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    Production of polylaurolactam
    11.
    发明专利
    Production of polylaurolactam 未知

    公开(公告)号：GB1077310A

    公开(公告)日：1967-07-26

    申请号：GB4268164

    申请日：1964-10-20

    Applicant: BASF AG

    Inventor： KUNDE JOACHIM ,  WILHELM HANS ,  METZGER HORST ,  DOERFEL HELMUT

    IPC: C08G69/16

    Abstract: Laurolactam is partially polymerized at 200-340 DEG C. and autogenous pressure in the presence of 10-300 mole per cent of water, the water is removed and the polymerization continued at 270-340 DEG C. Before polymerization the reactants may be freed of oxygen. 0.05-2 mole per cent of a chain terminator, e.g. acetic, propionic, butyric, benzoic or stearic acid or dodecylamine, may be added before or during polymerization. Other additives may be fillers, fibres, pigments and dyes. Both polymerization stages may be conducted under an inert atmosphere. The pressure of the first may be up to 73 atmospheres; that of the second atmospherics sub- or super-atmospheric. The water may be removed by releasing the pressure and heating. The products may be extruded as fibres directly from the bottom of the pressure vessel. They may be injection moulded, extruded, or fluidized bed coated to produce rods, gears, pipe, film, sheeting bristles or fibres.

    Production of cyclododecanone oxime and its hydrochloride
    13.
    发明专利
    Production of cyclododecanone oxime and its hydrochloride 未知

    公开(公告)号：GB978497A

    公开(公告)日：1964-12-23

    申请号：GB3029963

    申请日：1963-07-31

    Applicant: BASF AG

    Inventor： METZGER HORST

    Abstract: Cyclododecanone oxime hydrochloride is made by hydrogenating 2-chlorocyclododecanone-(1)-oxime or a corresponding compound containing one or two olefinic double linkages in the presence of palladium or platinum as a catalyst. The catalyst may be colloidally dispersed or deposited on inert carriers, such as aluminium oxide, active carbon, barium sulphate, calcium sulphate or silicates. Between 0.01 and 5% by weight of platinum or palladium may be used with reference to the starting material. The reaction temperature is preferably between 0 DEG and 130 DEG C. and pressures up to 500 atm. may be used. Inert solvents such as alcohols, ethers, carboxylic acids, esters or hydrocarbons. The process may be batchwise or continuous. On completion of the reaction, the catalyst is filtered off, the solvent is wholly or partly evaporated until the cyclododecanone oxime hydrochloride crystallizes out. The free oxime may be obtained by hydrolysing the hydrochloride with water. In another embodiment, a solvent is used which is immiscible or only slightly miscible with strong acids and the oxime hydrochloride is separated by extraction with such an acid, e.g., 85% phosphoric acid or 80 to 100% sulphuric acid. The starting materials may be made by reaction of cyclododecatriene-(1, 5, 9), cyclododecadiene-1, 5 and/or cyclododecene with nitrosyl chloride in the presence of hydrogen chloride at between -50 DEG C. and +50 DEG C. forming 2-chloro-cyclododecadiene-5, 9- -one-1-oxime, 2 chloro-cyclododecene -5- one -1- oxime and/or 2-chlorocyclododecanone -1- oxime respectively. Instead of nitrosyl chloride, nitrogen monoxide and chlorine, dinitrogen trioxide and hydrogen chloride or nitrosylsulphuric acid and hydrogen chloride may be used. Inert solvents such as chlorohydrocarbons, or aliphatic, cyclo-aliphatic or aromatic hydrocarbon may be used. The a -choroximes need not be isolated but the hydrogen chloride may be expelled by an inert gas before use in the preparation of the cyclododecanone oxime hydrochloride. Detailed examples are given. Specifications 873,257 and 947,396 are referred to.

    Improvements in the production of omega-lauric lactam
    16.
    发明专利
    Improvements in the production of omega-lauric lactam 未知

    公开(公告)号：GB876946A

    公开(公告)日：1961-09-06

    申请号：GB659960

    申请日：1960-02-25

    Applicant: BASF AG

    Inventor： SCHICKH OTTO VON ,  METZGER HORST

    Abstract: o -lauric lactam is obtained by allowing a hydroxylammonium salt to act on cyclododecanone in aqueous sulphuric acid with a sulphuric acid content of more than 70% by weight or fuming sulphuric acid with a sulphur trioxide content of at the most 50% by weight at a temperature between 90 and 150 DEG C., and diluting the rearrangement mixture with such an amount of water and/or ice that the concentration of sulphuric acid in the diluted mixture is at most 60% by weight. Generally the ratio by weight of cyclododecanone to sulphuric acid or oleum will be between 1:0.6 and 1:5, advantageously between 1:06 and 1:2. Hydroxylammonium with strong acids, preferably inorganic, e.g. hydrochloric or, preferably sulphuric are suitable. They are preferably used in at least the stoichiometric amount with respect to cyclododecane and preferably in an excess, e.g. of 1-25%. The process may be operated batchwise or continuously.

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