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    Preparation of citral
    1.
    发明授权
    Preparation of citral 有权
    柠檬醛的制备

    公开(公告)号：US06175044B1

    公开(公告)日：2001-01-16

    申请号：US09404548

    申请日：1999-09-24

    申请人： Jörg Therre ,  Gerd Kaibel ,  Werner Aquila ,  G{umlaut over (u)}nter Wegner ,  Hartwig Fuchs

    发明人： Jörg Therre ,  Gerd Kaibel ,  Werner Aquila ,  G{umlaut over (u)}nter Wegner ,  Hartwig Fuchs

    IPC分类号： C07C4551

    CPC分类号： C07C45/515 ,  C07C45/513 ,  C07C45/67 ,  C07C47/21

    摘要： 3,7-Dimethyl-2,6-octadien-1-al of formula I is prepared continuously by: thermally cleaving, in the presence or absence of an acid catalyst, 3-methyl-2-buten-1-al diprenyl acetal of formula II: thereby eliminating 3-methyl-2-buten-1-ol of formula III and yielding cis/trans-prenyl 3-methylbutadienyl ether of formula IV: thermally rearranging the resultant butadienyl ether of formula IV thereby yielding 2,4,4-trimethyl-3-formyl-1,5-hexadiene of formula V: subsequently rearranging intermediate (V) thereby yielding citral product of formula I, which comprises: as the reaction proceeds, continuously distilling the reaction mixture thereby continuously removing prenol, which is formed by degradation of acetal II, and the intermediates of formula IV and V and any citral product which is formed during the reaction; and thermally rearranging said intermediates of formula IV and V at a temperature of 100-200° C. in the absence or presence of said prenol to form citral product.

    摘要翻译： 通过以下方式连续制备式I的3,7-二甲基-2,6-辛二烯-1-醇：在存在或不存在酸催化剂的情况下，热裂解3-甲基-2-丁烯-1-al阮内烯 式II：由此除去式III的3-甲基-2-丁烯-1-醇，得到式IV的顺/反 - 异戊烯基3-甲基丁二烯基醚：热重新排列所得的式IV的丁二烯基醚，由此得到2,4,4 式V的 - 三甲基-3-甲酰基-1,5-己二烯：随后重新排列中间体（V），从而产生式I的柠檬醛产物，其包括：随着反应的进行，连续蒸馏反应混合物，从而连续除去前醇， 由缩醛II的降解形成，以及式IV和V的中间体以及在反应期间形成的任何柠檬醛产物; 在不存在或存在所述prenol的情况下，在100-200℃的温度下热处理所述式IV和V的中间体，以形成柠檬醛产物。

    Continuous preparation of dimethylvinylcarbinol by isomerizing prenol
    5.
    发明授权
    Continuous preparation of dimethylvinylcarbinol by isomerizing prenol 失效
    通过异构化prenol连续制备二甲基乙烯基甲醇

    公开(公告)号：US06180839B2

    公开(公告)日：2001-01-30

    申请号：US09265923

    申请日：1999-03-10

    申请人： Matthias Kiefer ,  Wolfgang Siegel ,  Jörg Therre ,  Melanie Pahl ,  Werner Aquila ,  Ulrich Sch{umlaut over (a)}fer-L{umlaut over (u)}derssen

    发明人： Matthias Kiefer ,  Wolfgang Siegel ,  Jörg Therre ,  Melanie Pahl ,  Werner Aquila ,  Ulrich Sch{umlaut over (a)}fer-L{umlaut over (u)}derssen

    IPC分类号： C07C2700

    CPC分类号： C07C29/56 ,  C07C33/03

    摘要： A process is described for the continuous preparation of dimethylvinylcarbinol (DMVC) by continuously reacting prenol with the aqueous solution of a protic acid in the still or in the lower part of a rectification column while distilling off the DMVC formed in the form of an azeotropic mixture with water, which comprises a) during the reaction ensuring that as far as possible no liquid two-phase mixture forms in the reaction mixture, b) distilling off the DMVC which forms at a reflux ratio of at least 2, as a result of which there is virtually no more prenol present in the distillate from the column, and c) setting the reaction volume and/or the amount of prenol added per hour and/or the concentration of protons in the reaction mixture in such a manner that the quotient, defined as residence time concentration coefficient, of the reaction volume and the volume of prenol added per hour multiplied by the concentration of protons in the reaction mixture has a value between 0.001 h·mol/l and 1 h·mol/l. In this connection, the formation of a liquid two-phase mixture in the reaction mixture is prevented, in addition to avoiding too large a prenol excess, by continuously taking from the reaction mixture a partial stream, passing it over a phase separation vessel, completely or at least largely removing there the small quantities, formed in the course of the reaction, of organic by-products which are insoluble or only partially soluble in water, and returning the aqueous phase to the reaction volume.

    摘要翻译： 描述了通过在精馏塔的静止或下部连续地反应预先醇与质子酸的水溶液连续反应制备二甲基乙烯基甲醇（DMVC）的方法，同时蒸馏出以共沸混合物形式形成的DMVC 在反应过程中包含a）的水，确保尽可能在反应混合物中形成液体两相混合物，b）蒸发形成回流比至少为2的DMVC，结果是在那里 在柱的馏出物中基本上没有更多的prenol存在，并且c）使反应体积和/或每小时加入的prenol的量和/或反应混合物中的质子浓度设定为使得定义为 停留时间浓度系数，反应体积和每小时加入的prenol体积乘以反应混合物中质子浓度的值为0.001 h.mol / l和 1 h.mol / l。在这方面，防止反应混合物中的液体两相混合物的形成，除了避免过多的过量的过量以外，通过连续取出反应混合物的一部分流，将其通过 在相分离容器中，完全或至少大部分在反应过程中形成的少量去除不溶或仅部分溶于水的有机副产物，并将水相返回到反应体积中。

    Dividing-wall column with feed in whole or in part in the vaporous state and/or side stream take off in whole or in part in the vaporous state
    8.
    发明授权
    Dividing-wall column with feed in whole or in part in the vaporous state and/or side stream take off in whole or in part in the vaporous state 有权
    全部或部分进料在蒸发态和/或侧流中的分隔壁塔全部或部分脱气

    公开(公告)号：US07264696B2

    公开(公告)日：2007-09-04

    申请号：US11384370

    申请日：2006-03-21

    申请人： Gerd Kaibel ,  Christian Miller ,  Katrin Klaβ ,  Alois Kindler ,  Werner Aquila ,  Walter Dobler ,  Klaus Breuer ,  Achim Pommer ,  Thomas Dirnsteiner

    发明人： Gerd Kaibel ,  Christian Miller ,  Katrin Klaβ ,  Alois Kindler ,  Werner Aquila ,  Walter Dobler ,  Klaus Breuer ,  Achim Pommer ,  Thomas Dirnsteiner

    IPC分类号： B01D3/42

    CPC分类号： B01D3/141 ,  B01D3/14 ,  Y10S203/11 ,  Y10S203/20

    摘要： A dividing-wall column having a dividing wall which is essentially disposed along the long direction of the column is proposed, which divides the column interior into a feed part, a take off part, an upper shared column part and a lower shared column part, with feed in whole or in part in the vaporous state of a mixture to be separated between the upper region of the feed part and the lower region of the feed part and/or side stream take off in whole or in part in the vaporous state between the upper region of the take off part and the lower region of the take off part, where if feed is in whole or in part in the vaporous state the cross-sectional area of the upper region of the feed part is increased by plane-parallel displacement of the dividing wall toward the upper region of the take off part, and/or if the side stream take off is in whole or in part in the vaporous state, the cross-sectional area of the lower region of the take off part is increased by displacement of the dividing wall toward the lower region of the feed part, in such a manner that the F factor is substantially the same in all column regions.

    摘要翻译： 提出了具有分隔壁的分隔壁，该分隔壁基本上沿着塔的长方向设置，其将塔内部分为进料部分，脱落部分，上共享塔部分和下共享塔部分， 在进料部分的上部区域和进料部分的下部区域和/或侧馏分之间在蒸气状态下的全部或部分蒸气状态下的进料全部或部分地在蒸气状态之间分离， 取出部分的上部区域和脱落部分的下部区域，如果进料全部或部分处于气态，则进料部分的上部区域的横截面面积被平面平行地增加 分流壁向脱气部的上部区域的位移，和/或侧流的脱落全部或部分处于蒸发状态，脱落部的下部区域的截面积为 由分界位移增加 壁朝向馈送部分的下部区域，使得F因子在所有列区域中基本相同。