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    Method for purifying trimethylolpropane, which is produced by hydrogenation, by means of continuous distillation
    32.
    发明专利
    Method for purifying trimethylolpropane, which is produced by hydrogenation, by means of continuous distillation 未知

    公开(公告)号：AU2171001A

    公开(公告)日：2001-07-09

    申请号：AU2171001

    申请日：2000-12-21

    Applicant: BASF AG

    Inventor： DERNBACH MATTHIAS ,  KRATZ DETLEF ,  STAMMER ACHIM ,  RUST HARALD ,  SCHULZ GERHARD

    IPC: C07B61/00 ,  C07C29/80 ,  C07C31/22 ,  C07C29/141

    Abstract: A process is disclosed for the purification, by distillation, of trimethylolpropane originating from the hydrogenation of 2,2-dimethylolbutanal, said process including the following steps:(a) reaction of n-butyraldehyde with formaldehyde in the presence of catalytic amounts of a tertiary amine, and hydrogenation of the resulting mixture to give a mixture containing trimethylolpropane;(b) separation of water, methanol, trialkylamine and/or trialkylammonium formate by distillation;(c) heating of the residue obtained in (b) under reduced pressure to a temperature at which TMP is volatile and compounds boiling above TMP are cleaved, in order to separate off, by distillation, TMP and compounds more volatile than TMP;(d) distillation of the distillate obtained in (c) in order to separate off the more volatile compounds and recover pure TMP; and(e) optional distillation of the TMP obtained in (d) in order to recover TMP with a low APHA color index.A process is also disclosed in which trialkylammonium formate is distilled under mild conditions from crude mixtures of polyhydric alcohols, predominantly trimethylolpropane.

    33.
    发明专利
    未知

    公开(公告)号：DE19963435A1

    公开(公告)日：2001-07-05

    申请号：DE19963435

    申请日：1999-12-28

    Applicant: BASF AG

    Inventor： DERNBACH MATTHIAS ,  KRATZ DETLEF ,  STAMMER ACHIM ,  RUST HARALD ,  SCHULZ GERHARD

    IPC: C07B61/00 ,  C07C29/80 ,  C07C31/22

    Abstract: The invention relates to a method for carrying out the pure distillation of trimethylolpropane originating from the hydrogenation of 2,2-dimethylolbutanal with the following steps: (a) reacting n-butyraldehyde with formaldehyde in the presence of catalytic quantities of a tertiary amine and hydrogenating the mixture that is obtained in such a manner in order to form a mixture containing trimethylolpropane; (b) separating water, methanol, trialkylamine and/or trialkylammonium formate by distillation; (c) heating the remainder obtained in (b), under a vacuum, to a temperature at which TMP is volatile and at which compounds that boil at temperatures greater than that of TMP are cleaved while separating by distillation TMP as well as compounds that are less volatile than TMP; (d) distilling the distillate obtained in (c) while separating out the less volatile compounds and obtaining pure TMP; (e) carrying out the facultative distillation of the TMP obtained in (d) in order to obtain TMP that has a low alpha color index. The invention also relates to a method in which trialkylammonium formate is separated by distillation, while preserving the same, from raw mixtures consisting of polyvalent alcohols, mainly of trimethylolpropane.

    METHOD FOR PRODUCING POLYALCOHOLS
    35.
    发明专利
    METHOD FOR PRODUCING POLYALCOHOLS 未知

    公开(公告)号：CA2274083A1

    公开(公告)日：1998-07-02

    申请号：CA2274083

    申请日：1997-12-04

    Applicant: BASF AG

    Inventor： VOIT GUIDO ,  KRATZ DETLEF ,  STAMMER ACHIM ,  SCHULZ GERHARD

    IPC: C07B61/00 ,  C07C29/141 ,  C07C29/80 ,  C07C31/22 ,  C07C45/75 ,  C07C47/19

    Abstract: The invention relates to a method for producing polymethylol compounds of formula (I), in which R represents a further methylol group or an alkyl group with between 1 and 22 C atoms or an aryl or alkyl aryl group with between 6 and 22 C atoms, by condensating aldehydes with between 2 and 24 C atoms with formaldehyde, using tertiary amines as catalysts, with a view to obtaining compounds of formula (II), in which R has the meaning assigned to it above. The invention further relates to a process for hydrogenating polymethylol compounds by condensation in stages. For this, a) in a first (reaction) stage, the aldehydes with 2 or more C atoms are reacted with 2 to 8 times the molar quantity of formaldehyde in the presence of a tertiary amine as catalyst; b) in a second (separation) stage, either the reaction mixture is separated into a distillation residue containing primarily the compounds of formula (II) and a destillation flow containing primarily the compounds of unreacted or partly reacted starting materials which is fed back to the first stage, or the reaction mixture of the first stage is separated into an aqueous and an organic phase by means of a phase separation device and the organic phase fed back to the first stage, and c) in a third (post-reaction distillation) stage, the distillation residue of the second stage or the aqueous phase obtained by phase separation during the second stage is subjected to a catalytic and/or heat treatment, the compound of formula (III) which has not been fully methylolized is transformed into the corresponding compound of formula (II) and into the corresponding methylene compound of formula (IV), in which R' represents hydrogen or has the meaning assigned above to R, the reaction mixture obtained in this way is distilled, and the distillation overhead product, which contains a compound of formula (IV) and unreacted formaldehyde, is fed back to the first stage. Thereafter, the still bottom of this distillation process, which essentially contains the compound of formula (II), is hydrogenated in the known manner so as to obtain the corresponding end product of formula (I).

    39.
    发明专利
    未知

    公开(公告)号：DE50014147D1

    公开(公告)日：2007-04-19

    申请号：DE50014147

    申请日：2000-12-27

    Applicant: BASF AG

    Inventor： DERNBACH MATTHIAS ,  KRATZ DETLEF ,  STAMMER ACHIM ,  SCHULZ GERHARD

    IPC: C07C45/80 ,  C07B61/00 ,  C07C29/14 ,  C07C31/22 ,  C07C45/75 ,  C07C45/82 ,  C07C45/83 ,  C07C45/86 ,  C07C47/058 ,  C07C47/19

    Abstract: Formaldehyde is removed by distillation from reaction solutions containing a methlolated alkanal which was obtained from the reaction of formaldehyde with an alkanal which has at least one acidic hydrogen atom alpha to the carbonyl function or from the reaction of a 2-alkylacrolein or acrolein with water and formaldehyde, by a process in which this reaction was carried out in the presence of catalytic amounts of organic amine. The process permits the improved removal of formaldehyde from the reaction mixture and furthermore facilitates the hydrogenation of the alkanals thus obtained to give polyols.

    40.
    发明专利
    未知

    公开(公告)号：DE50013064D1

    公开(公告)日：2006-08-03

    申请号：DE50013064

    申请日：2000-12-21

    Applicant: BASF AG

    Inventor： DERNBACH MATTHIAS ,  KRATZ DETLEF ,  STAMMER ACHIM ,  RUST HARALD ,  SCHULZ GERHARD

    IPC: C07C29/80 ,  C07B61/00 ,  C07C29/141 ,  C07C31/22

    Abstract: A process is disclosed for the purification, by distillation, of trimethylolpropane originating from the hydrogenation of 2,2-dimethylolbutanal, said process including the following steps:(a) reaction of n-butyraldehyde with formaldehyde in the presence of catalytic amounts of a tertiary amine, and hydrogenation of the resulting mixture to give a mixture containing trimethylolpropane;(b) separation of water, methanol, trialkylamine and/or trialkylammonium formate by distillation;(c) heating of the residue obtained in (b) under reduced pressure to a temperature at which TMP is volatile and compounds boiling above TMP are cleaved, in order to separate off, by distillation, TMP and compounds more volatile than TMP;(d) distillation of the distillate obtained in (c) in order to separate off the more volatile compounds and recover pure TMP; and(e) optional distillation of the TMP obtained in (d) in order to recover TMP with a low APHA color index.A process is also disclosed in which trialkylammonium formate is distilled under mild conditions from crude mixtures of polyhydric alcohols, predominantly trimethylolpropane.

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