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    Production of lactams by rearrangement of cyclic ketoximes
    13.
    发明专利
    Production of lactams by rearrangement of cyclic ketoximes 未知

    公开(公告)号：GB1048074A

    公开(公告)日：1966-11-09

    申请号：GB2905463

    申请日：1963-07-23

    Applicant: BASF AG

    Inventor： IRNICH RUDOLF

    IPC: C07D201/04

    Abstract: A lactam is produced by treating a solid cycloalkanone oxime at 210-450 DEG C. with an acid catalyst in a fluidized bed, the oxime being a solid and being introduced in a current of inert gas. Cycloalkanone oximes specified have 5-12 carbon atoms, e.g. cyclopentanone, cyclohexanone, methylcyclopentanone, methylcyclohexanone, cyclooctanone and cyclodecanone oximes. The reaction pressure may be atmospheric or above or below atmospheric. The catalyst, e.g. phosphoric acid, boric acid, or a Li, Na or K hydrogen sulphate may be mixed with a solid carrier, e.g. an oxide of an element in the 3rd or 4th group of the periodic table, e.g. Al, Si, Sn or Ti or pumice, activated charcoal or ZnO. The catalyst and carrier may be mixed with water, extruded into rods or pellets, dried at 120 DEG C. and further heated to 400-800 DEG C. The catalyst carrier ratio may vary from 1: 0.25 to 1:100. Inert gases specified are N2, CO2 and argon. 2-3 1. may be required per gram ketoxime. The catalyst and oxime may be supplied through a single metering device. The heat liberated during the reaction is sufficient to evaporate the oxime and the reaction zone may in fact be cooled. The volatile reaction products may be passed through a cyclone to separate out catalyst particles. The majority of lactam may then be condensed at 60-80 DEG C. the remainder being washed out with water. The uncondensed gases may be returned to the fluidized bed. The product may be purified by distillation under reduced pressure optionally with the addition of oleum, treatment with KMnO4, filtration and redistillation. In Example (1) the catalyst is boric oxide. In Example (2) the catalyst is used boric oxide recycled from Example 1.

    17.
    发明专利
    未知

    公开(公告)号：NO149470C

    公开(公告)日：1984-04-25

    申请号：NO794080

    申请日：1979-12-13

    Applicant: BASF AG

    Inventor： BOTT KASPAR ,  KAIBEL GERD ,  HOFFMANN HERWIG ,  KRATZER OTTO ,  IRNICH RUDOLF

    IPC: C07C51/00 ,  C07C51/09 ,  C07C53/02 ,  C07C51/44 ,  C07C51/48 ,  C07C67/00 ,  C07C27/02

    Abstract: A process for the production of anhydrous or substantially anhydrous formic acid by hydrolysis of methyl formate which is carried out in a column having an upper fractionating section, a middle hydrolysis section and a lower extraction section and in which (a) the hydrolysis is carried out in the middle section of the columm, with water and methyl formate in countercurrent, (b) the resulting formic acid is extracted, in the lower section of the column, by means of a carboxylic acid amide which is fed into the lower end of the middle section of the column, (c) the extract phase, consisting in the main of formic acid and the carboxylic acid amide, is distillatively dehydrated, or substantially dehydrated, in the lower section of the column, (d) the methanol and uncovered methyl formate are removed by fractional distillation in the upper section of the column and (e) the pure formic acid or concentrated aqueous formic acid is distilled from the anhydrous or substantially anhydrous extract phase in a second column, leaving the carboxylic acid amide.

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