公开(公告)号：GB1046656A

公开(公告)日：1966-10-26

申请号：GB706964

申请日：1964-02-20

Applicant: BASF AG

Inventor： JOCKERS KURT ,  MEIER HERMANN ,  EBERHARDT ERNST ,  TAGLINGER LUDWIG

IPC: C01B21/14

Abstract: In the preparation of hydroxylammonium salts, in a continuous process by catalytic reduction of No with H2 in contact with Pt catalysts in the presence of dilute inorganic acids, the reduction is carried out in at least two successive stages; fresh acid is supplied at the first stage and hydroxylammonium salt withdrawn from the last stage, the acid concentration decreases from stage to stage. The catalyst may be periodically gassed with NO, a mixture of NO and N2 or a mixture of NO and CO2, in each case in the absence of hydrogen. Reaction temperature may be 40 DEG to 50 DEG C. and the catalyst may have Pt content of 0.3 to 5%. Fig. 3 illustrates a four-stage process for this reaction. E.g. 4 to 5 N H2So4 together with Pt catalyst from the separator S are introduced into reactor I and passed through reactors II, III and IV to the separator S. The normalities of H2SO4 in the zones range from 3.20 to 0.30. No and H2 mixture is passed in parallel through reactors IV, III and II, the off-gas from these reactors is collected and passed through reactor I. After leaving I, remaining off-gas is burnt. Fig. 1 (not shown) illustrates a system in which 8 reactors are arranged in two parallel lines of 4. Fig. 2 (not shown) is a 5-stage system where Stages I and II are fed with off-gas from Stages III, IV and V.

公开(公告)号：GB894751A

公开(公告)日：1962-04-26

申请号：GB922360

申请日：1960-03-16

Applicant: BASF AG

Inventor： SUESSENGUTH HERMANN ,  MEIER HERMANN ,  CORR HUBERT ,  SIMON WALTER

IPC: B01J23/34 ,  B01J23/50 ,  B01J23/70 ,  B01J37/08 ,  B01J37/14 ,  B01J37/18 ,  C07C209/36 ,  C07C209/48 ,  C07C209/72 ,  C07C241/02

Abstract: A process for the hydrogenation of aromatic amino compounds and acyclic and carbocyclic compounds containing nitrogenous groups reducible to amino groups, wherein a hydrogenation of an aromatic ring to give a cycloaliphatic ring and a reduction of a nitrogenous group to give an amino group is achieved, comprises carrying out the hydrogenation in the absence of sulphur at a temperature between 40 DEG C. and 250 DEG C. under a pressure between 20 and 600 atmospheres in the liquid phase in the presence of at least one metal hydrogenation catalyst, the catalytic activity of which is impaired by sulphur, the catalyst having been sintered prior to the hydrogenation. The catalyst may contain, for example, silver, manganese, copper, iron, cobalt or nickel and may be prepared by sintering the oxide at 800 DEG C.-1,400 DEG C. and heating the sintered oxide with hydrogen at 250 DEG C.-600 DEG C. The catalyst may be supported on a carrier and promotors may be added. Aromatic amines may be hydrogenated at 200 DEG C.-250 DEG C. to give cycloaliphatic amines and other nitrogenous compounds containing, for example, nitro, nitroso, isonitroso and cyano groups may be hydrogenated at 60 DEG C.-150 DEG C. to give amino compounds. Other substituents such as aldehyde groups which are reduced and carboxylic, halogen, amino and alkoxy groups which are not reduced may also be present in the reactants. A list of suitable reactants is given. In the examples, ethylene diamine, cyclohexylamine, tolylene diamine, dimethyl hydrazine and isopropylamine are prepared.ALSO:Oxides of silver, manganese, copper, iron, cobalt or nickel are converted to the metal by sintering the oxide by heating for example, to a temperature within 20-60 DEG C. of the melting point and reducing the sintered oxide with a stream of hydrogen. Mixtures of metal oxides may be reduced after sintering to give alloys and in examples alloys of cobalt and aluminium and cobalt, nickel and aluminium are prepared.