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    PRODUCTION OF MODIFIED POLYALKYLENE TEREPHTHALATES
    14.
    发明专利
    PRODUCTION OF MODIFIED POLYALKYLENE TEREPHTHALATES 未知

    公开(公告)号：CA1050693A

    公开(公告)日：1979-03-13

    申请号：CA204585

    申请日：1974-07-11

    Applicant: BASF AG

    Inventor： STREHLER HUGO ,  BEER LUDWIG ,  KUNDE JOACHIM ,  MATTHIES HANS G ,  POHLEMANN HEINZ

    IPC: C08G63/00 ,  C08G63/181 ,  C08G63/183 ,  C08G63/78 ,  C08G63/18 ,  C08G63/22

    Abstract: A process for the production of a modified polyalkylene terephthalate from the radical of terephthalic acid and the radical of a glycol of two to six carbon atoms in which from 1 to 50 mole % of the terephthalic acid radical has been replaced by an aliphatic dicarboxylic acid radical of four to twelve carbon atoms. The aliphatic dicarboxylic acid is esterified by heating with the glycol in a molar ratio of from 1:1.2 to 1:1.8 at a temperature of from about 5 to 20.degree.C below the boiling point of the glycol until the degree of esterification is from 90 to 95 mole % based on the aliphatic dicarboxylic acid; a dialkyl terephthalate is transesterified with the glycol in a molar ratio of from 1:1.2 to 1:2 in the presence of a catalyst in an amount of from 0.01 to 0.2% by weight base on dialkyl-terephthalate by heating to a temperature of from 130.degree. to 240.degree.C at atmospheric pressure until at least 95% of the alkoxy groups present have been eliminated. The esterification product is mixed with the transesterification product and polycondensation is carried out at a temperature of from 240.degree. to 290.degree.C and a pressure of from 0.1 to 760 mm, in the presence of a catalyst in an amount of from 0.01 to 0.2% by weight based on the polyester. The polyester obtained is suitable for example for mouldings or as an adhesive.

    CONTINUOUS MANUFACTURE OF POLYESTERS
    15.
    发明专利
    CONTINUOUS MANUFACTURE OF POLYESTERS 未知

    公开(公告)号：CA953448A

    公开(公告)日：1974-08-20

    申请号：CA98379

    申请日：1970-11-17

    Applicant: BASF AG

    Inventor： BEER LUDWIG ,  FISCHER HERMANN ,  HEIL EDUARD

    IPC: C08G63/00 ,  B01J14/00 ,  C08G63/78

    Abstract: 1321115 Polymerisation apparatus BADISCHE ANILIN-& SODA-FABRIK AG 20 Nov 1970 [22 Nov 1969] 55205/70 Heading B1X [Also in Division C3] Apparatus used in the production of linear polyester by a continuous process in which diglycol terephthalate and/or its precondensate are polycondensed, optionally in the presence of other polyester-forming components, at a temperature of 240‹-300‹C at reduced pressure, comprise a bundle of stationary, substantially vertical heated tubes 1 surrounded by heating jacket 2 containing heating medium 3 immediately above which is located at least one hold tank 4, which may be heated, connected to a vacuum at outlet 5, the major portion or all of the heat required to heat the reaction mixture and evaporate the volatile portions thereof being applied to the tubes. Liquid catching surfaces 6 may be provided between tank 4 and vacuum outlet 5. The heating jacket surrounding the bundle of tubes may be divided into two separate zones, the temperature of the heating medium in the upper zone being higher than that in the lower zone. Bottle necks may be provided in the tubes by squeezing them to provide slot-like depressions using a suitable die or by inserting orifice plates or capillaries.

    Purification of lactams
    16.
    发明专利
    Purification of lactams 未知

    公开(公告)号：GB1044018A

    公开(公告)日：1966-09-28

    申请号：GB3030063

    申请日：1963-07-31

    Applicant: BASF AG

    Inventor： BEER LUDWIG ,  METZGER HORST ,  WEISER DIETER

    IPC: C07D201/16

    Abstract: Lactams, produced by rearrangement of oximes derived by irradiating saturated cycloaliphatic hydrocarbons and nitrosyl chloride or a mixture of nitric oxide and chlorine are purified by contact with 0.01-10% of Mg, Al, Cu, Zn, a metal of the iron group, a chloride or carbonate of a Group IIA or IIB element, AlCl3 or an oxide of an element of Group IIIA or IIB or the iron group or of copper and distillation. Rearrangement of the oxime may be effected at 80-150 DEG C. by H3PO4, 80-100% H2SO4, oleum containing up to 10% SO3 or a solid catalyst. The lactams may have 5-12 carbon atoms, e.g. laurolactam, capryllactam, piperidone, oenanthlactam and omega-amino-decanoic acid lactam. They may be liquid or gaseous or dissolved in an inert solvent, e.g. an aliphatic, cyclo-aliphatic or aromatic alcohol. Catalysts specified are Zn amalgam, a Raney metal of the iron group, e.g. Ni, ZnCl2, CaCl2, ZnCO3, MgCO3, oxides of Fe, Zn, Al, Co and Ni and mixtures thereof. The metal may be granular and may be activated, e.g. by treating Zn or Al with I2 or a mercury salt. The purification may take place at 0-250 DEG C. in an inert atmosphere, e.g. H2, and the pressure may be atmospheric or above or below. A polymerization stabilizer, e.g. 2,4,6-tri-tert.-butyl-phenol may be present. The product may be distilled out batchwise or continuously and the mixture may be filtered prior to distillation. In Example (1) laurolactam is treated under an atmosphere of nitrogen with, Zn dust activated with mercuric chloride, nickelous oxide, ferrous oxide, cupric oxide, magnesium activated with iodine, zinc dust, zinc dust aluminium powder and copper powder activated with mercury, iron powder, CaCO3 and BaCl2. In Example (2) Raney nickel and Raney cobalt are used separately in admixture with Zn dust. In Example (5) methanol is used as a solvent. In Example (6) the lactam is capric lactam.ALSO:In Example 1 laurolactam prepared and purified by a particular process (see Division C2) is fused with 3% of hexamethylene diammonium adipate and heated at 270-280 DEG C. under a nitrogen atmosphere of superatmospheric pressure to polymerize it.

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