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    4.
    发明专利
    未知

    公开(公告)号：DE3775235D1

    公开(公告)日：1992-01-30

    申请号：DE3775235

    申请日：1987-01-24

    Applicant: BASF AG

    Inventor： HUTMACHER HANS-MARTIN ,  MERGER FRANZ ,  BROECKER FRANZ J ,  FISCHER ROLF ,  VAGT UWE ,  HARDER WOLFGANG ,  PRIESTER CLAUS-ULRICH

    IPC: B01J23/00 ,  B01J23/74 ,  B01J23/78 ,  B01J25/00 ,  C07B61/00 ,  C07D201/08

    Abstract: (i) 5-formyl-valeric acid ester is reacted with excess NH3 and H2 in alkanols as solvents, in the presence of hydrogenation catalysts, under increased pressure, at 40-130 deg.C. (ii) NH3 and H2 are removed from the reaction mixt. obtd. (iii) The reaction mixt. is reacted with water, with heating, esp. at 80-150 deg. C, with the simultaneous sepn. of the alkanols. (iv) The reaction mixt. obtd. is heated to 150-370 deg.C and epsilon-caprolactam is recovered. (A) Prefd. catalysts are prepd. by calcining cpds. having formula (I): ((MgaNi(II)bCo(II)c)Al2)CO3(OH)16x 4 H2O (I) a = integer or decimal no. 0-4; b,c = integer or decimal nos. 0-6; provided that 2 x (a + b + c) = 12, at 200-600 deg.C, and subsequent redn. with H2 at higher temp., e.g. 350-400 deg.C (B) Ni catalysts can also be used contg. 30-60 wt.% finely-divided Ni pptd. on Mg silicate. (C) Raney-Ni or Raney-Co can be used as catalyst for working in a suspension process. (D) The Raney-Ni or Raney-Co catalyst can be fixed magnetically or electro-magnetically in the reaction zone.

    PREPARATION OF CAPROLACTAM
    5.
    发明专利
    PREPARATION OF CAPROLACTAM 未知

    公开(公告)号：CA1272718A

    公开(公告)日：1990-08-14

    申请号：CA527729

    申请日：1987-01-20

    Applicant: BASF AG

    Inventor： VAGT UWE ,  FISCHER ROLF ,  MERGER FRANZ ,  HUTMACHER HANS-MARTIN

    IPC: C07D223/04 ,  C07D201/08 ,  C07D223/10

    Abstract: .epsilon.-caprolactam is prepared by a process in which a) a 5-formylvalerate is reacted with water in the presence of an acidic agewnt at from 30 to 200.degree.C, b) the 5-formylvaleric acid thus obtained is reacted with excess ammonia and hydrogen in the presence of a hydrogenation catalyst and of a solvent which is inert under the reaction conditions, at from 50 to 150.degree.C under superatmospheric pressure, and c) after the ammonia has been separated off, the resulting solution of 6-aminocaproic acid is heated to 150370.degree.C and the caprolactam formed is isolated.

    7.
    发明专利
    未知

    公开(公告)号：DE3775080D1

    公开(公告)日：1992-01-23

    申请号：DE3775080

    申请日：1987-01-23

    Applicant: BASF AG

    Inventor： HUTMACHER HANS-MARTIN ,  MERGER FRANZ ,  BROECKER FRANZ JOSEF ,  FISCHER ROLF ,  VAGT UWE ,  HARDER WOLFGANG ,  PRIESTER CLAUS-ULRICH ,  SCHNEIDER HEINZ-WALTER ,  RICHTER WOLFGANG

    IPC: B01J23/74 ,  B01J23/78 ,  B01J25/00 ,  C07B61/00 ,  C07D201/08

    Abstract: (i) 5-formyl-valeric acid ester is reacted with excess NH3 and H2, using alkanols as solvents, in the presence of hydrogenation catalysts, at 40-130 deg.C. (ii) NH3 and H2 are removed from the reaction mixt. obtd. (iii) The reaction mixt. is heated to 150-250 deg.C and caprolactam is recovered. (A) Catalysts are used which are prepd. by calcining cpds. having formula (I): ((MgaNi(II)bCo(II)c)Al2)CO3(OH)16 x 4 H2O (I) a = integer or decimal no. 0-4; b,c = integers or decimal nos. 0-6; provided that 2 x (a + b + c) = 2. at 200-600 deg.C and subsequent redn. with H2 at higher temp. (B) Ni catalysts can also be used contg. 30-60 wt.% finely-divided Ni pptd. on Mg silicate. (C) Raney-Ni or Raney-Co catalysts can be used in a suspension process. (D) The Raney-Ni or Raney-Co catalyst can be fixed magnetically or electro-magnetically in the reaction-zone.

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