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    4.
    发明专利
    未知

    公开(公告)号：DE2713195A1

    公开(公告)日：1978-10-05

    申请号：DE2713195

    申请日：1977-03-25

    Applicant: BASF AG

    Inventor： KUMMER RUDOLF DIPL CHEM DR ,  SCHNEIDER HEINZ-WALTER DIPL CH ,  PLATZ ROLF DIPL CHEM DR ,  MAGNUSSEN PETER DIPL CHEM DR ,  WEISS FRANZ-JOSEF DIPL CHEM DR

    IPC: C07C69/44 ,  B01J31/00 ,  C07B61/00 ,  C07C67/38 ,  C07C69/34 ,  C07C69/52

    Abstract: A process for the manufacture of butanedicarboxylic acid esters, wherein (A) AN AQUEOUS COBALT SALT SOLUTION IS TREATED, AT FROM 50 DEG TO 200 DEG C. and under a pressure of from 50 to 500 bars, 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 BUTADIENE-HYDROCARBON MIXTURE, CONTAINING COBALT CARBONYL HYDRIDE, COBALT CARBONYL AND BUTENYL-COBALT TRICARBONYL IS REACTED WITH CARBON MONOXIDE AND AN EXCESS OF AN ALKANOL OF 1 TO 4 CARBON ATOMS 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 DEG to 150 DEG C. under a pressure of from 300 to 2,000 bars, and (D) THE RESULTING REACTION MIXTURE IS FREED FROM THE TERTIARY NITROGEN BASE CONTAINED THEREIN, EXCEPT FOR FROM 0.1 TO 0.3 MOLE PER MOLE OF PENTENOIC ACID ESTER, AND FROM EXCESS HYDROCARBONS, THE PENTENOIC ACID ESTER REMAINING IN THE REACTION MIXTURE IS REACTED WITH CARBON MONOXIDE AND AN EXCESS OF AN ALKANOL OF 1 TO 4 CARBON ATOMS AT FROM 140 DEG TO 200 DEG C. and under pressures of from 100 to 400 bars in the presence of the amounts of cobalt carbonyl and tertiary nitrogen base contained in the reaction mixture, and excess alkanol and free nitrogen base are then distilled off, and (E) THE REACTION MIXTURE WHICH REMAINS, AND WHICH CONTAINS COBALT CATALYST, THE BUTANEDICARBOXYLIC ACID ESTER AND BY-PRODUCTS IS TREATED WITH AN OXIDIZING AGENT IN AN AQUEOUS ACID MEDIUM AND THE MIXTURE IS SEPARATED INTO AN ORGANIC PHASE, FROM WHICH THE BUTANEDICARBOXYLIC ACID ESTER IS ISOLATED BY DISTILLATION, AND INTO AN AQUEOUS PHASE CONTAINING COBALT SALTS.

    Ester interchange catalysed by acid ion exchanger - with addn. of water to give quantitative yield
    5.
    发明专利
    Ester interchange catalysed by acid ion exchanger - with addn. of water to give quantitative yield 未知

    公开(公告)号：DE2950100A1

    公开(公告)日：1981-06-19

    申请号：DE2950100

    申请日：1979-12-13

    Applicant: BASF AG

    Inventor： KUMMER RUDOLF DIPL CHEM DR ,  TAGLIEBER VOLKER DIPL CHEM DR

    IPC: C07C67/02 ,  C07C67/03 ,  C07C69/34

    Abstract: In the prodn. of esters (I) of mono- or polybasic carboxylic acids by ester interchange, using acid ion exchanger as esterification catalyst, ester interchange is carried out in the presence of 0.01-10 wt.% water, w.r.t. the amt. of liquid phase in the reaction mixt. Practically quantitative yields of (I) are obtd. corresp. to an increase in yield of 10-40% age points. In an example, a homogeneous soln. of 348 g (2 mole) dimethyl adipate, 624 g (4.8 mole) 2-ethylhexan-1-ol and 4.8 g water (0.5 wt.% of the liquid phase) was heated 2 h under reflux in the presence of 10 g acid ion exchanger (sulphonated crosslinked polystyrene). Then the water and excess 2-ethylhexanol were distilled off at normal pressure and 65 deg.C for the first 4 h and then at 10 mbar and 80 deg.C. Di(2-ethylhex-l-yl) adipate was obtd. in 99.7% yield. If no water was added, the yield of ester was only 64.8%.

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