Production of diaminodicyclohexylalkanes or ethers
    4.
    发明授权
    Production of diaminodicyclohexylalkanes or ethers 失效
    生产DIAMINODICYCLOHEXYLALKANES或其他物质

    公开(公告)号:US3634512A

    公开(公告)日:1972-01-11

    申请号:US3634512D

    申请日:1968-12-02

    Applicant: BASF AG

    CPC classification number: B01J37/00 B01J23/70 B01J37/0009 B01J37/0201

    Abstract: PRODUCTION OF DIAMINODICYCLOHEXYLALKANES OR ETHERS BY HYDROGENATION OF DIAMINODIPHENYLALKANES OR ETHERS AT ELEVATED TEMPERATURE AND SUPERATOMSPHERIC PRESSURE IN THE PRESENCE OF A SUPPORTED CATALYST CONTAINING COBALT OR NICKEL WHICH HAS BEEN PREPARED BY TREATING THE CARRIER MATERIAL (AND/OR THE FINISHED CATALYST) WITH A BASIC REACTING ALKALI METAL OR ALKALINE EARTH METAL COMPOUND AND THEN WITH A BINDER, APPLYING FINELY DIVIDED COBALT OXIDE OR NICKEL OXIDE OR FINELY DIVIDED COMPOUNDS OF COBALT OR NICKEL WHICH CHANGE INTO THE OXIDES WHEN HEATED, AND THEN DRYING AND HEATING IT TO 500* TO 1100*C.

    Production of n,n-secondary dialkyl aryldiamines

    公开(公告)号:GB950151A

    公开(公告)日:1964-02-19

    申请号:GB1898862

    申请日:1962-05-17

    Applicant: BASF AG

    Abstract: N-N1-secondary dialkylaryl diamines are prepared in a continuous process by treating aryl diamines with secondary alkanols at above 150 DEG C. in the liquid phase and at a raised pressure in the presence of a catalyst containing nickel and (or) cobalt and in the presence or absence of hydrogen or other inert gas. Specified aryl diamines are o, m- and p-phenylene diamine and 1, 4- and 1,5-diaminonaphthalene. Specified secondary alcohols are isopropanol, 2-octanol and secondary butyl and amyl alcohols. The process may be combined directly with the preparation of the diamino aryl compound by hydrogenation of the corresponding dinitro or nitroamino compound, the alcohol required for the alkylation process being used as a solvent in the reduction process. The catalyst may be Raney nickel or Raney cobalt and may be used as such or in association with copper and (or) manganese as promoters. Addition to the catalyst of up to 4% of alkali compounds (calculated as oxides), e.g. alkali hydroxides, carbonates or silicates, is advantageous. The catalyst may be used in granulated, tableted or pelleted form and may be deposited on inert carriers. A number of carriers are specified. In the examples, (1) a solution of p-phenylene diamine in secondary butyl alcohol is passed at 160-180 DEG C. under 14 atm. pressure through a column charged with a granulated catalyst consisting of nickel 15, copper 5 and manganese 1% supported on pumice; N, N1-di-sec.-butyl-p-phenylene diamine is obtained; (2) a solution of p-nitraniline in secondary butyl alcohol is fed to a first reaction vessel together with hydrogen at 160-180 DEG C. and 14 atm. pressure, the vessel containing a catalyst comprising 20% of copper on silica pellets; the product, after release of gas, is passed to a second reaction vessel under the same temperature and pressure, the second vessel containing a nickel catalyst, as described in example 1; N,N1-di-sec.-butyl-p-phenylene is again obtained with some N-mono-sec.-butyl-p-phenylene diamine; (3) a solution of p-nitraniline in secondary butyl alcohol is fed with hydrogen under 14 atm. pressure to a column charged with a catalyst as described in example 1; reduction of p-nitraniline to p-phenylene diamine takes place at 160 DEG C. in the upper part of the column and alkylation of the p-phenylene diamine at 170-180 DEG C. proceeds in the lower part.ALSO:Catalysts for use in the continuous production of diamines comprise nickel and/or cobalt which may be Raney nickel or Raney cobalt and may be used as such or in association with copper and/or manganese as promoters. Addition to the catalyst of up to 4% of alkali compounds (calculated as oxides), e.g. alkali hydroxides, carbonates or silicates, is advantageous. The catalyst may be used in granulated, tableted or pelleted form and may be deposited on inert carriers. Specified carriers are diatomaceous earth, clay, kaolin, bleaching earths, pumice, bauxites, silica gel, aluminium oxide, zinc oxide, thorium oxide, mixtures of these oxides, and "Bayer mass", a product obtained in the production of aluminium oxide and having the approximate composition ferric oxide 40-50, aluminium oxide 17-25, silica 2-10, titanium dioxide 3-8, alkaline-earth oxides 0,2-4 and alkali-metal oxides 2-5% by weight, the balance being water. In the examples, (1) a solution of p-phenylene diamine in secondary butyl alcohol is passed at 160-180 DEG C. under 14 atm. pressure through a column charged with a granulated catalyst consisting of nickel 15, copper 5 and manganese 1% supported on pumice; N,N1-di-sec.-butyl-p-phenylene diamine is obtained; (2) a solution of p-nitraniline in secondary butyl alcohol is fed to a first reaction vessel together with hydogen at 160-180 DEG C. and 14 atm. pressure, the vessel containing a catalyst comprising 20% of copper on silica pellets; the product, after release of gas, is passed to a second reaction vessel under the same temperature and pressure, the second vessel containing a nickel catalyst, as described in example 1; N,N1-di-sec.-butyl-p-phenylene diamine is again obtained, with some N-mono-sec.-butyl-p-phenylene diamine; (3) a solution of p-nitraniline in secondary butyl alcohol is fed with hydrogen under 14 atm. pressure to a column charged with a catalyst as described in example 1; reduction of p-nitraniline to p-phenylene diamine takes place at 160 DEG C. in the upper part of the column and alkylation of the p-phenylene diamine at 170-180 DEG C. proceeds in the lower part.

    Process for the production of pure cyclohexanone

    公开(公告)号:GB914425A

    公开(公告)日:1963-01-02

    申请号:GB4421960

    申请日:1960-12-23

    Applicant: BASF AG

    Abstract: Cyclohexanone is obtained from crude cyclohexanol by evaporating the bulk of the latter in a first vaporization zone at 140-180 DEG C., supplying the liquid residue to a second vaporization zone wherein it is vaporized as far as possible by a suitably correlated adjustment of temperature and pressure, returning the vapours from the second to the first zone (alternatively having condensed the vapours to liquid and returning this to the first zone), the vapours preheated to 250-400 DEG C. being then passed over a dehydrogenation catalyst at a velocity of 50-100 cm./sec., the residence period at the catalyst being 4-12 seconds. The catalyst is a heavy metal of Group Ib, IIb, VIa or VIII or an oxide or carbonate or mixtures thereof; copper supported on pumice or ferric oxide is specified.

Patent Agency Ranking