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公开(公告)号:JPS62185067A
公开(公告)日:1987-08-13
申请号:JP1633487
申请日:1987-01-28
Applicant: BASF AG
Inventor: HUTMACHER HANS-MARTIN , MERGER FRANZ , BROECKER FRANZ J , FISCHER ROLF , VAGT UWE , HARDER WOLFGANG , PRIESTER CLAUS-ULRICH
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公开(公告)号:JPS62178565A
公开(公告)日:1987-08-05
申请号:JP1015987
申请日:1987-01-21
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
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公开(公告)号:DE3780318D1
公开(公告)日:1992-08-20
申请号:DE3780318
申请日:1987-01-23
Applicant: BASF AG
Inventor: HUTMACHER HANS-MARTIN , BROECKER FRANZ JOSEF DR , MERGER FRANZ DR , FISCHER ROLF DR , VAGT UWE DR , SCHNEIDER HEINZ-WALTER DR , RICHTER WOLFGANG DR , HARDER WOLFGANG DR , PRIESTER CLAUS-ULRICH DR
IPC: C07B61/00 , B01J21/16 , B01J23/00 , B01J23/74 , B01J23/755 , B01J25/02 , C07C67/00 , C07C227/00 , C07C227/04 , C07C227/08 , C07C229/04 , C07C229/08
Abstract: Esters of 6-aminocaproic acid are prepd. by reacting esters of 5-formyl-valeric acid with NH3 and H2, with alcohols as solvents, in presence of hydrogenation catalysts under increased pressure and at 40-95 deg. C. Pref. the catalyst is (i) prepd. by calcination of: ((MgaNi(II)bCo(II)cAl2)CO3(OH)16.4H2O at 200-600 deg. C, followed by redn. with H2 at raised temp., or (ii) 30-60 wt.% of finely divided Ni pptd. on Mg silicate. In the formulae, a = 0-4; b, c = 0-6; 2 x (a+b+c) = 12. Pref. alkanol solns. of 5-formyl valeric acid esters are led with NH3 over a fixed bed catalyst. Raney Ni or Raney Co may be used in a suspension process, opt. fixed in the reaction zone (electro)-magnetically. The catalyst is 0.2-2 kg of 5-formylvaleric acid ester/l of catalyst/h. Partic. methyl 5-formylvalerate is used, in soln. in methanol.
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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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公开(公告)号:DE3602376A1
公开(公告)日:1987-07-30
申请号:DE3602376
申请日:1986-01-28
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
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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
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.
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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.
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公开(公告)号:CA1274827A
公开(公告)日:1990-10-02
申请号:CA527730
申请日:1987-01-20
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 , C07D223/10
Abstract: Caprolactam is prepared by a process in which a) the 5-formylvalerate is reacted with excess ammonia and hydrogen in the presence of an alkanol as the solvent and in the presence of a hydrogenation catalyst under superatmospheric pressure in the liquid phase at from 40 to 130.degree.C, b) excess ammonia and hydrogen are separated off from the reaction mixture, c) the resulting reaction mixture is reacted with water at elevated temperatures with simultaneous removal of alkanols, and d) the reaction mixture thus obtained is heated to 150-370.degree.C and .epsilon.-caprolactam is obtained.
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公开(公告)号:CA1274826A
公开(公告)日:1990-10-02
申请号:CA527726
申请日:1987-01-20
Applicant: BASF AG
Inventor: HUTMACHER HANS-MARTIN , MERGER FRANZ , BROECKER FRANZ J , 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 , C07D223/10
Abstract: Caprolactam is prepared by a process in which a) a 5-formylvalerate is reacted with excess ammonia and hydrogen in the presence of an alkanol as a solvent and in the presence of a hydrogenation catalyst under superatmospheric pressure in the liquid phase at from 40 to 130.degree.C, b) excess ammonia and hydrogen are separated off from the reaction mixture and c) the reaction mixture thus obtained is heated to 150 250.degree.C and .epsilon.-caprolactam is obtained.
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公开(公告)号:DE3602375A1
公开(公告)日:1987-07-30
申请号:DE3602375
申请日:1986-01-28
Applicant: BASF AG
Inventor: HUTMACHER HANS-MARTIN , MERGER FRANZ , BROECKER FRANZ J , FISCHER ROLF , VAGT UWE , HARDER WOLFGANG , PRIESTER CLAUS-ULRICH
Abstract: Caprolactam is prepared by a process in which (a) the 5-formylvalerate is reacted with excess ammonia and hydrogen in the presence of an alkanol as the solvent and in the presence of a hydrogenation catalyst under superatmospheric pressure in the liquid phase at from 40 DEG to 130 DEG C., (b) excess ammonia and hydrogen are separated off from the reaction mixture, (c) the resulting reaction mixture is reacted with water at elevated temperatures with simultaneous removal of alkanols, and (d) the reaction mixture thus obtained is heated to 150 DEG -370 DEG C. and epsilon -caprolactam is obtained.
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