Method for preparing caprolactam
    2.
    发明专利

    公开(公告)号:SK284227B6

    公开(公告)日:2004-11-03

    申请号:SK63697

    申请日:1995-11-29

    Applicant: BASF AG

    Abstract: Method for preparing caprolactam by heating 6-aminocapric acid nitrile in the presence of heterogeneous catalysts and 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.

    3.
    发明专利
    未知

    公开(公告)号:ES2201127T3

    公开(公告)日:2004-03-16

    申请号:ES95942198

    申请日:1995-12-22

    Applicant: BASF AG

    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.

    Process for preparing caprolactam

    公开(公告)号:CZ291034B6

    公开(公告)日:2002-12-11

    申请号:CZ146997

    申请日:1995-11-14

    Applicant: BASF AG

    Abstract: The present invention relates to a process for preparing caprolactam 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 50 to 98 percent by weight of water, and 2 to 50 percent by weight of a mixture containing 50 to 90 percent by weight of caprolactam and 10 to 50 percent by weight of 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 50 to 90 percent by weight of caprolactam and the 10 to 50 percent by weight of the high-boiling fraction, then (c) the caprolactam and the high-boiling fraction from the mixture II are separated from one another by distillation, and then either (d1) the high-boiling fraction from stage (c) is fed into the reactor A of stage (a) or (d2) the high-boiling fraction is heated similarly to stage (a) in a further reactor B to a temperature in the range of 250 to 350 degC and then worked up similarly to stages (b) and (c) to give further caprolactam, or (d3) the high-boiling fraction is heated under reduced pressure to a temperature in the range of 200 to 400 degC and in the presence of a base in a reactor C and the reacted mixture is worked up by distillation to give caprolactam.

    METHOD OF SIMULTANEOUSLY PREPARING CAPROLACTAM AND HEXAMETHYLENE DIAMINE

    公开(公告)号:SK84297A3

    公开(公告)日:1998-03-04

    申请号:SK84297

    申请日:1995-12-22

    Applicant: BASF AG

    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.

    8.
    发明专利
    未知

    公开(公告)号:BR9509948A

    公开(公告)日:1998-01-27

    申请号:BR9509948

    申请日:1995-11-29

    Applicant: BASF AG

    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.

    Process for the continuous preparation of pure 5-formyl valeric acid esters

    公开(公告)号:AU6787296A

    公开(公告)日:1997-03-05

    申请号:AU6787296

    申请日:1996-07-26

    Applicant: BASF AG

    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.

    Method of producing caprolactam
    10.
    发明专利

    公开(公告)号:AU3928795A

    公开(公告)日:1996-06-19

    申请号:AU3928795

    申请日:1995-11-14

    Applicant: BASF AG

    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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