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    Diacyloxy-alkanes from carboxylic acid - by electrolysis
    12.
    发明专利
    Diacyloxy-alkanes from carboxylic acid - by electrolysis 未知

    公开(公告)号：DE1950283A1

    公开(公告)日：1971-04-15

    申请号：DE1950283

    申请日：1969-10-06

    Applicant: BASF AG

    Inventor： HAUFE JUERGEN DR ,  BECK FRITZ DR

    IPC: B23K11/28 ,  C07C69/02

    Abstract: The title cpds'. acyl gps. contain 1-2C-atoms and are sepd. by >=4C-atoms in the alkane. Acyloxy-alkane carboxylic acids, with 2H-atoms alpha to the carboxyl gp. and in which the acyl residue of the acyloxy gp. contains 1-2C-atoms and is sepd. from the carboxyl gp. by >=2C-atoms, are electrochemically condensed in a solvent mixture. The latter consists of 60-98 wt.% lower alcohols, 0-30 wt.% (cyclic) N-alkyl-substd. amides or lower alkane carboxylic acids and opt., 0.30 wt.% H2O, pref., methanol and formamide. Pref., the degree of neutralization of the carboxylic acid is kept at >10% and simultaneously, the current density is kept at >10, esp. 25-50 amp/dm2. Process gives yield of approx. 80%.

    13.
    发明专利
    未知

    公开(公告)号：AT274748B

    公开(公告)日：1969-09-25

    申请号：AT656966

    申请日：1966-07-08

    Applicant: BASF AG

    Inventor： BECK FRITZ DR ,  LEITNER HANS DR ,  GUTHKE HARALD DR ,  WINTERSBERGER KARL DR

    IPC: C25B3/25 ,  C25B3/29 ,  C25B9/17 ,  C25B15/00 ,  C25B15/06

    Abstract: 1,145,539. Electrolytic cell for producing organic compounds. BADISCHE ANILIN - & SODA - FABRIK A.G. July 8, 1966 [July 9, 1965; Jan.13, 1966], No.30712/66. Heading C7B. Apparatus for performing electro-chemical reactions of organic compounds in a flowing electrolyte, particularly the hydrodimerization of acrylonitrile to adiponitrile, comprises at least one uniformly liquid-permeable electrode pair 1a, b in which the electrodes are spaced less than 1 mm. apart, preferably separated by a liquid-permeable insulator 22, e.g. porous glass fibre cloth or paper, or porous plastic sheeting or ceramics. Electrolyte may be supplied and withdrawn, preferably recycled through a heat exchanger, to enable it to flow through the electrode pair(s). Pulsations may be imparted to the electrolyte and/or the electrode pair(s), e.g. by securing the electrode support and connection 4 to a vibrator 23. Current may be supplied through metal sleeves 2 pressed coaxially into plastic spoked-wheel shaped members 3. The electrodes may be made of metal or wire cloth, screens, expanded metal or sintered articles. Cathodes may be composed of Cu, brass or iron wire coated with Pb, Cd, Hg, Hg-Pb, Pb-Th, Hg-Ag, or Zn, Cu, Pt, Pd, Ni or graphite activated with Pt; anodes may be composed of metal or wire cloth or expanded metal support of Pt, Ni, Ti, or Ta coated with Ni or Pt with a coating of PbO 2 or Tl 2 O 3 , Pt, Pt-Ir, Pt-Rh, Ni, Fe, alloy steel or graphite. For producing adiponitrile with some propionitrile, examples are given of electrolytes composed of 66-81À5% acrylonitrile, 5-15% methanol or 20 or 22À5% isopropanol or 20% dioxane or dimethyl formamide, 7 or 8% water, and 0À5 or 1% tetramethyl ammonium methyl (or p-totuene) sulphate; the pH is regulated by adding acetic acid and triethylamine through a dropping funnel 27, and the off gas pipe passes through a reflux condenser 28. A solution of monomethyl adipate in methanol, electrochemically reacted with sodium methylate, is condensed to dimethyl sebacate. The apparatus may be used for other organic electro-chemical reactions.

    16.
    发明专利
    未知

    公开(公告)号：DE2023080A1

    公开(公告)日：1971-12-02

    申请号：DE2023080

    申请日：1970-05-12

    Applicant: BASF AG

    Inventor： BECK FRITZ DR ,  NOHE HEINZ DR ,  HAUFE JUERGEN DR

    IPC: C25B3/29 ,  C07C69/50

    Abstract: 1340095 Sebacic acid diesters BADISCHE ANILIN- & SODA-FABRIK AG 11 May 1971 [12 May 1970] 14117/71 Heading C2C [Also in Division C7] Sebacic acid diesters of C 4-12 alcohols, e.g. di- 2-ethylhexyl sebacate, are made by electrochemical condensation of the corresponding adipic acid monoesters, e.g. mono-2-ethylhexyl adipate, in methanolic solution additionally containing (a) 5 to 40% of a saturated mono- or poly-valent aliphatic ether, e.g. diethyl, di-isopropyl, diglycoldimethyl or -ethyl ether, or saturated cyclic ether or diether, e.g. tetrahydrofuran, tetrahydropyran or dioxane, and/or (b) 0À1 to 2% of an alkanoic acid having up to 4 C atoms, e.g. glacial acetic, propionic or butyric acid. The current flow may be continuous or intermittent, e.g. breaking for 2 to 60 seconds after flowing for 1 to 30 minutes. The C.D. may be 5 to 50 A/dm. 2 The acidic solution may be partially neutralized by adding sodium (bi)- carbonate or methoxide. The anode may be of Pt, Pt-Rh, Pt-Ir, Au, Au-Pt, Au plated or platinized Ti or Ta; the cathode may be of Pt, steel, Ni or Ti. The electrolytic cell may have permeable vibrating or impermeable pairs of electrodes.

    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

    Inventor： SUTER HUBERT DR ,  NOHE HEINZ DR ,  BECK FRITZ DR ,  BRUEGEL WERNER DR ,  ASCHENBRENNER HEINZ

    IPC: C07C51/36 ,  C25B3/25 ,  C25B3/29 ,  C07C

    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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