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    4.
    发明专利
    未知

    公开(公告)号：DE3868970D1

    公开(公告)日：1992-04-16

    申请号：DE3868970

    申请日：1988-04-27

    Applicant: BASF AG

    Inventor： MERGER FRANZ DR ,  HETTINGER PETER DR ,  HUPFER LEOPOLD DR ,  PAETSCH JUERGEN DR ,  DECK HERIBERT ,  AUER HEINZ ,  BRUNNER ERWIN DR

    IPC: C07C69/06 ,  C07C27/00 ,  C07C27/02 ,  C07C29/38 ,  C07C29/74 ,  C07C29/88 ,  C07C31/22 ,  C07C67/00 ,  C07C67/03 ,  C07C67/08 ,  C07C67/54 ,  C07C209/00 ,  C07C209/82 ,  C07C209/86 ,  C07C211/03 ,  C07C211/05

    Abstract: Recovery of trialkylamines (I) and methyl formate (II) from reaction mixts. from the prodn. of trimethylolalkanes by reacting n-alkanals (IV) with 2.2-4.5 mole HCHO in aq. soln. and 0.6-3 mole (I) per mole (IV), followed by hydrogenation, involves: (a1) heating the mixt. to 100-200 deg. C to distil off the water present, opt. with any excess (I), and liberate (I), which is distilled off, from the trialkylammonium formate (V), giving the trimethylolalkane formate (VI); and (a2) subjecting (VI) to ester exchange with MeOH, opt. in the presence of catalytic amts. of alkali(ne earth) alcoholates (VII), giving trimethylolalkane and (II); or (b1) dehydration and sepn. of any excess free (I); and (b2) liberating (I) from (V) by treating the remaining mixt. with MeOH and heating to 100-200 deg. C to form (II) and (I); and isolating the reaction prods. in the usual way. Pref. the reaction mixt. is treated with 1-20 mole MeOH/mole (VI). (VII) is NaOMe or KOMe and is used in an amt. of 0.005-0.05 mole (VI). In method (a), (VI) is reacted with MeOH at 0-60 deg. C. In method (b), reaction with MeOH is carried out continuously at 10-25 bar and the water content of the reaction mixt. is reduced to ca. 5-15 wt.% before liberation of (I).

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