11.
    发明专利
    未知

    公开(公告)号:DE1643654A1

    公开(公告)日:1971-07-15

    申请号:DE1643654

    申请日:1967-08-29

    Applicant: BASF AG

    Abstract: 1,228,623. Bicyclo-[2,2,2]-oct-7-en-2,3,5,6- tetracarboxylic dianhydride. BADISCHE ANILIN- & SODA-FABRIK A.G. 28 Aug., 1968 [29 Aug., 1967], No. 41125/68. Heading C2C. Bicyclo - [2,2,2] - oct - 7 - en - 2,3,5,6 - tetracarboxylic dianhydride is prepared by first heating 3,5 - cyclohexadiene - 1,2 - trans - dicarboxylic acid in the anhydride of a C 2-4 alkanecarboxylic acid in the presence of active carbon having an internal surface area of more than 500 m. 2 /g., an adsorbent clay, silica gel, aluminium oxide or aluminium hydroxide, to the reaction temperature of 50-150‹ C. and only then adding maleic anhydride for reaction. Batch or continuous reaction may be used. The mixture may be held at reaction temperature for 5-10 minutes in the presence of the absorbent before adding the maleic anhydride.

    12.
    发明专利
    未知

    公开(公告)号:DE1953259A1

    公开(公告)日:1971-05-06

    申请号:DE1953259

    申请日:1969-10-23

    Applicant: BASF AG

    Abstract: 1318795 Cyclohexadiene dioic acids BADISCHE ANILIN- & SODA-FABRIK AG 22 Oct 1970 [23 Oct 1969] 50117/70 Heading C2C [Also in Division C7] 3,5-Cyclohexadiene-1,2-dioic acid and 2,5- cyclohexadiene-1,4-dioic acid are prepared by the electrochemical reduction of o-phthalic acid and terephthalic acid respectively in a cell wherein the anode and cathode chambers are separated by a diaphragm, using a catholyte containing an organic solvent, the flow of electrolysis current being periodically broken and the electrolytic cell short-circuited. Typically the catholyte contains 5-25 wt. per cent phthalic acid, 40-80% of organic solvent (ethers, carboxamides, and/or nitriles, e.g. dioxane, tetrahydrofuran, glycolmonoethylether, dimethylformamide or acetonitrile), 5-40% H 2 O, and 1-20% H 2 SO 4 ; the anolyte is 2-20% H 2 SO 4 . The diaghragm may be an ion-exchange material or plastic tissue; the anode Pb, PbO 2 , graphite or a platinum metal, and the cathode Pb. A current density of 1-30 A/dm 2 and a temperature of 20-70‹ C. may be used, the current being interrupted and shortcircuiting taking place for 5 sec.-15 min. every 6 min.-20 hrs.; the ratio electrolysis period: no current period being 10,000 : 1 to 100 : 5. At intervals the current may be reversed at 1/100 to 1/5 of working value instead of the above-mentioned cessation. In an embodiment, six bipolar plate-shaped Pb electrodes are connected in series (and optionally water-cooled) with sulphonated polystyrene diaphragms between anodes and cathodes; the cathode chambers are connected in series to permit continuous pumping of catholyte; the product is recovered by evaporation of the organic solvent and filtration.

    13.
    发明专利
    未知

    公开(公告)号:DE1618136A1

    公开(公告)日:1971-03-11

    申请号:DEB0092089

    申请日:1967-04-15

    Applicant: BASF AG

    Abstract: 1,180,117. Distillation columns; purification of phthalic anhydride. BADISCHE ANILIN-& SODA-FABRIK A.G. 19 May, 1967 [21 May, 1966; 15 April, 1967], No. 23398/67. Heading BIB. [Also in Division. C2] Phthalic anhydride is purified by distillation in a plant comprising two fractionating columns 1, 5 of the tray-type connected as shown to two evaporators 2, 8 each containing a vertically-disposed bundle of tubes, the arrangement being such that the distilland flows down as a thin film on the inside of the tubes. The material to be purified is introduced about half-way up column 1, which is maintained under reduced pressure. Vapours comprising about 37% of the feed, including all the low-boiling impurities, leave the head of column 1, and are condensed; and part of the condensate is refluxed to the column. Highboiling impurities are withdrawn from the system through line 9. Purified phthalic anhydride is obtained at the head of column 5.

    18.
    发明专利
    未知

    公开(公告)号:DE1956238A1

    公开(公告)日:1971-05-13

    申请号:DE1956238

    申请日:1969-11-08

    Applicant: BASF AG

    Abstract: Continuous manufacture of dichloroisocyanuric acid by reacting cyanuric acid with chlorine aqueous alkaline solution at a specific ratio of the reactor dimensions, under specific conditions of temperature and flow rate of the reaction mixture and at a specific molar ratio of the starting materials.

    19.
    发明专利
    未知

    公开(公告)号:DE1618078B1

    公开(公告)日:1971-02-04

    申请号:DE1618078

    申请日:1967-01-11

    Applicant: BASF AG

    Abstract: 1,203,108. Cyclohexadiene dicarboxylic acids. BADISCHE ANILIN- & SODA-FABRIK A.G. 10 Jan., 1968 [11 Jan., 1967], No. 1413/68. Heading C2C. [Also in Division C7] 3,5 - Cyclohexadiene - 1,2 - dicarboxylic acid and 2,5-cyclohexadiene-1,4-dicarboxylic acid are produced by electrochemical hydrogenation of o-phthalic acid and terephthalic acid respectively in dilute aqueous sulphuric acid at a temperature up to 80‹ C. and at a current density of 1-40 amps per sq. decimetre at the cathode, there being added to the catholyte an ether, amide and/or nitrile which is miscible with water, is inert under the reaction conditions and is liquid at room temperature. The organic solvents which may be used are saturated cyclic ethers, e.g. dioxane, or tetrahydrofuran; monoethers or diethers of ethylene glycol or 1,2- propylene glycol; alkyl radicals of ether groups such as ethylene glycol monomethyl ether.; N- monoalkyl substituted and N,N-dialkyl substituted amides of aliphatic monocarboxylic acids such as methyl formamide, N-methylacetamide, N-ethylacetamide, dimethyl formamide, diethyformamide or N,N-dimethylacetamide and other N,N-dialkylacetamides, N,N-dimethylpropionamide; N-alkyl substituted laotams such as N-methylpyrrolidone, N-ethylpyrrolidone or N-methylpiperidone; formamide; or nitriles such as acetonitrile. As anolyte an aqueous solution of sulphuric acid may be used. The anodes used may be formed of lead, lead dioxide, platinum, graphite, silicon carbide or magnetic materials, and the cathodes used may be of lead, amalgamated lead, cadmium, tin, thallium, bismuth or alloys of at least two of the metals lead, mercury, silver, cadmium, tin, thallium and bismuth. The cell used may be formed of glass, metal or plastics. The diapragm separating analyte and catholyte may comprise an ion exchange membrane, plastics fabric or ceramic materials, e.g. porous clay. One form of cell comprises a double-walled glass tube which is cooled with water, a cylindrical lead cathode in contact with the inner wall of the glass tube, a cylindrical clay diaphragm positioned within the cathode and separating cathode from anode, and an anode comprising a lead tube cooled by water.

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