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    Continuous production of alkane dicarboxylic acids
    23.
    发明专利
    Continuous production of alkane dicarboxylic acids 未知

    公开(公告)号：GB1092603A

    公开(公告)日：1967-11-29

    申请号：GB1012365

    申请日：1965-03-10

    Applicant: BASF AG

    Inventor： RIEGELBAUER GEORG ,  WEGERICH ANTON ,  KUERZINGER ALFRED ,  HAARER ERICH

    IPC: C07C55/02 ,  C07C51/00 ,  C07C67/00

    Abstract: Alkane dicarboxylic acids are prepared by a continuous process wherein cycloalkanols, cycloalkanones, cycloalkylamines, o - hydroxyalkane carboxylic acids having at least four carbon atoms, lactones of such acids and/or tetrahydrofurane are oxidized by intensely mixing said organic reactant with a large excess of 40 to 70% by weight nitric acid, the reaction is allowed to proceed at atmospheric or superatmospheric pressure and a temperature of 20 DEG to 100 DEG C., after a residence period of less than four minutes the mixture leaving the reaction zone is freed from nitrous oxides, the concentration of nitric acid is restored by evaporation of water to a level which is approximately that of the reaction zone nitric acid concentration, the alkane dicarboxylic acid is separated by a conventional method from a minor portion of the reaction mixture, the mother liquor is united with the remainder of the reaction mixture, fresh nitric acid, if desired, is added to the mixture thus obtained and this mixture is intensely mixed with fresh initial organic material and returned to the reaction zone.

    Tube reactors
    24.
    发明专利
    Tube reactors 未知

    公开(公告)号：GB1004234A

    公开(公告)日：1965-09-15

    申请号：GB4888263

    申请日：1963-12-11

    Applicant: BASF AG

    Inventor： POEHLER GUENTER ,  WEGERICH ANTON ,  GOEHRE OTTO ,  GIEHNE HELLMUT

    IPC: B01J8/06 ,  B01J19/24 ,  C07C45/00

    Abstract: A catalytic dehydrogenation reactor, e.g. for dehydrogenating paraffins and naphthenes comprises a plurality of tubes each having a diameter of at least 70 mm. arranged in a reactor so as to leave a central free space and baffles arranged perpendicularly to the tubes and alternately at the reactor wall and in the central space to deflect a gaseous heating medium which is passed between the tubes in the same direction as reactants are passed through the tubes. The ratio of diameter to length of the tubes may be 12-17 : 1000 with a diameter of 70-120 mm. and a length of 5-12 m. The free space in the centre of the reactor may be 7-25% of the total cross-sectional area. The baffles are alternate central circular baffles occupying 25-60% of the total cross-sectional area extending into the section containing tubes and outer annular baffles occupying 50-75% of the total area. The baffles, particularly in the tubed area, may have perforations, e.g. 3-10 mm. in diameter. The tubes may be spaced 15-60 mm. from each other. Heating medium is preferably introduced by an annular duct 2 surrounding the reactor. The medium is divided into two streams by a baffle 9 which flow in opposite directions round the reactor and enter the reactor through slots which increase in size in the direction of flow. The heating medium is withdrawn by a similar duct 5 and is reheated and re-used. The ducts 2 and 5 may have a cross-sectional area 5-20% that of the reactor.ALSO: A catalytic dehydrogenation reactor e.g. for converting alcohols to ketones comprises a plurality of tubes each having a diameter of at least 70 mm. arranged in a reactor so as to leave a central free space and baffles arranged perpendicularly to the tubes and alternately at the reactor wall and in the central space to deflect a gaseous heating medium which is passed between the tubes in the same direction as reactants are passed through the tubes. The ratio of diameter to length of the tubes may be 12-17 : 1,000 with a diameter of 70-120 mm. and a length of 5-12 cm. The free space in the centre of the reactor may be 7-25% of the total cross sectional area. In Fig. 1 the baffles 4 are alternate central circular baffles occupying 25-60% of the total cross-sectional area extending into the section containing tubes and outer annular baffles occupying 50-75% of the total area. The baffles, particularly in the tubed area, may have perforations, e.g. 3-10 mm. in diameter. The tubes may be spaced 15-60 mm. from each other. Heating medium is preferably introduced by an annular duct 2 surrounding the reactor. The medium is divided into two streams by a baffle 9 which flow in opposite directions round the reactor and enter the reactor through slots which increase in size in the direction of flow. The heating medium is withdrawn by a similar duct 5 and is reheated and reused. The ducts 2 and 5 may have a cross-sectional area 5-20% that of the reactor. In examples cyclohexanol is converted to cyclohexanone and sec.-butanol to methyl ethyl ketone.

    Production of aniline
    26.
    发明专利
    Production of aniline 未知

    公开(公告)号：GB913444A

    公开(公告)日：1962-12-19

    申请号：GB146761

    申请日：1961-01-13

    Applicant: BASF AG

    Inventor： SPERBER HEINRICH ,  POEHLER GUENTER ,  PISTOR HANS JOACHIM ,  WEGERICH ANTON

    IPC: C07C209/36

    Abstract: In a process for the production of aniline, or an amine of an alkyl benzene, by the hydrogenation of nitrobenzene, or an alkylated nitrobenzene e.g. nitrotoluene or nitroxylene, using a metal hydrogenation catalyst in a fluidised layer, preferably provided with cooling means, the nitrobenzene is introduced into the layer at least partly in liquid phase at a plurality of points at least some of which are at different heights. The hydrogen and nitrobenzene are introduced into the reaction zone in a molar ratio of at least 3 : 1. The reaction is preferably carried out at a pressure of 4-25 atmospheres at temperatures between 200 and 400 DEG C. The hydrogen may be introduced with the nitrobenzene e.g. by using a two-component nozzle, or at the bottom of the reaction vessel. The points of introduction of the nitrobenzene are preferably distributed over the lower three-quarters of the fluidised catalyst layer. When a reactor of large crosssectional area is used, several inlets may be provided at the same level. In examples, the hydrogenation is carried out at 275 DEG C. and at 300 DEG C. at 10 atm. using a Cu on alumina catalyst and at 280-290 DEG C. at 5 atm. using Cu with traces of Cr, Ba, and Zn on silicic acid as catalyst. An Ni/Mo catalyst may also be used.

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