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    21.
    发明专利
    未知

    公开(公告)号：DE4422610A1

    公开(公告)日：1996-01-04

    申请号：DE4422610

    申请日：1994-06-28

    Applicant: BASF AG

    Inventor： FUCHS EBERHARD DR ,  WITZEL TOM DR

    IPC: C07D201/08 ,  C07D223/10 ,  C07D227/087 ,  C07D211/76 ,  C07B47/00

    Abstract: Production of cyclic lactames by reaction with water of aminocarboxylic acid compounds of general formula (I) in which R is -OH, -O-C1-C2-alkyl or -NR -R , R and R are mutually independently hydrogen, C1-C12 alkyl and C5-C8 cycloalkyl and m is a whole number from 3 to 12. The reaction is conducted in the liquid phase using heterogeneous catalysts.

    Process for preparing caprolactam
    23.
    发明专利
    Process for preparing caprolactam 未知

    公开(公告)号：CZ290643B6

    公开(公告)日：2002-09-11

    申请号：CZ152597

    申请日：1995-11-29

    Applicant: BASF AG

    Inventor： FUCHS EBERHARD DR ,  ACHHAMMER GUNTER DR

    IPC: C07D201/08 ,  C07D223/10

    Abstract: In the present invention there is disclosed a process for preparing caprolactam comprising the following steps: (a) heating 6-aminocaproic acid nitrile or a mixture of nitrile/water/alcohol with a catalyst in a reactor A to obtain a mixture I; (b) distillation of the mixture I to obtain overhead distillate, caprolactam and a sink, whereby ammonia being present in the mixture I is optionally distilled off therefrom; (c) treating the overhead distillate in the A reactor of the step (a) after optional mixing thereof with the nitrile/water/alcohol mixture used in the step (a) prior introduction into the reactor A, or by introducing the overhead distillate, optionally with the sink of the step (b) into a reactor B, whereby prior introducing the overhead distillate into the reactor B can be optionally mixed with the nitrile/water/alcohol mixture used in the step (a) and then caprolactam is obtained by distillation in analogous way to the step (b), and (d) mixing the sink with water and heating thereof in a reactor D to obtain a reaction product, from which caprolactam is subsequently distilled off.

    Simultaneous separation process of 6-aminocapronitrile and hexamethylenediamine
    24.
    发明专利
    Simultaneous separation process of 6-aminocapronitrile and hexamethylenediamine 未知

    公开(公告)号：CZ289878B6

    公开(公告)日：2002-04-17

    申请号：CZ20012583

    申请日：2001-07-13

    Applicant: BASF AG

    Inventor： ACHHAMMER GUNTHER DR ,  BASSLER PETER DR ,  FISCHER ROLF DR ,  FUCHS EBERHARD DR ,  LUYKEN HERMANN ,  SCHNURR WERNER DR ,  WITZEL TOM DR

    IPC: C07C209/48 ,  C07C211/12 ,  C07D223/10

    Abstract: Simultaneous prepn of caprolactam and hexamethylene diamine (HMD) from adipo-dinitrile (ADN) comprises (a) partial hydrogenation of (I) to a mixt. of ADN; HMD, 6-amino-capronitrile (ACN) ammonia and hexamethylenimine (HMI); (b) distillation in a first column at 10-30 br and 60-220 deg C in the presence of an inert substance (A) that boils at 60-220 deg C at 18 bar, to remove most of the ammonia at the head, leaving a residue; (c) distillation in a second column of the residue which contains ADN, HMD, ACN, HMI, (A) and residual NH3) at 100-220 deg C and 2-15 bar, under conditions different from those in the first column, giving at column head temp. of at least 20 deg C and a sump. temp. of 220 deg C max, to remove the NH3 and some (A), leaving a residue; (d) distillation in a third column, of the residue (which contains ADN, HMD, ACN, HMI and (A) at 10-220 deg C and 0.1-2 bar, (opt. in the presence of an inert substance (B) that boils at 50-220 deg C at 0.3 bar) to remove (A) for return to the second column, leaving a residue; (e) distillation in a fourth column, of the residue (which contains ADN, HMD, ACN, HMI and opt. (B)) at 100-220 deg C and 10-500 mbar to give a head fraction KPI (contg. HMD, HMI and opt. (B) and a residue (R4); (f) distillation of KPI in a fifth column at 100-220 deg C and 50-2000 mbar, to give a head fraction KP2 (contg. HMI and opt. (B)) which is returned to column 3 or partly returned and partly removed, and a residue comprising 95% HMD; and (g) the residue (R4) from the fourth column, contg. ACN and (I), is distilled in a sixth column at 100-220 deg C and 1-500 mbar to give a head product contg. 95% ACN and a residue (R2) contg. ADN); (h) cyclising. Also claimed is a process for the simultaneous separation of HDM and ACN for (M) by steps (b)-(g).

    25.
    发明专利
    未知

    公开(公告)号：DE59506066D1

    公开(公告)日：1999-07-08

    申请号：DE59506066

    申请日：1995-03-02

    Applicant: BASF AG

    Inventor： WITZEL TOM DR ,  FUCHS EBERHARD DR ,  ZIMMERMANN HORST DR

    IPC: B01J23/44 ,  B01J23/58 ,  B01J23/63 ,  C07B61/00 ,  C07C209/48 ,  C07C209/60 ,  C07C211/09 ,  C07C213/02 ,  C07C215/08 ,  C08G18/18 ,  C08G59/68

    Abstract: Prodn. of tert. amines of formula AXCH2NR1R2 (I) comprises reacting nitriles of formula AXCN (II) with sec. amines of formula HNR1R2 (III) and H2 at 50-250 degrees C and 5-350 bar in the presence of a catalyst comprising Pd on an oxide support: R1 and R2 = 1-200C alkyl, 3-8C cycloalkyl, 4-20C alkylcycloalkyl, 4-20C cycloalkylalkyl, 2-20C alkoxyalkyl, aryl, 7-20C alkaryl, 7-20C aralkyl, 2-8C hydroxyalkyl, 2-8C mercaptoalkyl, 8-20C phenoxyalkyl, 2-8C aminoalkyl, R4NH(2-8C)alkyl or R4R5N(2-8C)alkyl, or R1 + R2 = satd. or unsatd. 2-6C alkylene, opt. substd. by up to three 1-4C alkyl gps. and opt. interrupted by O or N; X = 4-8C cycloalkylene or 2-20C alkenylene or 2-20C alkylene opt. substd. by 1-5 of R3, 1-8C alkyl, 1-8C alkoxy, di(1-8C alkyl)amino, OPh, NPh2 and/or 2-8C alkoxycarbonyl; A = H, 1-20C alkyl, 3-8C cycloalkyl, 4-20C alkylcycloalkyl, 4-20C cycloalkylalkyl, 2-20C alkoxyalkyl, aryl, 7-20C alkaryl, 7-20C aralkyl, 1-20C alkoxy, OH, 1-20C hydroxyalkyl, NH2, 1-20C alkylamino, 2-20C dialkylamino, 3-12C alkenylamino, 3-8C cycloalkylamino, arylamino, aryl(1-8C)alkylamino, halogen, SH, 2-20C alkenyloxy, 3-8C cycloalkoxy or aryloxy; R3 = CH2NR1R2; R4 and R5 = 1-20C alkyl.

    CONTINUOUS PURIFICATION PROCESS OF RAW CAPROLACTAM BEING PREPARED FROM 6-AMINOCAPRONITRILE
    28.
    发明专利
    CONTINUOUS PURIFICATION PROCESS OF RAW CAPROLACTAM BEING PREPARED FROM 6-AMINOCAPRONITRILE 未知

    公开(公告)号：CZ197297A3

    公开(公告)日：1998-03-18

    申请号：CZ197297

    申请日：1995-12-22

    Applicant: BASF AG

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

    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.

    29.
    发明专利
    未知

    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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