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    Production of Amines from Mixtures Containing n-Amyl Alcohol and Cyclopentanol
    62.
    发明专利
    Production of Amines from Mixtures Containing n-Amyl Alcohol and Cyclopentanol 未知

    公开(公告)号：GB1167412A

    公开(公告)日：1969-10-15

    申请号：GB768467

    申请日：1967-02-17

    Applicant: BASF AG

    Inventor： WINDERL SIEGFRIED ,  CORR HUBERT ,  HAARER ERICH

    Abstract: 1,167,412. The production of cyclopentylamine and n-pentylamine. BADISCHE ANILIN- & SODA-FABRIK A.G. 17 Feb., 1967 [19 Feb., 1966], No. 7684/67. Heading C2C. Cyclopentylamine and n-pentylamine are prepared by reacting a mixture, which contains mainly cyclopentanol and n-pentanol and which has been prepared by the hydrogenation of the by-products obtained from the air oxidation of cyclohexane after the removal of cyclohexanone and cyclohexanol, with 8 to 20 moles of ammonia per mole of alcohol at temperatures of 100‹ to 300‹ C. and at pressures of 10 to 500 atmospheres in the presence of a conventional hydrogenation catalyst to form a mixture of the corresponding amines, adding water and separating the n-pentylamine by azeotropic distillation. Suitably the reaction is carried out in the presence of hydrogen and using cobalt and/or nickel as catalyst and the starting mixture contains 50 to 80% w/w of n-pentanol and 10 to 14% w/w of cyclopentanol.

    Continuous production of alkane dicarboxylic acids
    64.
    发明专利
    Continuous production of alkane dicarboxylic acids 未知

    公开(公告)号：GB1092603A

    公开(公告)日：1967-11-29

    申请号：GB1012365

    申请日：1965-03-10

    Applicant: BASF AG

    Inventor： RIEGELBAUER GEORG ,  WEGERICH ANTON ,  KUERZINGER ALFRED ,  HAARER ERICH

    IPC: C07C55/02 ,  C07C51/00 ,  C07C67/00

    Abstract: Alkane dicarboxylic acids are prepared by a continuous process wherein cycloalkanols, cycloalkanones, cycloalkylamines, o - hydroxyalkane carboxylic acids having at least four carbon atoms, lactones of such acids and/or tetrahydrofurane are oxidized by intensely mixing said organic reactant with a large excess of 40 to 70% by weight nitric acid, the reaction is allowed to proceed at atmospheric or superatmospheric pressure and a temperature of 20 DEG to 100 DEG C., after a residence period of less than four minutes the mixture leaving the reaction zone is freed from nitrous oxides, the concentration of nitric acid is restored by evaporation of water to a level which is approximately that of the reaction zone nitric acid concentration, the alkane dicarboxylic acid is separated by a conventional method from a minor portion of the reaction mixture, the mother liquor is united with the remainder of the reaction mixture, fresh nitric acid, if desired, is added to the mixture thus obtained and this mixture is intensely mixed with fresh initial organic material and returned to the reaction zone.

    Separating ammonia from trimethylamine
    67.
    发明专利
    Separating ammonia from trimethylamine 未知

    公开(公告)号：GB1049579A

    公开(公告)日：1966-11-30

    申请号：GB3560163

    申请日：1963-09-10

    Applicant: BASF AG

    Inventor： HAARER ERICH ,  PLASS REINHOLD

    IPC: C01C1/00 ,  C01C1/10 ,  C01C1/12

    Abstract: The individual components of a mixture consisting essentially of ammonia and trimethylamine, containing traces of mono- and di-, are separated by (a) cooling the mixture to - 55 DEG to - 85 DEG C., preferably - 65 DEG to - 85 DEG C., and (b) adding 0.5 to 6%, preferably 0.5 to 1.5%, by weight of water, in either sequence, and separating the resulting two layers from each other. The lower layer, according to the examples, is the aqueous layer containing most of the ammonia.ALSO:The individual components of a mixture consisting essentially of ammonia and trimethylamine, containing traces of mono- and diare separated by (a) cooling the mixture to -55 DEG to -85 DEG C., preferably -65 DEG to -85 DEG C., and (b) adding 0.5 to 6%, preferably 0.5 to 1.5%, by weight of water, in either sequence, and separating the resulting two layers from each other. The lower layer, according to the examples is the aqueous layer containing most of the ammonia.

    Production of diamines
    68.
    发明专利
    Production of diamines 未知

    公开(公告)号：GB1027508A

    公开(公告)日：1966-04-27

    申请号：GB596563

    申请日：1963-02-14

    Applicant: BASF AG

    Inventor： WINDERL SIEGFRIED ,  HAARER ERICH ,  CORR HUBERT ,  HORNBERGER PAUL

    IPC: B01J23/38 ,  B01J23/70 ,  C07C209/16 ,  C07C211/10 ,  C07C211/11 ,  C07C211/12

    Abstract: Catalysts for the production of diamines (see Division C2) comprise at least one of the metals silver, copper, iron, cobalt and nickel prepared by sintering the metal powder or by reducing the sintered metal oxide or hydroxide, carbonate, nitrate or nitrite before or after shaping. Examples employ sintered Co, (Co + Ni), and (Co + Cu) or Ni. The powdered metal is sintered in admixture with a carrier such as pumice, alumina, corundum, diatomaceous earth, silica gel, silicon carbide, silicates, porcelain or quartz. Promoters such as alkali metal compounds, alkaline earth metal compounds, titanium dioxide, antimony, bismuth, or compounds of Group V or V1 of the Periodic System may also be added.ALSO:Open-chain diamines are prepared by passing a dihydric aliphatic alcohol, an alkanolamine, alkylene oxide or hexamethyleneimine or mixtures thereof, with a stoichiometric excess of ammonia or a primary or secondary amine, in the presence of at least 2 litres of hydrogen per mole of alcohol, alkanolamine, alkylene oxide or hexamethyleneimine, in the presence or absence of water, at 150-300 DEG C. at a pressure of at least 10 atmospheres, over a catalyst containing at least one of the metals silver, copper, iron, cobalt and nickel, said catalyst having been prepared by sintering. Examples prepare (1) ethylene diamine and piperazine from ethylene glycol and ammonia, and 1,2-diaminopropane similarly from 1,2-propanediol; (2) ethylene diamine and piperazine from ethanolamine, diethanolamine and ammonia, or from ethylene oxide and ammonia; (3), (4), (5) 1,6-hexamethylenediamine and hexamethyleneimine from 1,6-hexanediol and ammonia or hexamethyleneimine and ammonia; (6) N,N,N1,N1 - tetra ethyl ethylenediamine and N,N-diethylethanolamine from ethylene glycol and diethylamine; and (7) N-isopropyl-1,3-diaminopropane from 1,3-propanolamine and isopropylamine. Other reactants are listed.ALSO:Catalysts for the production of diamines (see Division C2) contain at least one of the metals silver, copper, iron, cobalt and nickel and are prepared by sintering the powdered metal in admixture with a carrier such as pumice, alumina, corundum, diatomaceous earth, silica gel, silicon carbide, silicates, porcelain or quartz, or by sintering oxides of the metal or compounds converted into oxides at sintering temperature, such as hydroxides, carbonates, nitrates and nitrites, in the presence of a carrier as above and/or a promoter such as alkali metal compounds, alkaline earth metal compounds, titanium dioxide, antimony, bismuth, or compounds of metals of Group V or VI of the Periodic System, and then reducing the sintered oxide with hydrogen.

    69.
    发明专利
    未知

    公开(公告)号：FR1426720A

    公开(公告)日：1966-01-28

    申请号：FR9533

    申请日：1965-03-17

    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.

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