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    Purification of aliphatic dinitriles
    42.
    发明专利
    Purification of aliphatic dinitriles 未知

    公开(公告)号：GB917788A

    公开(公告)日：1963-02-06

    申请号：GB4241260

    申请日：1960-12-09

    Applicant: BASF AG

    Inventor： ADAM KARL ,  AREND WOLFGANG ,  FRICK REINHOLD ,  HAAS HANS

    Abstract: Aliphatic dinitriles containing from 4 to 22 carbon atoms and having at least two carbon atoms between the nitrile groups are purified by heating with water and a neutral salt of ammonia or an amine. A suitable temperature range is 50 DEG to 200 DEG C. The water is preferably present in an amount which is 1 to 20% by weight of the dinitrile, and the neutral salt is preferably present in an amount which is 0.01 to 10% by weight of the dinitrile. Dinitriles exemplified are adipodinitrile, suberodinitrile, sebacodinitrile and mixtures of 1,9- and 1,10-dicyanoheptadecanes. After heating, the mixture of dinitrile, neutral salt and water may be subjected to distillation. The process may be adapted to both continuous and discontinuous operation.

    43.
    发明专利
    未知

    公开(公告)号：FR1272896A

    公开(公告)日：1961-09-29

    申请号：FR843174

    申请日：1960-11-07

    Applicant: BASF AG

    Inventor： ADAM KARL ,  AREND WOLFGANG ,  FRICK REINHOLD ,  HAAS HANS

    IPC: C07C253/34 ,  C07C255/45

    Abstract: Aliphatic dinitriles containing 4-22 carbon atoms, having at least 2 carbon atoms between the nitrile groups, and having, apart from the nitrile groups, a hydrocarbon structure, are purified by bringing them in the presence of water into contact with an alkali metal bisulphate, ammonium bisulphate, an ammonium bisulphate N-substituted by 1-3 alkyl groups having 1-4 carbon atoms, or a bisulphate of a divalent metal which does not form a sulphate which is difficulty soluble in water, e.g. iron, manganese, zinc, cobalt and nickel. The amount of water is preferably 3-8% by weight of dinitrile, and the amount of bisulphate preferably 0.01-10% by weight of dinitrile. Specified dinitriles are adipodinitrile, suberodinitrile, sebacodinitrile and the mixture of 1.9- and 1,10-dicyanoheptadecane known as heptadecane dicarboxylic acid dinitrile. The temperature may be from the solidification point of the dinitrile to 200 DEG C. or more. The purified dinitriles may be reduced to the corresponding diamines.

    Cobalt-containing hydrogenation catalysts and the production of the same
    44.
    发明专利
    Cobalt-containing hydrogenation catalysts and the production of the same 未知

    公开(公告)号：GB874861A

    公开(公告)日：1961-08-10

    申请号：GB3059359

    申请日：1959-09-08

    Applicant: BASF AG

    Inventor： ADAM KARL

    IPC: B01J21/00 ,  B01J23/84 ,  B01J27/00 ,  B01J27/186 ,  B01J27/188 ,  C07C209/48

    Abstract: A hydrogenation catalyst containing 5-30 (preferably 10-20) % wt. Co oxide, less than 6% wt. Cr oxide (preferably 0.03-5% wt. thereof) and/or Mn oxide (preferably 0.01-2% wt. thereof) and 0.05-5 (preferably 0.3-1.5% wt.) of phosphoric, boric or sulphuric acid in the pyro or poly acid form, applied to more than 59% (preferably 71.5% or more) of a carrier, is prepared by treating the catalyst ingredients with such acid and heating to a temperature at which conversion to the pyro or poly form is effected; thus, using phosphoric acid, the catalyst may be heated to 500-650 DEG C. Alternatively, a carrier need not be used, in which case the other catalyst ingredients are used in the same relative proportions. Specified carriers are fullers earth, silicic acid strings, silica gel, aluminium oxide and silicates, e.g magnesium silicate. The catalysts are particularly suitable for conversion of aliphatic nitriles (including dinitriles) to the corresponding amines (or diamines); examples are given of the hydrogenation in liquid ammonia of adiponitrile to hexamethylenediamine, and the hydrogenation of suberonitrile to octamethylenediamine is also mentioned.ALSO:A hydrogenation catalyst containing 5-30% (preferably 10-20%) wt. Co oxide, less than 6% wt. Cr oxide (preferably 0.03-5% wt. thereof) and/or Mn oxide (preferably 0.01-2% wt. thereof) and 0.05-5% (preferably 0.3-1.5% wt.) of phosphoric, boric or sulphuric acid in the pyro or poly acid form, applied to more than 59% (preferably 71.5% or more) of a carrier, is prepared by treating the catalyst ingredients with such acid and heating to a temperature at which conversion to the pyro or poly form is effected; thus, using phosphoric acid, the catalyst may be heated to 500-650 DEG C. Alternatively, a carrier need not be used, in which case the other catalyst ingredients are used in the same relative proportions. Specified carriers are fuller's earth, silicic acid strings, silica gel, aluminium oxide and silicates, e.g. magnesium silicate. The catalysts are particularly suitable for conversion of nitriles (including dinitriles) to the corresponding amines (or diamines).

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