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    1.
    发明专利
    未知

    公开(公告)号：DE1804809A1

    公开(公告)日：1970-06-04

    申请号：DE1804809

    申请日：1968-10-24

    Applicant: BASF AG

    Inventor： BECK DR FRITZ ,  LEITNER DR HANS

    IPC: C25B3/29 ,  C07B29/06

    Abstract: Process for the production of adiponitrile by direct electrochemical hydrodimerization of acrylonitrile using a medium containing acrylonitrile, an electrolyte salt, water and, if desired, a solvent at a temperature of from 10 DEG to 60 DEG C. at a pH of from 1 to 10. In the process, electrolysis is carried out in a cell having a liquid cathode which is contacted by a solid anode which is not wetted by the liquid cathode or into which the solid anode is immersed to a depth of up to 20 mm. Adiponitrile is an important intermediate for synthetic fiber manufacture.

    4.
    发明专利
    未知

    公开(公告)号：DE1568094A1

    公开(公告)日：1970-05-06

    申请号：DE1568094

    申请日：1966-03-24

    Applicant: BASF AG

    Inventor： SUTER DR HUBERT ,  NOHE DR HEINZ ,  BECK DR FRITZ ,  HRUBESCH DR ADOLF

    IPC: C25B3/25 ,  C07C51/40

    Abstract: 1,176,036. Cyclohexadiene dicarboxylic acids. BADISCHE ANILIN- & SODA-FABRIK A.G. 23 March, 1967 [24 March, 1966], No. 13721/67. Heading C2C. [Also in Division C7] 3,5 or 2,5-Cyclohexadiene-1,2 or 1,4-dicarboxylic acid is produced by electrochemical hydrogenation of o- and/or tere-phthalic acid in aqueous H 2 SO 4 at 70-100‹ C. with a current density of 1-40 amp./sq. dm. on a cathode of Cd, Sn, Bi, Tl, or an alloy of at least two of the metals Pb, Hg, Ag, Cd, Sn, Tl and Bi; the cathode metal or alloy may be amalgamated. The phthalic acid may be dispersed in a concentration of 2-8% in aqueous H 2 SO 4 of concentration 2-50% by weight. The hydrogenation cell may be a heated or cooled doublewalled tube provided with a cylindrical cathode on or as its inner wall surrounding a cylindrical porous clay diaphragm and a water-cooled lead pipe anode; alternatively, the anode may be of Pb, Pt, PbO 2 , graphite or SiC. The catholyte may be continuously fed to the cell by a metering pump; withdrawn catholyte may be returned to the cell after crystallizing out the product and adding phthalic acid. Aqueous H 2 SO 4 may form the anolyte.

    5.
    发明专利
    未知

    公开(公告)号：DE1263768B

    公开(公告)日：1968-03-21

    申请号：DEB0082757

    申请日：1965-07-09

    Applicant: BASF AG

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

    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.

    7.
    发明专利
    未知

    公开(公告)号：DE1802865A1

    公开(公告)日：1970-09-17

    申请号：DE1802865

    申请日：1968-10-12

    Applicant: BASF AG

    Inventor： BECK DR FRITZ ,  BRUNOLD DIPL-ING ANDREAS ,  HIMMELE DR WALTER ,  HAUFE DR JUERGEN

    IPC: C25B3/29 ,  C07C69/50

    Abstract: Process for the electrochemical condensation of carboxylic acids by the electrolysis of monocarboxylic acids, half esters of dicarboxylic acids or aminocarboxylic acids in which current densities of more than 10 amp./dm.2 on vibrating electrode pairs are used, and in which the degree of neutralization of the carboxylic acids is kept below 10 percent, said process providing high space-time yields and a reaction product which can be worked up without difficulty.

    9.
    发明专利
    未知

    公开(公告)号：DE1205539B

    公开(公告)日：1965-11-25

    申请号：DEB0071842

    申请日：1963-05-10

    Applicant: BASF AG

    Inventor： BECK DR FRITZ ,  SCHUSTER DR LUDWIG

    IPC: C07C5/05 ,  C07C5/08 ,  G01N27/416 ,  G01N31/00

    Abstract: Unsaturated hydrocarbons are selectively hydrogenated in a liquid containing hydrogen ions and in the presence of a finely-divided metallic catalyst, the electrochemical hydrogen reference potential being measured during hydrogenation and the hydrogenation being stopped when the change in the reference potential with respect to time reaches or approximates to a maximum value at the prevailing pH value. Hydrogenation is carried out either by saturating the catalyst with hydrogen in a shaker prior to the addition of the organic compound, or the organic compound/catalyst mixture is put into an autoclave and the hydrogen forced in. For suitable catalysts, solvents, electrolytes and buffers (see Division B1). Examples of suitable unsaturated compounds are cyclic, mono- or polyunsaturated hydrocarbons, particularly cycloolefins and cyclo-diolefins with 5-12 C atoms, phenylacetylene; 1,3,5-triethinyl benzene, cyclohexene, cyclooctadiene. The following hydrogenations are exemplified. Example 3, one double bond in cyclooctadiene, and cyclohexene; Example 10, phenylacetylene to phenylethylene (i.e. styrene).ALSO:The electrochemical hydrogen reference potential is measured during the hydrogenation of C-C multiple bonds in organic compounds in a liquid containing hydrogen ions and in the presence of a finely divided metallic catalyst, and selective hydrogenation is effected by stopping the hydrogenation when the change in the reference potential with respect to time reaches or approximates to a maximum value at the prevailing pH value. Hydrogenation is carried out either by saturating the catalyst with hydrogen in a shaker prior to the addition of the organic compound, or the organic compound/catalyst mixture is put into an autoclave and the hydrogen forced in. For suitable catalysts, solvents, electrolytes and buffers (see Division B1). Compounds that may be hydro-genated are aralkyl compounds having acetylenic side chains, particularly those having a benzene radical and one to three side chains each having a triple bond, the side chains containing from 2-6 C atoms; acetylene alcohols, particularly acetylene alcohols with 3-16 C atoms, 1-2 triple bonds and 1-2 hydroxy groups; olefine alcohols with 3-16 C atoms, 2-3 double bond and 1-2 hydroxy groups; esters of these acetylene or olefine alcohols with lower fatty acids with 1-4 C atoms; vinyl esters; olefinically and acetylenically unsaturated carboxylic acids, particularly acetylene carboxylic acids with one to two acid groups and 3-10 C atoms; olefine carboxylic acids with 1-3 double bonds, 1-2 carboxylic groups and 3-12 C atoms; derivatives of these acids, e.g. esters of lower alcohols with 1-4 C atoms in each alkyl; unsaturated ketones, e.g. alkylalkenyl ketones and alkylalkinyl ketones with 1-6 C atoms in the alkyl and 2-6 C atoms in the unsaturated radical. Preferred compounds are named. The following hydrogenations are exemplified Ex. 1 the triple bond in 2-butinediol-(1,4) to a double bond; Ex. 2 the terminal double bond in linalool; Ex. 4 the triple bond in 1,1,4,4 - tetramethyl - 2 - butinediol - (1,4) to a double bond; Ex. 5 dimethyl ethinyl carbinol to dimethylvinyl carbinol; Ex. 6-9 (1,4)-butinediol to butenediol; Ex. 12 one double bond in farnesylacetone; Ex. 13 acetylene dicarboxylic acid to ethylene dicarboxylic acid.

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