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    Separating succinic acid,glutaric acid and adipic acid from mixtures containing them
    11.
    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 A mixture of adipic acid with a small amount of glutaric acid is withdrawn at 27 from the still from which adipic acid may be recovered by crystallization.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.

    15.
    发明专利
    未知

    公开(公告)号：FR1511539A

    公开(公告)日：1968-01-26

    申请号：FR95219

    申请日：1967-02-16

    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.

    Production of Amines from Mixtures Containing n-Amyl Alcohol and Cyclopentanol
    18.
    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.

    Production of diamines
    19.
    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.

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