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    Continuous fine dispersion of pigments in fiber forming polymers
    11.
    发明专利
    Continuous fine dispersion of pigments in fiber forming polymers 未知

    公开(公告)号：GB1081965A

    公开(公告)日：1967-09-06

    申请号：GB1918266

    申请日：1966-05-02

    Applicant: BASF AG

    Inventor： DORFNER KONRAD ,  LINGE HERMANN ,  SCHAEFER EBERHARD ,  STREHLER HUGO

    IPC: C08G63/78 ,  C08G85/00

    Abstract: Water-insoluble pigments are continuously finely dispersed in fibre-forming polymers by grinding the pigment in a sand mill or bead mill, passing the dye suspension leaving the mill into a mixing unit in which it is mixed with the molten intermediates for the polymer, then passing the mixture into a reactor at 250-300 DEG C. for polymerization or polycondensation. Suitable pigments are TiO2, Fe2O3, MgO, CaCO3, BaSO4 and the phthalocyanines. These are preferably suspended in water, or when for use with polyethylene terephthalate, in glycol. The suspension may contain 7-25 wt. per cent of pigment. Materials to be pigmented may be polyamides and polyesters deriving from e.g. caprolactam, laurolactam, capryllactam or from dimethyl terephthalate and ethylene glycol, or the monomeric transesterification product thereof. The mill may be heated up to 250 DEG C. Suitable apparatus comprises a sand or bead mill with an inlet at the bottom, and an outlet at the top leading to a closed, heatable, cylindrical mixing unit, from which an outlet leads to a polymerization vessel. In examples TiO2 is suspended in water containing sodium metaphosphate or in ethylene glycol containing alumina sol and mixed with caprolactam or an ethylene glycol/dimethyl terephthalate mixture respectively.

    PRODUCTION OF MODIFIED POLYALKYLENE TEREPHTHALATES
    12.
    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the radical of a glycol of two to six carbon atoms in which from 1 to 50 mole % of the terephthalic acid radical has been replaced by an aliphatic dicarboxylic acid radical of four to twelve carbon atoms.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.

    PRODUCTION OF CONCENTRATES OF TITANIUM DIOXIDE IN POLYCAPROLACTAM
    15.
    发明专利
    PRODUCTION OF CONCENTRATES OF TITANIUM DIOXIDE IN POLYCAPROLACTAM 未知

    公开(公告)号：CA1180834A

    公开(公告)日：1985-01-08

    申请号：CA404707

    申请日：1982-06-08

    Applicant: BASF AG

    Inventor： STREHLER HUGO ,  HOERAUF WERNER ,  VALENTIN GUENTER

    IPC: C08J3/22 ,  C08K3/22 ,  C08L77/02 ,  C09D17/00 ,  C08J3/20

    Abstract: The invention relates to a process for the production of a concentrate of from 20 to 50% by weight of titanium dioxide in polycaprolactam, wherein a 5 - 15% strength by weight aqueous suspension of titanium dioxide is metered into a solution of caprolactam in water at from 110 to 150.degree.C at the same rate at which water is distilled off, and after all the water has been distilled off the resulting mixture is polymerized at from 240 to 280.degree.C. This process allows to obtain concentrates of titanium dioxide, which have a long shelf life and a constant concentration, can readily be dispersed in the caprolactam or polycaprolactam melt, and in addition, owing to the omission of water, do not adversely affect the capacity of the polymerization plant.

    Simultaneous recovery of pure ammonium sulphate and pure lactams from rearrangement mixtures of alicyclic ketoximes
    18.
    发明专利
    Simultaneous recovery of pure ammonium sulphate and pure lactams from rearrangement mixtures of alicyclic ketoximes 未知

    公开(公告)号：GB996322A

    公开(公告)日：1965-06-23

    申请号：GB1568962

    申请日：1962-04-25

    Applicant: BASF AG

    Inventor： NIESWANDT WERNER ,  STREHLER HUGO ,  RAPP GUENTHER ,  KAHR KURT

    IPC: C01C1/242 ,  C07D201/16

    Abstract: A process for continuously recovering pure ammonium sulphate in the preparation of lactams (see Division C2) by Beckmann rearrangement of a cycloalkanone oxime having 6 to 10 ring carbon atoms with 98 to 100% wt. sulphuric acid or oleum containing up to 35% wt. of free sulphur trioxide, which reaction mixture contains 30 to 50% wt. lactam, followed by neutralizing said reaction mixture by contact with ammonia in the presence of 5 to 50 times the amount (with reference to the weight of reaction mixture) of 25 to 45% wt. ammonium sulphate solution, comprises separating the resulting lactam and ammonium sulphate phases, evaporating the ammonium sulphate phase until ammonium sulphate has been precipitated in an amount corresponding to the sulphuric acid in the rearrangement mixture, diluting the mother liquor with such an amount of water as is necessary to restore the ammonium sulphate solution to its original concentration, and returning the diluted mother liquor to the neutralization zone. Concentration of the ammonium sulphate fraction may be effected by evaporation under reduced pressure. Preferably 5 to 50 times the weight of mother liquor (with reference to the weight of rearrangement mixture) is returned to the neutralization zone.ALSO:A process for the recovery of pure lactams and pure ammonium sulphate from reaction mixtures obtained by Beckmann re-arrangement of a cycloalkanone oxime having 6 to 10 ring carbon atoms with 98 to 100% wt. sulphuric acid or oleum containing up to 35% wt. of free sulphur trioxide, which reaction mixture contains 30 to 50% wt. of lactam, comprises neutralizing said reaction mixtures by contact with ammonia in the presence of 5 to 50 times the amount (with reference to the weight of the reaction mixture) of 25 to 45% wt. ammonium sulphate solution, separating the resulting lactam and ammonium sulphate phases, evaporating the ammonium sulphate phase until ammonium sulphate has been precipitated in an amount corresponding to the sulphuric acid in the re-arrangement mixture, diluting the mother liquor with such an amount of water as is necessary to restore the ammonium sulphate solution to its original concentration, returning the diluted mother liquor to the neutralization zone, extracting the lactam phase with at least three times its weight of benzene, toluene or xylene, and distilling to obtain the lactam. Preferably 5 to 50 times the amount of mother liquor (with reference to the weight of re-arrangement mixture) is returned to the neutralization zone. Concentration of the ammonium sulphate solution may be effected by evaporation under reduced pressure. The lactam may be extracted by a countercurrent extraction in a one-stage or multi-stage process. In specific examples caprolactam and caprylolactam are produced from cyclohexanone oxine and cyclooctanone oxine respectively.

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