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    1.
    发明专利
    未知

    公开(公告)号：DE1190929B

    公开(公告)日：1965-04-15

    申请号：DEB0073156

    申请日：1963-08-17

    Applicant: BASF AG

    Inventor： EISFELD DR KARL ,  HAUG DR PETER ,  SCHOLZ DR HEINRICH ,  WEGERICH DR ANTON

    IPC: C07C255/04 ,  B01D9/02 ,  C07C20060101 ,  C07C67/00 ,  C07C253/00

    Abstract: Adiponitrile is purified by cooling the liquid or heating the solid so as to produce a suspension of adiponitrile crystals in liquid adiponitrile at a temperature of below 2.0 DEG C., separating the crystals, e.g. on a filter press, vacuum filter, pressure filter or in a centrifuge, washing the crystals, e.g. with pure liquid adiponitrile or with water or an organic liquid, and returning the separated liquid adiponitrile, with or without the wash liquid, to the first or another crystallization zone. The wash liquid may be pure adiponitrile obtained by partly melting the separated solid adiponitrile, e.g. while still in the separation apparatus.

    10.
    发明专利
    未知

    公开(公告)号：DE1272913B

    公开(公告)日：1968-07-18

    申请号：DEB0072428

    申请日：1963-06-26

    Applicant: BASF AG

    Inventor： WEGERICH DR ANTON ,  FUERST DR ERNST ,  HAARER DR ERICH ,  CORR DR HUBERT

    IPC: C07C51/44

    Abstract: A mixture of succinic, glutaric and adipic acids, such as obtained by the oxidation of cyclohexanol, cyclohexanone or cyclohexane is separated by fractional distillation under subatmospheric pressure in the presence of steam. The mixture is introduced from tank 1 into evaporator 2, which is heated to about 200 DEG C. and is maintained at an absolute pressure of 40 to 100 mm. Hg. The mixture then flows down column 4 into a still 5 at 195 DEG to 220 DEG C. into which superheated steam is injected through line 7. The steam laden with acid vapours is conducted from the head of the column into the evaporator, the vapours then passing through line 8 into a condenser 9 and being sprayed therein with an aqueous solution from a receiver 10. Crystals of succinic acid suspended in an aqueous solution are obtained by cooling in a vessel 14, are separated out in a centrifuge 15. The mother liquid is evaporated and the residue is returned to the crude product. The product received in vessel 6 from the still is substantially glutaric and adipic acids. Water is added to convert anhydrides into acids before preheating in 17 and passing the mixture into a column 18. The still 19 of the column is heated to 200 DEG C., a vacuum of 40-50 mm. Hg is maintained at the top of the column, and superheated steam is passed through line 20 into the still. The vapours leaving the head of the column are cooled in a condenser 21 and liquid glutaric acid so formed flows into a receiver 22 while steam with a small amount of succinic acid flows into a condenser 23. A mixture of adipic acid with a small amount of glutaric acid is withdrawn at 27 from the still from which adipic acid may be recovered by crystallization. The columns are provided with packings, baffles, spirals or bubble trays.

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