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    Production of pure caprolactam
    1.
    发明专利
    Production of pure caprolactam 未知

    公开(公告)号：GB1123805A

    公开(公告)日：1968-08-14

    申请号：GB4581965

    申请日：1965-10-29

    Applicant: BASF AG

    Inventor： PETRI NORBERT ,  STREHLER HUGO

    IPC: C07D201/04

    Abstract: A process for preparing caprolactam by the catalytic rearrangement of cyclohexanone oxime in contact with solid catalysts at elevated temperature and in the presence or absence of an inert gas, is characterized in that the gas mixture leaving the reaction chamber is quenched by liquid caprolactam, and the subsequent condensation of caprolactam is effected in a column equipped with baffles, a low boiling liquid being added at the top of the column. Reaction is conducted at 210-450 DEG C., at a pressure from 10 mm./Hg up to 1 at. gauge. Suitable catalysts are phosphoric or boric acids, heteropolyacids, alkali metal bisulphates, or mixtures thereof; they may be incorporated on a carrier, e.g. alumina (which may be calcined), silica gel or TiO2. Steam is a suitable inert gas. Specified low-boiling liquids are water, C1- 4 alkanols, C3- 5 dialkylketones, C5- 7 alkanes or benzene. The temperature difference between the gas leaving the reaction chamber and the caprolactam should be at least 10 DEG C., and the column should contain sufficient baffles to prevent loss of caprolactam vapour.

    Process for the conversion of cyclic ketoximes
    3.
    发明专利
    Process for the conversion of cyclic ketoximes 未知

    公开(公告)号：GB999851A

    公开(公告)日：1965-07-28

    申请号：GB2076062

    申请日：1962-05-30

    Applicant: BASF AG

    Inventor： HUBER WOLFGANG ,  PETRI NORBERT ,  SCHREINER SIEGFRIED ,  WINTERSBERGER KARL

    IPC: C07D201/04

    Abstract: A process for the production of lactams by the catalytic rearrangement of cycloalkanone oximes in the presence of supported or unsupported solid acidic catalysts at 210 DEG to 450 DEG C. is characterized by contacting the oxime in the liquid state with the heated catalyst. The catalyst may be fluidized by the vaporized oxime and/or an inert gas, e.g. nitrogen or water vapour. Cycloalkanone oximes specified are those containing 5 to 12 carbon atoms, e.g. cyclopentanone oxime, methyl cyclopentanone oxime, cyclohexanone oxime, methylcyclohexanone oxime, cyclo-octanone oxime and cyclododecanone oxime; these may be used in the anhydrous state or may contain up to about 15% wt. of water, i.e. the amount present when the oxime is prepared from a ketone and a hydroxylamine salt. Catalysts specified are phosphoric acid, anhydrous boric acid (i.e. boron oxide), boric acid, or alkali metal hydrogen sulphates, e.g. lithium, sodium or potassium hydrogen sulphates or mixtures thereof. These may be suported on suitable carriers, for example oxides of those elements of Group III and IV of the Periodic Table having an atomic weight greater than 25, e.g. alumina, bayerite, corundum, silica gel, diatomaceous earth, tin dioxide and titanium dioxide; pumice, activated charcoal and zinc oxide may also be used as carriers. The process may be carried out at subatmospheric, atmospheric, or superatmospheric pressures. The product may be purified by distillation under reduced pressure, where necessary with the addition of oleum, followed by treatment with potassium permanganate, filtration, and further distillation. Specific examples relate to the preparation of caprolactam, methylcaprolactam and caprylolactam.

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