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    PREPARATION OF BUTANEDICARBOXYLIC ACID ESTERS
    123.
    发明专利
    PREPARATION OF BUTANEDICARBOXYLIC ACID ESTERS 未知

    公开(公告)号：CA1126753A

    公开(公告)日：1982-06-29

    申请号：CA332104

    申请日：1979-07-19

    Applicant: BASF AG

    Inventor： PLATZ ROLF ,  KUMMER RUDOLF ,  SCHNEIDER HEINZ-WALTER

    IPC: B01J31/00 ,  C07B61/00 ,  C07C67/38 ,  C07C69/44 ,  C07C69/533

    Abstract: O.Z. 0050/033363 In a process for the preparation of butanedicarboxylic acid esters, whereina) an aqueous cobalt salt solution is treated, at from 50 to 200.degree.C and under a pressure of from 50 to 500 bar, with excess carbon monoxide and hydrogen in the presence of active charcoal laden with cobalt carbonyl,b) the resulting aqueous solution of cobalt carbonyl hydride is extracted with butadiene, or with a hydrocarbon mixture containing butadiene, and the aqueous phase is separated off,c) the butadiene, or the butadiene/hydrocarbon mixture, containing cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl, is reacted with carbon monoxide and a C1-C4-alkanol in excess in the presence of from 0.5 to 2 moles, per mole of butadiene, of a tertiary nitrogen base having a pKa of from 3 to 11, at from 80 to 150.degree.C and under a pressure of from 300 to 2,000 bar,d) the tertiary nitrogen base contained in the resulting reaction mixture is removed until its content reaches 0.1-0.3 mole per mole of pentenoic acid ester, excess hydrocarbons are also removed, the pentenoic acid ester remaining in the reaction mixture is reacted with carbon monoxide and a C1-C4-alkanol in excess at from 140 to 200.degree.C and under a pressure of from 100 to 400 bar in the presence of the amounts of cobalt carbonyl and tertiary nitrogen base present in the reaction mixture, and excess alkanol and free nitrogen base are then distilled off, ande) the reaction mixture which is left and which con O.Z. 0050/033363 tains a cobalt catalyst, butanedicarboxylic acid ester and by-products is treated with oxidizing agents in the presence of the aqueous acid solution which has been removed in stage b), and the mixture is separated into an organic phase, from which butanedicarboxylic acid ester is isolated by distillation, and an aqueous phase, containing cobalt salts, which is recycled to stage a), the improvement that the aqueous phase separated off in stage b) is heated at from 250 to 350.degree.C under superatmospheric pressure, before being used in stage e).

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