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    Separating tertiary phosphines from olefinic compounds
    3.
    发明专利
    Separating tertiary phosphines from olefinic compounds 未知

    公开(公告)号：GB1100250A

    公开(公告)日：1968-01-24

    申请号：GB3810166

    申请日：1966-08-25

    Applicant: BASF AG

    Inventor： REIF WERNER ,  HAUG PETER ,  FREYSCHLAG HERWIG ,  POMMER HORST

    IPC: C07C11/00 ,  C07C403/00

    Abstract: Olefinic compounds of formula where R4, R5, R6 and R7 are hydrogen atoms or saturated or unsaturated aliphatic, cycloaliphatic, araliphatic or aromatic radicals, the total number of carbon atoms being at least eight, and in which radicals R4 and R5 and/or R6 and R7 may form a fiveto eight-membered ring, said compounds being contaminated by tertiary phosphines of formula where R1, R2 and R3 are aliphatic, cycloaliphatic, araliphatic or aromatic hydrocarbon radicals having one to eight carbon atoms, are purified by contacting water-insoluble organic solutions of the olefinic compounds with aqueous solutions of peroxides or with redox resins bearing peroxide groups to convert the phosphines to tertiary phosphine oxides of formula and then separating the tertiary phosphine oxides, e.g. by extraction with suitable solvents. Olefinic compounds which may be purified include axerophthene and lycopene.ALSO:Olefinic compounds of formula where R4, R5, R6 and R7 are hydrogen atoms or saturated or unsaturated aliphatic, cyclo-aliphatic, araliphatic or aromatic radicals which may contain ester, ether, nitrile, carbonyl or hydroxyl groups, the total number of carbon atoms being at least eight, and in which radicals R4 and R5 and/or R6 and R7 may form a fiveto eight-membered ring, said compounds being contaminated by tertiary phosphines of formula where R1, R2 and R3 are aliphatic, cycloaliphatic, araliphatic or aromatic hydrocarbon radicals having one to eight carbon atoms, are purified by contacting water-insoluble organic solutions of the olefinic compounds with aqueous solutions of peroxides or with redox resins bearing peroxide groups to convert the phosphines to tertiary phosphine oxides of formula and then separating the teritary phosphine oxides, e.g. by extraction with suitable solvents. In examples, Vitamin A acid ethyl ester, Vitamin A acetate and Vitamin A palmitate, all containing triphenyl phosphine, are dissolved in octane, cyclohexane and light naphtha, and contacted with aqueous solutions of potassium hydrogen permonosulphate, hydrogen peroxide and permonosulphuric acid and with a peroxide redox resin, the phosphine oxides then being removed by extraction with mixtures of methanol and water and ethanol and water. Other olefinic compounds which may be purified are linalool, dehydrolinalool, a -ionone, b -ionone, Vitamin A aldehyde, Vitamin A2 acetate, Vitamin A2 acid ethyl ester, axeropthene, b - apo - 121 - carotenal, b - apo-121-carotenal acetate, b -apo-121-carotenic acid ethyl ester, b -apo-81-carotenal, b -apo-81-caro-tenal acetate, b -apo-81-carotenic acid ethyl ester, a -carotene, b -carotene, lycopene, farnesylacetone and isophytol.

    Purification of adipodinitrile
    5.
    发明专利
    Purification of adipodinitrile 未知

    公开(公告)号：GB1065725A

    公开(公告)日：1967-04-19

    申请号：GB3297364

    申请日：1964-08-13

    Applicant: BASF AG

    Inventor： EISFELD KARL ,  HAUG PETER ,  SCHOLZ HEINRICH ,  WEGERICH ANTON

    IPC: C07C255/04 ,  B01D9/02 ,  C07C20060101 ,  C07C67/00 ,  C07C253/00

    Abstract: Adiponitrile is purified by cooling the liquid or heating the solid so as to produce a suspension of adiponitrile crystals in liquid adiponitrile at a temperature of below 2.0 DEG C., separating the crystals, e.g. on a filter press, vacuum filter, pressure filter or in a centrifuge, washing the crystals, e.g. with pure liquid adiponitrile or with water or an organic liquid, and returning the separated liquid adiponitrile, with or without the wash liquid, to the first or another crystallization zone. The wash liquid may be pure adiponitrile obtained by partly melting the separated solid adiponitrile, e.g. while still in the separation apparatus.

    6.
    发明专利
    未知

    公开(公告)号：FR1404936A

    公开(公告)日：1965-07-02

    申请号：FR985337

    申请日：1964-08-17

    Applicant: BASF AG

    Inventor： EISFELD KARL ,  HAUG PETER ,  SCHOLZ HEINRICH ,  WEGERICH ANTON

    IPC: C07C255/04 ,  B01D9/02 ,  C07C20060101 ,  C07C67/00 ,  C07C253/00

    Abstract: Adiponitrile is purified by cooling the liquid or heating the solid so as to produce a suspension of adiponitrile crystals in liquid adiponitrile at a temperature of below 2.0 DEG C., separating the crystals, e.g. on a filter press, vacuum filter, pressure filter or in a centrifuge, washing the crystals, e.g. with pure liquid adiponitrile or with water or an organic liquid, and returning the separated liquid adiponitrile, with or without the wash liquid, to the first or another crystallization zone. The wash liquid may be pure adiponitrile obtained by partly melting the separated solid adiponitrile, e.g. while still in the separation apparatus.

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