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公开(公告)号：DE4443125A1
公开(公告)日：1996-06-05
申请号：DE4443125
申请日：1994-12-03
Applicant: BASF AG
Inventor： FUCHS EBERHARD DR , ACHHAMMER GUENTHER DR
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 6-aminocapric 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 6-aminocapric 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.
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公开(公告)号：DE19614153A1
公开(公告)日：1997-10-16
申请号：DE19614153
申请日：1996-04-10
Applicant: BASF AG
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 or-NR'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.
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公开(公告)号：DE19548289A1
公开(公告)日：1997-06-26
申请号：DE19548289
申请日：1995-12-22
Applicant: BASF AG
Inventor： ACHHAMMER GUENTHER DR , BASLER PETER DR , FISCHER ROLF DR , FUCHS EBERHARD DR , LUYKEN HERMANN , SCHNURR WERNER DR , VOIT GUIDO DR , HILPRECHT LUTZ DR
IPC: C07C209/48 , C07C209/86 , C07C211/12 , C07D201/08 , C07D223/10
Abstract: A process is disclosed for simultaneously preparing caprolactam and hexamethylene diamine starting from adipodinitrile.
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公开(公告)号：DE19536777C1
公开(公告)日：1997-05-15
申请号：DE19536777
申请日：1995-10-04
Applicant: BASF AG
Inventor： HEINEKE DANIEL DR , RIEKER CHRISTOPHER WILLIAM , OOSTVOGELS JOZEF , POSTELMANS DANY DR , SCHNEIDER HEINZ-WALTER DR , THOME ALFRED DR , ACHHAMMER GUENTHER DR
Abstract: The invention relates to a hydrogenation catalyst by the reduction from platinum in the stage of oxidation of +4 (Pt (IV)) with a selective reducing agent in an acidic aqueous medium in the presence of a carbon-containing carrier to platinum in the stage of oxidation +2 (Pt (II)), subsequent poisoning of the platinum thus obtained with a sulphur-containing selective reducing agent, and subsequent reduction of the platinum thus partially poisoned to form metallic platinum (Pt(0)) and subsequent processing as known per se in that (a) Pt (II) is partially poisoned with a sulphur-containing selective reducing agent, wherein the sulphur-containing selective reduction agent is used in an amount which corresponds to from 15 to 70 mol % of the amount of the sulphur-containing selective reducing agent which might be needed to reduce Pt(IV) to Pt (II), provided that the amount of Pt (IV) corresponds to the amount of Pt (II) used and to be poisoned, and subsequently the partially poisoned Pt (II) is reduced with an alkali metal formate to Pt (0); or (b) platinum in the stage of oxidation of greater than +2 is partially poisoned and subsequently or simultaneously reduced with an alkali metal formate to Pt (0). The invention also relates to a hydrogenation catalyst, use of the hydrogenation catalyst for preparing hydroxylammonium salts, a process for the preparation of hydroxylammonium salts, and a process for regenerating platinum-containing hydrogenation catalysts.
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Patent Agency Ranking
公开(公告)号：DE19529239A1
公开(公告)日：1997-02-13
申请号：DE19529239
申请日：1995-08-09
Applicant: BASF AG
Inventor： ACHHAMMER GUENTHER DR , ROEPER MICHAEL PROF DR
IPC: C07C67/54 , C07C69/716 , C07C69/738 , C07C67/38
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 DEG 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.
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公开(公告)号：DE4441962A1
公开(公告)日：1996-05-30
申请号：DE4441962
申请日：1994-11-25
Applicant: BASF AG
Inventor： ACHHAMMER GUENTHER DR , FUCHS EBERHARD DR
IPC: C07D201/08 , C07D223/10
Abstract: Caprolactam is prepared by reacting a solution of 6-aminocapronitrile with water in the liquid phase at elevated temperatures by a process in which (a) an aqueous solution of 6-aminocapronitrile in the liquid phase is heated without the addition of a catalyst in a reactor A to give a mixture I consisting essentially of water, caprolactam and a high-boiling fraction (high boiler), then (b) the water is removed from the resulting mixture I to give a mixture II consisting essentially of caprolactam and the high boilers, then (c) the caprolactam and the high boilers from mixture II are separated from one another by distillation, and then either (d1) the high boilers from stage (c) are fed into the reactor A of stage (a) or (d2) the high boilers are heated similarly to stage (a) in a further reactor B and then worked up similarly to stages (b) and (c) to give further caprolactam, or (d3) the high boilers are heated under reduced pressure in the presence of a base in a reactor C and the reacted mixture is worked up by distillation to give caprolactam.
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公开(公告)号：DE19628805A1
公开(公告)日：1998-01-22
申请号：DE19628805
申请日：1996-07-17
Applicant: BASF AG
Inventor： RITZ JOSEF DR , ACHHAMMER GUENTHER DR , FISCHER ROLF DR , FUCHS EBERHARD DR , VOIT GUIDO DR
IPC: C07C231/06 , C07C237/06 , C07C253/00 , C07C255/24 , C07D201/08 , C07D201/12 , C07D201/16 , C07D223/10
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.
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公开(公告)号：DE19500222A1
公开(公告)日：1996-07-11
申请号：DE19500222
申请日：1995-01-05
Applicant: BASF AG
Inventor： ACHHAMMER GUENTHER DR , BASLER PETER DR , FISCHER ROLF DR , FUCHS EBERHARD DR , LUYKEN HERMANN , SCHNURR WERNER DR , WITZEL TOM DR
IPC: C07D201/02 , C07C209/48 , C07C211/12 , C07D201/08 , C07D223/10 , C07D233/10
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.
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公开(公告)号：DE19500041A1
公开(公告)日：1996-07-04
申请号：DE19500041
申请日：1995-01-03
Applicant: BASF AG
Inventor： RITZ JOSEF DR , FISCHER ROLF DR , SCHNURR WERNER DR , FUCHS EBERHARD DR , ACHHAMMER GUENTHER DR , LUYKEN HERMANN
IPC: C07D201/08 , C07B63/02 , C07D201/16 , C07D223/10
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.
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