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    Production of mixtures of cyclic ethers
    51.
    发明专利
    Production of mixtures of cyclic ethers 未知

    公开(公告)号：GB1095779A

    公开(公告)日：1967-12-20

    申请号：GB5133066

    申请日：1966-11-16

    Applicant: BASF AG

    Inventor： ADAM KARL ,  HAARER ERICH

    IPC: C07D307/06 ,  C07D309/04 ,  C07D313/04

    Abstract: A mixture of cyclic ethers is obtained by dehydration of hexanediol-(1,6) at elevated temperatures in the presence of solid dehydration catalysts, a mixture of hexanediol and water containing 1-20% by weight based on the mixture of water being used. The catalyst should preferably be non-alkaline, some examples are aluminium phosphate, aluminium oxide/chromate, aluminium oxide/boric acid and aluminium phosphate/copper chromite. Temperatures in the range 160-400 DEG C. are normally used. The cyclic ethers obtained in the mixture are hexamethylene oxide and a -methyltetrahydropyran.

    Production of alcohols by catalytic hydrogenation of carboxylic acids
    52.
    发明专利
    Production of alcohols by catalytic hydrogenation of carboxylic acids 未知

    公开(公告)号：GB1094727A

    公开(公告)日：1967-12-13

    申请号：GB1104065

    申请日：1965-03-16

    Applicant: BASF AG

    Inventor： ADAM KARL ,  HAARER ERICH ,  DORFNER KONRAD

    IPC: B01J23/18 ,  B01J23/75 ,  B01J23/84 ,  B01J27/18 ,  C07C29/149 ,  C07C29/17

    Abstract: Alcohols are prepared from carboxylic acids by catalytic hydrogenation at an elevated temperature in the presence of a cobalt catalyst which contains copper, manganese and/or chromium. Inorganic acids which can form polyacids and/or an alkali metal, alkaline earth metal or earth metal salts thereof, e.g. sulphuric, boric, phosphoric, molybdic, vanadic and tungstic acids may also be present. The catalysts may be supported, e.g. on silicic acid, bauxite, fuller's earth or aluminium oxide, or unsupported. Examples describe the hydrogenation of propionic, butyric, lauric, oleic, suberic, azelaic, and sebacic acids, decane dicarboxylic acid-(1-12) benzoic, hexahydrobenzoic, phenylacetic, and salicylic acids and a mixture containing succinic glutaric, adipic, e -hydroxycaproic, butyric, valeric and caproic acids obtained as by-product in the catalytic oxidation of cyclohexane with air.

    Separating succinic acid,glutaric acid and adipic acid from mixtures containing them
    54.
    发明专利
    Separating succinic acid,glutaric acid and adipic acid from mixtures containing them 未知

    公开(公告)号：GB1063054A

    公开(公告)日：1967-03-30

    申请号：GB2627164

    申请日：1964-06-25

    Applicant: BASF AG

    Inventor： WEGERICH ANTON ,  FUERST ERNST ,  HAARER ERICH ,  CORR 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.

    Continuous production of carboxylic amides
    56.
    发明专利
    Continuous production of carboxylic amides 未知

    公开(公告)号：GB1057726A

    公开(公告)日：1967-02-08

    申请号：GB4255863

    申请日：1963-10-29

    Applicant: BASF AG

    Inventor： SCHOLZ HEINRICH ,  STROHMEYER MAX ,  HAARER ERICH

    IPC: C07C231/02 ,  C07C233/02 ,  C07D213/72

    Abstract: In a continuous process for preparing amides by reaction of esters with primary or secondary amines, the reactants are introduced into a column in which there is, both above and below the point of introduction, a countercurrent flow of ascending vaporous products and descending liquid products (the amide being withdrawn from a point below the supply point), and a temperature gradient increasing from top to bottom. The esters are derived from C1- 4 acids and C1- 4 alcohols and the amines have 1-12 C atoms and may contain 1 or 2 OH groups or ether bridges; the column temperatures are not more than 260 DEG C. at the bottom and at least 20 DEG C. at the top. A part only of the top product is removed at a minimum reflux ratio of 2: 1. Exemplified products are HCONMe2, HCONHEt, HCONEt2, HCONBu2, HCONH (cyclohexyl) and AcNHEt.

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