtain a reaction effluent II, and c) removing caprolactam formed and any 6-aminocapronitrile from reaction effluent II of stage b) to obtain separation from unconverted high boilers and acid used.

公开(公告)号：TR9800187T1

公开(公告)日：1998-05-21

申请号：TR9800187

申请日：1996-07-26

Applicant: BASF AG

Inventor： ACHHAMMER GUENTHER ,  ROEPER MICHAEL

IPC: C07C67/54 ,  C07C69/716

CPC classification number: C07C67/54 ,  C07C69/716

公开(公告)号：TR199800187T1

公开(公告)日：1998-05-21

申请号：TR9800187

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：HUT77062A

公开(公告)日：1998-03-02

申请号：HU9702104

申请日：1995-11-29

Applicant: BASF AG

Inventor： ACHHAMMER GUENTHER ,  FUCHS EBERHARD

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：BG101596A

公开(公告)日：1998-02-27

申请号：BG10159697

申请日：1997-06-10

Applicant: BASF AG

Inventor： FUCHS EBERHARD ,  ACHHAMMER GUENTHER

IPC: C07D201/08 ,  C07D223/10

Abstract: The invention relates to a method for the preparation ofcaprolactam by heating of 6-aminocapronitrile in the presence ofheterogenous catalyst and water under increased pressure where:(a) 6-aminocapronitrile or a mixture containing basically6-aminocapronitrile and water and low-boiling or high-boilingalcohol are heated in the presence of heterogenous catalyst inreactor (A) for producing mixture (I). Then, (b) mixture (I) isdistilled, divided in a fraction from the top of the column,caprolactam and bottom residue as any ammonia in mixture (I) isremoved before the distillation, after which (c1) fraction fromthe top of the column is introduced in the reactor from stage (a).The fraction from the top of the column is usually mixed withalcohol and/or water, and/or 6-aminocapronitrile used in stage(a), before being introduced in reactor (A), or (c2) the fractionfrom the top of the column is optionally introduced in reactor (B)together with the bottom residue of stage (b). The fraction fromthe top of the column is optionally mixed with the alcohol and/orwater, and/or 6-aminocapronitrile used in stage (a) before beingintroduced in reactor (B). Finally, analogically to stage (b) bydistillation caprolactam is extracted and (d1) the bottom residueof stage (b) is introduced in reactor (A) of stage (a) or (d2) thebottom residue is mixed in a given case with water and optionally- with low-boiling or high-boiling alochol. After that,analogically to stage (a) it is heated in a subsequent reactor (C)to the preparation of a reaction product which is subjected todistillation for the production of caprolactam, or (d3) water isadded to the bottom residue heated in reactor (D) without theaddition of any catalyst for the production of a reaction productwhich is distilled for the production of the caprolactam, or (d4)water and base is added to the bottom residue. The residue isheated in reactor (E) until the production of a reaction productwhich is distilled for the preparation of caprolactam.

公开(公告)号：PL321162A1

公开(公告)日：1997-11-24

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：CA2209336A1

公开(公告)日：1996-07-11

申请号：CA2209336

申请日：1995-12-22

Applicant: BASF AG

Inventor： RITZ JOSEF ,  LUYKEN HERMANN ,  FISCHER ROLF ,  ACHHAMMER GUENTHER ,  SCHNURR WERNER ,  FUCHS EBERHARD

IPC: C07D201/08 ,  C07B63/02 ,  C07D201/16 ,  C07D223/10

Abstract: Cleaning raw caprolactam by hydration, subsequent treatment in an acid medium and final distillation in an alkaline medium, in which (a) 6-amino capronitrile is converted into raw caprolactam by reaction with water; (b) difficultly and easily boiling components are removed from the raw caprolactam from step (a); (c) the raw caprolactam from step (b) is treated with hydrogen at a temperature in the 50 to 150 .degree.C range and a pressure in the 1.5 to 250 bar range in the presence of a hydration catalyst and, if desired, a solvent, to give a mixture A;(d1) mixture A is taken at a temperature in the 30 to 80 .degree.C range and a pressure in the 1 to 5 bar range over an ion exchanger containing acid terminal groups to give a mixture B1 or (d2) mixture A is distilled in the presence of sulphuric acid, in which any solvent is removed before the addition of the sulphuric acid to give a mixture B2; and (e) mixture B1 or B2 is distilled in the presence of a base to yield pure caprolactam.

公开(公告)号：PL187887B1

公开(公告)日：2004-10-29

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：PL186239B1

公开(公告)日：2003-12-31

申请号：PL32050295

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：DE59510717D1

公开(公告)日：2003-07-10

申请号：DE59510717

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.