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    Method for purifying trimethylolpropane, which is produced by hydrogenation, by means of continuous distillation
    1.
    发明授权
    Method for purifying trimethylolpropane, which is produced by hydrogenation, by means of continuous distillation 失效
    通过连续蒸馏通过氢化制备三羟甲基丙烷的方法

    公开(公告)号：US06692616B2

    公开(公告)日：2004-02-17

    申请号：US10168980

    申请日：2002-06-26

    申请人： Matthias Dernbach ,  Detlef Kratz ,  Achim Stammer ,  Harald Rust ,  Gerhard Schulz

    发明人： Matthias Dernbach ,  Detlef Kratz ,  Achim Stammer ,  Harald Rust ,  Gerhard Schulz

    IPC分类号： B01D314

    CPC分类号： C07C29/80 ,  C07C31/225 ,  C07C31/12 ,  C07C31/245 ,  C07C31/04

    摘要： 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.

    摘要翻译： 公开了一种通过蒸馏纯化来自2,2-二羟甲基丁烷的氢化的三羟甲基丙烷的方法，所述方法包括以下步骤：（a）在催化量的叔碳酸存在下，正丁醛与甲醛的反应 胺，并氢化得到的混合物，得到含有三羟甲基丙烷的混合物;（b）通过蒸馏分离水，甲醇，三烷基胺和/或三烷基铵甲酸盐;（c）将（b）中得到的残余物在减压下加热至 TMP挥发的温度和TMP沸点高的化合物被切割，以便通过蒸馏分离TMP和比TMP更易挥发的化合物;（d）蒸馏（c）中获得的馏出物，以分离出更多的 挥发性化合物，回收纯TMP; 为了回收具有低APHA颜色指数的TMP，还可以任选地蒸馏（d）中获得的TMP。还公开了一种方法，其中在温和条件下从多元醇，主要是三羟甲基丙烷的粗混合物中蒸馏出三烷基铵甲酸盐。

    Method for the separation of formaldehyde from a reaction mixture containing polyols by the addition of solvents before and/or during the distillation
    2.
    发明授权
    Method for the separation of formaldehyde from a reaction mixture containing polyols by the addition of solvents before and/or during the distillation 失效
    在蒸馏之前和/或期间通过加入溶剂从含有多元醇的反应混合物中分离甲醛的方法

    公开(公告)号：US06809224B2

    公开(公告)日：2004-10-26

    申请号：US10168999

    申请日：2002-06-26

    申请人： Matthias Dernbach ,  Detlef Kratz ,  Achim Stammer ,  Gerhard Schulz

    发明人： Matthias Dernbach ,  Detlef Kratz ,  Achim Stammer ,  Gerhard Schulz

    IPC分类号： C07C4582

    CPC分类号： C07C45/82 ,  C07C45/83 ,  C07C47/19

    摘要： 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 &agr; 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.

    摘要翻译： 从甲醛与具有至少一个羰基官能度的至少一个酸性氢原子的α-烷醛或由2-烷基丙烯醛或丙烯醛与水的反应的甲醛反应获得的含有甲基化的烷醛的反应溶液中蒸馏除去甲醛， 甲醛，通过在催化量的有机胺存在下进行该反应的方法。 该方法允许从反应混合物中改善甲醛的去除，并且进一步促进由此获得的链烷烃的氢化以产生多元醇。

    Method for the decomposition of high boiling by-products produced in the synthesis of polyhydric alcohols
    4.
    发明授权
    Method for the decomposition of high boiling by-products produced in the synthesis of polyhydric alcohols 失效
    分解合成多元醇产生的高沸点副产物的方法

    公开(公告)号：US06586641B2

    公开(公告)日：2003-07-01

    申请号：US10169001

    申请日：2002-06-26

    申请人： Matthias Dernbach ,  Detlef Kratz ,  Achim Stammer ,  Gerhard Schulz

    发明人： Matthias Dernbach ,  Detlef Kratz ,  Achim Stammer ,  Gerhard Schulz

    IPC分类号： C07C3118

    CPC分类号： C07C29/80 ,  C07C31/20 ,  C07C31/22 ,  C07C31/205 ,  C07C31/245

    摘要： A process is provided for increasing the yield in the preparation of polyhydric alcohols obtained from methylolated alkanals by hydrogenation, wherein derivatives of these alcohols are decomposed by adding 5 ppm to 1% by weight, preferably 100 to 1000 ppm, of a suitable acid to an anhydrous mixture containing these derivatives, heating the mixture to temperatures of 100 to 300° C. and then separating off the polyhydric alcohol by distillation. This process makes it possible simply and efficiently to decompose compounds which boil above the polyhydric alcohol and are unwanted by-products of its synthesis.

    摘要翻译： 提供了一种通过氢化提高由羟甲基化的链烷醇制备的多元醇的产率的方法，其中这些醇的衍生物通过将5ppm至1wt％，优选100-1000ppm的合适的酸加成到 含有这些衍生物的无水混合物，将混合物加热至100-300℃，然后蒸馏除去多元醇。 该方法使得可以简单有效地分解沸腾在多元醇上的化合物并且是其合成的不希望的副产物。

    Method for hydrating poly-or monomethylol alkanals
    5.
    发明授权
    Method for hydrating poly-or monomethylol alkanals 有权
    水合多羟基或单羟基链烷醇的方法

    公开(公告)号：US07060861B2

    公开(公告)日：2006-06-13

    申请号：US10399502

    申请日：2001-11-02

    申请人： Matthias Dernbach ,  Michael Koch ,  Gerhard Schulz ,  Hagen Weigl ,  Steffen Maas

    发明人： Matthias Dernbach ,  Michael Koch ,  Gerhard Schulz ,  Hagen Weigl ,  Steffen Maas

    IPC分类号： C07C33/26 ,  C07C27/00 ,  C07C31/18

    CPC分类号： C07C29/141 ,  C07C31/20 ,  C07C33/26 ,  C07C31/22

    摘要： In a process for the catalytic hydrogenation of a polymethylolalkanal or a monomethylolalkanal of the formula (I) where R may be identical or different and are each a substituted or unsubstituted aliphatic hydrocarbon having from 1 to 22 carbon atoms, an aryl or arylalkyl group having from 6 to 22 carbon atoms or a methylol group, in the presence of a copper-containing catalyst, the hydrogenation feed comprising the polymethylolalkanal or monomethylolalkanal has a total content of metal ions of groups 3 to 14 of the Periodic Table of the Element of up to 5 ppm.

    摘要翻译： 在其中R可以相同或不同并且各自为具有1至22个碳原子的取代或未取代的脂族烃的式（I）的多羟甲基烷醇或单羟基烷醇的催化氢化的方法中， 6至22个碳原子或羟甲基，在含铜催化剂存在下，包含多羟甲基烷醛或单羟基烷醇的氢化进料具有元素周期表第3至14组的金属离子总含量，直至 5 ppm。

    Method for increasing yield in the production of polyvalent alcohols by splitting by-products containing acetal
    8.
    发明申请
    Method for increasing yield in the production of polyvalent alcohols by splitting by-products containing acetal 失效
    通过分解含缩醛的副产物来提高多元醇生产中产率的方法

    公开(公告)号：US20050256346A1

    公开(公告)日：2005-11-17

    申请号：US10521810

    申请日：2003-07-18

    申请人： Alexander Wartini ,  Tilman Sirch ,  Johann-Peter Melder ,  Matthias Dernbach

    发明人： Alexander Wartini ,  Tilman Sirch ,  Johann-Peter Melder ,  Matthias Dernbach

    IPC分类号： C07C29/10 ,  C07C29/141 ,  C07C29/88 ,  C07C45/75 ,  C07C29/14

    CPC分类号： C07C29/141 ,  C07C29/10 ,  C07C29/88 ,  C07C45/75 ,  C07C31/22 ,  C07C47/19

    摘要： The invention relates to a method for increasing yield in the production of polyvalent alcohols, especially trimethylolpropane, obtained by condensing formaldehyde with a higher aldehyde. According to the inventive method, acid treatment is carried out on a mixture (high-boiling fraction) that is obtained by reprocessing, contains derivatives of said alcohols and has a higher boiling point than the respective alcohol, and the polyvalent alcohol is recovered from the acid-treated high-boiling fraction. The inventive method is characterised in that the water content of the high-boiling fraction amounts to between 20 and 90 wt. % in relation to the entire mixture of the high-boiling fraction and water.

    摘要翻译： 本发明涉及通过将甲醛与较高级醛缩合而获得的多价醇，特别是三羟甲基丙烷的生产中提高产量的方法。 根据本发明的方法，通过后处理获得的含有所述醇的衍生物并且具有比各醇更高的沸点的混合物（高沸点馏分）进行酸处理，并且从所述醇中回收多元醇 酸处理的高沸点馏分。 本发明的方法的特征在于高沸点馏分的含水量在20-90wt。之间。 相对于高沸点馏分和水的整个混合物的％。