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    Production of catalysts containing cobalt
    11.
    发明专利
    Production of catalysts containing cobalt 未知

    公开(公告)号：GB1145046A

    公开(公告)日：1969-03-12

    申请号：GB2716266

    申请日：1966-06-17

    Applicant: BASF AG

    Inventor： ADAM KARL ,  HAARER ERICH

    IPC: B01J23/84 ,  B01J27/188

    Abstract: 1,145,046. Preparation of amines. BADISCHE ANILIN- & SODA-FABRIK A.G. 17 June, 1966 [19 June, 1965], No. 27162/66. Heading C2C. [Also in Division B1] Isopropylamine and di-isopropylamine are prepared when 78À5 kg/hr. of isopropanol, 180 litres/hr. of liquid NH 3 and 50 cu. m. of recycled off-gas are passed over the reduced catalyst specified below at 220‹ C. together with hydrogen at a pressure of 300 atm. Phenylethylamine and diphenylethylamine are prepared by loading the reduced catalyst specified below with 4À04 kg/hr. of phenyl ethyl alcohol and 28 litres/hr. of liquid NH 3 and hydrogen at a pressure of 300 atmospheres at 220‹ C. 10 cu. m. of off-gas is recycled. The catalyst is prepared by allowing a solution containing cobalt nitrate, manganese nitrile or chromium trioxime and phosphoric acid to flow into a solution of sodium carbonate, filtering, washing and heating the resulting product, to form a composition containing more than 50% by weight of oxides, and reducing with hydrogen.

    Production of amines by the catalytic hydrogenation of nitriles
    13.
    发明专利
    Production of amines by the catalytic hydrogenation of nitriles 未知

    公开(公告)号：GB1143390A

    公开(公告)日：1969-02-19

    申请号：GB2716366

    申请日：1966-06-17

    Applicant: BASF AG

    Inventor： ADAM KARL ,  HAARER ERICH

    IPC: C07C209/48

    Abstract: 1,143,390. Preparing amines by the catalytic reduction of nitriles. BADISCHE ANILIN- & SODA-FABRIK A.G. 17 June, 1966 [19 June, 1965], No. 27163/66. Heading C2C. [Also in Division B1] Amines are prepared by hydrogenating nitriles at elevated temperature and atmospheric or superatmospheric pressure using catalysts containing 70-98% by weight of cobalt, 0À7-10% by weight of manganese and/or chromium; and pyro- or poly-acids in an amount of 0À01-10% by weight calculated as the acid or, in the case of metal acids, as the metal and optionally up to 3% by weight of other metallic activators. The catalyst employed is one which has been prepared by co-precipitating all the components from which the catalyst is derived from aqueous solutions of the metals and acids which are convertible into pyroacids or polyacids by adding caustic alkali, filtering off the precipitate, washing with water, drying, heating to obtain a mixture containing mainly oxides, heating again if desired, and prior to use, reducing with hydrogen at 200-400‹ C. to give a catalyst which is at least partly metallic.

    Production of hexamethylene oxide
    14.
    发明专利
    Production of hexamethylene oxide 未知

    公开(公告)号：GB1129279A

    公开(公告)日：1968-10-02

    申请号：GB5132866

    申请日：1966-11-16

    Applicant: BASF AG

    Inventor： ADAM KARL ,  HAARER ERICH

    IPC: C07D309/04 ,  C07D313/04

    Abstract: 1,129,279. Hexamethylene oxide. BADISCHE ANILIN- & SODA-FABRIK A.G. 16 Nov., 1966 [17 Nov., 1965], No. 51328/66. Heading C2C. Hexamethylene oxide is made by dehydrating hexane-diol-(1,6) at elevated temperatures in the presence of solid dehydration catalysts the reaction of the starting material being incomplete. The catalyst is preferably non- alkaline and porous. Numerous catalysts are specified including porous materials impregnated with dehydrating agents such as sulphuric acid. Advantageously conversions of 20-88% are effected. Reaction may be effected in an inert diluent especially water c.f. Specification 1,129,280 and 1,095,779. Advisably an inert gas, e.g. nitrogen or hydrogen, should be present. 2-Methyltetrahydropyran, polyhexamethylene oxide and hexenol-(1,6), the latter especially when catalysts containing vanadium are used, may be obtained as by-products. Examples are provided the catalysts used being (1) active aluminium oxide with 20% by weight aluminium chromate, (2) and (3) aluminium oxide containing 0À5% by weight of copper chromite, (4) aluminium oxide containing 20% by weight of aluminium chromate and 10% of boric acid, (5) aluminium phosphate containing 0À5% by weight of vanadium (as vanadium pentoxide) and (6) aluminium hydroxide containing 20% by weight of aluminium chromate and 0À5% of tungsten (as tungstic acid).

    Production of polyethers
    16.
    发明专利
    Production of polyethers 未知

    公开(公告)号：GB1125386A

    公开(公告)日：1968-08-28

    申请号：GB4695465

    申请日：1965-11-05

    Applicant: BASF AG

    Inventor： GEHM ROBERT ,  ADAM KARL

    IPC: C08G2/00 ,  C08G4/00 ,  C08G18/48 ,  C08G65/06 ,  C08G65/16 ,  C08G65/18

    Abstract: 1,125,386. Hexamethylene oxide and polymers therefrom. BADISCHE ANILIN- & SODAFABKIK A.G. 5 Nov., 1965 [6 Nov., 1964], No. 46954/65. Heading C2C. [Also in Division C3] Polymers and copolymers of hexamethylene oxide are made by polymerizing hexamethylene oxide, with or without other comonomers, in the presence of one or more Friedel-Crafts catalysts or Lewis acids in an amount of from 0À01-10 mole per cent with reference to the monomer(s) at from about - 40‹ to 150‹ C. in substance or in the presence of inert solvents. Comonomers to be used are cyclic ethers, e.g. ethylene, propylene and styrene oxides, epichlorhydrin, oxacyclobutane, di- (chloromethyl)-oxacyclobutane, tetrahydrofuran and allyl glycidyl ether, and cyclic acetals, e.g. dioxolane, trioxane, butanediolformal, and diethylene glycolformal. There may also be present in the reaction mixture regulators containing active hydrogen, such as alcohols, glycols, amines, mercaptans and water. The examples describe the preparation of polymers and copolymers from hexamethylene oxide alone and with epichlorhydrin, ethylene oxide alone and with epichlorhydrin and ethylene oxide with epichlorhydrin and butane diol-(1,4). Hexamethylene oxide (oxacycloheptane) is made by the action of potassium hydroxide on hexamethylene bromohydrin and forms an addition compound with boron trifluoride.

    Production of Polyethers.
    19.
    发明专利
    Production of Polyethers. 未知

    公开(公告)号：GB1156709A

    公开(公告)日：1969-07-02

    申请号：GB5133166

    申请日：1966-11-16

    Applicant: BASF AG

    Inventor： ADAM KARL ,  HAARER ERICH

    IPC: C08G65/00 ,  C07C41/09 ,  C07C43/13 ,  C08G65/34

    Abstract: 1,156,709. Polyethers prepared by intramolecular dehydration of diols. BADISCHE ANILIN- & SODA-FABRIK A.G. 16 Nov., 1966 [17 Nov., 1965], No. 51331/66. Heading C2C. [Also in Division C3] Polyethers are prepared by inter-molecular dehydration of alkane diols having from 5 to 12 carbon atoms and terminal hydroxyl groups at elevated temperatures in the presence of a solid, non-basic dehydration catalyst, resulting water being removed from the reaction zone at the rate at which it is formed. Suitable alkane diols, which preferably have an unbranched carbon chain, are pentanediol-(1,5), hexanediol- (1,6), octanediol-(1,8), decanediol-(1,10) and dodecanediol-(1,12) or mixtures thereof. Examples of suitable catalysts, which are preferably weakly acidic, are oxides of aluminium, thorium, tungsten, vanadium, bismuth, molybdenum, titanium, osmium and chromium, or mixtures thereof to which zinc oxide or cadmium oxide may be added; boric acid; boron phosphate; borates and phosphates, especially weakly acid phosphates; aluminas, kieselguhr, silica gel; and porous materials, e.g. pumice or active carbon, impregnated with sulphuric acid, phosphoric acid, boric acid, acid phosphates or acid-forming metal oxides. Chromates or chromites of alkaline earth or heavy metals can be added to activate the catalyst. The reaction is carried out at a temperature of from 200‹ to 400‹ C. at a pressure between 50 torr and 10 atmospheres and the residence period in the reaction zone is between 1 and 1800 seconds. Water is removed from the reaction zone by azeotropic distillation or by simultaneously passing an inert gas, e.g. nitrogen or hydrogen, and the diol over the catalyst. The diol is preferably not reacted to completion so that it may act as solvent for the polyether formed. The resulting polyethers preferably have molecular weights between 300 and 1500.

    Production of amines from aldehydes or ketones
    20.
    发明专利
    Production of amines from aldehydes or ketones 未知

    公开(公告)号：GB1130212A

    公开(公告)日：1968-10-09

    申请号：GB674866

    申请日：1966-02-16

    Applicant: BASF AG

    Inventor： ADAM KARL ,  HAARER ERICH

    IPC: B01J23/86

    Abstract: 1,130,212. Amines from aldehydes or ketones. BADISCHE ANILIN- & SODA-FABRIK A.G. 16 Feb., 1966 [17 Feb., 1965], No. 6748/66. Heading C2C. Amines are obtained by reacting an aldehyde or ketone with liquid ammonia and hydrogen under superatmospheric pressure, preferably at 90‹ to 130‹ C. under a pressure of 60 to 700 atmospheres gauge, in the presence of a catalyst comprising (a) nickel and/or cobalt; (b) chromium; and (c) at least one non-volatile mineral acid which is capable of being converted into an insoluble anhydride or an insoluble polyacid. Specified non-volatile mineral acids are sulphuric, vanadic, molybdic, tungstic, titanic and phosphorus and boric acids, the catalyst may also include manganese, cadmium, zinc and/or silver, and it may be used without a carrier or supported on a carrier material capable of eliminating water.

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