3.
    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

    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.

    Bubble columns for gas-liquid reactions - with subdividing sieve plates having defined and adjustable openings

    公开(公告)号:DE2634785A1

    公开(公告)日:1978-02-09

    申请号:DE2634785

    申请日:1976-08-03

    Applicant: BASF AG

    Abstract: A reaction column contains intermediate sieve plates whose spacing is less than twice the column dia. and whose total hole area is 10-40% of the column cross-section. Specifically, bubbling type gas-liquid reaction column is subdivided internally by sieve plates which are arranged in a demountable module for easy replacement. Each plate is of double construction so that by relative rotation of the two parts the available hole opening may be adjusted to suit the characteristics of the reacting system. The individual hole dia. is pref. >10mm, and the holes are circular; in a 400 mm i/d column the plate spacing is >=200 mm. Used for continuous chemical reaction between counter-flowing gas and liq. or slurry streams, in columns of dia. >400 mm. Reduces back-mixing effect without the complexity of column packing and without the need for reaction systems in cascade.

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