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    63.
    发明专利
    未知

    公开(公告)号：FR1415121A

    公开(公告)日：1965-10-22

    申请号：FR994986

    申请日：1964-11-14

    Applicant: BASF AG

    Inventor： BEER LUDWIG ,  BRUNNMUELLER FRIEDRICH ,  METZGER HORST

    IPC: C07C233/09

    Abstract: Contaminated solid acrylamide is purified by dissolving same in a C1- 5 aliphatic alcohol, optionally in the presence of polymerization inhibitors, separating the solution from the insoluble portion, and isolating solid acrylamide from the solution by lowering the temperature.

    Separation of cycloalkanone oximes
    67.
    发明专利
    Separation of cycloalkanone oximes 未知

    公开(公告)号：GB977812A

    公开(公告)日：1964-12-16

    申请号：GB4319662

    申请日：1962-11-15

    Applicant: BASF AG

    Inventor： METZGER HORST ,  WEISER DIETER

    Abstract: A cycloalkanone oxime hydrochloride is separated from a reaction mixture formed by the action of nitrosyl chloride, or of nitric oxide and chlorine, on a cycloalkane under the influence of light by removing the reaction mixture from the reaction zone in which the photochemical reaction takes place into an extraction zone in which a photochemical reaction is not taking place, adding to this latter zone phosphoric acid of 70 to 90% strength, sulphuric acid of 80% to 100% strength or oleum with a content of up to 10% of free sulphur trioxide, mixing the concentrated acid with the reaction mixture at a temperature below 70 DEG C., separating the two phases formed, recycling the organic phase in the reaction zone in which the photochemical reaction takes place, and removing the acid solution which contains the extracted cycloalkanone oxime as such or in the form of its salt with the extraction acid used. The photonitrosation reaction used to produce the reaction mixtures containing the cycloalkanone oxime hydrochlorides may be carried out in an inert solvent at -30 DEG to +40 DEG C. under a pressure of from 1 to 10 atmospheres using light having an effective wavelength of 300 to 500 millimicrons, and in the presence of added hydrogen chloride. Cycloalkanes which can be used in this process include those having 5 to 12 ring carbon atoms which may contain 1 or 2 alkyl side chains having 1 to 5 carbon atoms, e.g. cyclopentane, cyclohexane, cycloheptane, cyclooctane, cyclodecane, cyclododecane, methyl cyclopentane, methyl cyclohexane and ethyl cyclohexane; the cycloalkane may also contain an attached aromatic ring as in tetrahydronaphthalene or an attached cycloaliphatic ring as in decahydronaphthalene. The extraction may be carried out with both the extraction acid and the reaction mixture as stationary phases, stirring being used to promote diffusion of the oxime hydrochloride into the extraction acid, or one of the components may be arranged as a stationary phase and the other component passed over the surface of the stationary phase or through it. In the latter procedure when the acid is the stationary phase, part of the acid containing the oxime may be continually removed and replaced by fresh extraction acid. It is also possible to contact the two components with each other in concurrent or countercurrent manner by stirring and/or distribution over suitable baffle or packing means, plates or other flow interrupters. The solutions of cycloalkanone oxime or its salt in the extraction acid used may be subjected directly to the Beckmann rearrangement to form an o -amino fatty acid lactam by heating the solution at 100 to 150 DEG C. and then pouring the solution on to an amount of water equivalent to at least the weight of extraction acid. In examples, caprolactam, caprylolactam and laurolactam are prepared by this method. Specifications 788,436, 789,732, 873,257 and U.S.A. Specifications 2,719,116 and 2,818,310 are referred to.

    Process for the purification of lactams
    68.
    发明专利
    Process for the purification of lactams 未知

    公开(公告)号：GB969993A

    公开(公告)日：1964-09-16

    申请号：GB3649062

    申请日：1962-09-26

    Applicant: BASF AG

    Inventor： WEISER DIETER ,  METZGER HORST

    Abstract: Lactams containing 4-12 carbon atoms are purified by treatment with activated hydrogen in the presence of acids at a pH of 3 to 0.5, the lactam being in the liquid phase, preferably dissolved in water or in an inert solvent. The acids may be mineral or organic acids having a pH of 4.9 or less, e.g., sulphuric, hydrochloric, formic or acetic, and are used in amounts of 0.01-10.0%, preferably 0.1-10.0%, by weight of lactam. The activated hydrogen may be in the form of nascent hydrogen or catalytically activated hydrogen. In the former instance, nascent hydrogen is generated in the reaction mixture by a process which takes place in an acid medium but under conditions which leave the lactams unattacked, e.g. sodium borohydride and zinc dust and acids, preferably in the presence of an hydrogenation catalyst. Sufficient reagent to provide 0.001-0.5, particularly 0.001-0.2, moles of hydrogen per mole of lactam is employed. The treatment may be carried out in 20-80% by weight solutions in the temperature range -15-250 DEG C., preferably 50-100 DEG C. and at pressures ranging from normal to 10 atmospheres for times of up to 5 hours. When catalytically activated hydrogen is employed the catalyst, generally 0.1-5% by weight of lactam, may be, e.g. palladium, platinum, nickel or noble metal oxides and may be supported on a carrier. Pressures of 1-300 atmospheres may be used at temperatures in the range -15-250 DEG C., particularly 0-120 DEG C., and treatment continued until hydrogen uptake ceases or falls off. Where necessary the lactam is isolated by neutralization and/or filtration and distillation or sublimation. Lactams purified by the present process give polymers of improved colour rating, permanganate number and volatile base number (see Division C3). Examples (1)-(12) describe the treatment of caprolactam with catalytically activated hydrogen and nascent hydrogen. In Example (B) pyrrolidone is treated with catalytically activated hydrogen. Specification 904,302 is referred to.ALSO:Polyamides are made from lactams containing 4-12 carbon atoms which have been purified by treatment in the liquid-phase, preferably dissolved in water or in an inert solvent, and in an acid medium at pH 3-0.5 with activated hydrogen. The hydrogen can be in the nascent state or catalytically activated using the usual hydrogenation catalysts. In examples caprolactam and pyrrolidene are purified and polymerized by heating with 3% hexamethylene-diammonium adipate under an atmosphere of N2 for 6 hours at 260-270 DEG C. The polymers have colour ratings on the Hagen scale of 40-80. Specification 904,302 is referred to.

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