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    Preparation of .gamma.,.delta.-unsaturated ketones by the Carroll reaction, novel catalysts therefor and the preparation thereof
    2.
    发明授权
    Preparation of .gamma.,.delta.-unsaturated ketones by the Carroll reaction, novel catalysts therefor and the preparation thereof 失效
    通过Carroll反应制备γ，δ-不饱和酮，其新型催化剂及其制备

    公开(公告)号：US6051741A

    公开(公告)日：2000-04-18

    申请号：US168378

    申请日：1998-10-08

    申请人： Heinz Etzrodt ,  Dietmar Weller ,  Carsten Oost ,  Hagen Jaedicke ,  Manfred Stroezel ,  Bernhard Bockstiegel ,  Lothar Laupichler ,  Klaus Reimer

    发明人： Heinz Etzrodt ,  Dietmar Weller ,  Carsten Oost ,  Hagen Jaedicke ,  Manfred Stroezel ,  Bernhard Bockstiegel ,  Lothar Laupichler ,  Klaus Reimer

    IPC分类号： B01J31/02 ,  B01J31/14 ,  C07B61/00 ,  C07C45/67 ,  C07C45/68 ,  C07C49/203 ,  C07F5/06 ,  C07C45/00

    CPC分类号： C07F5/069 ,  B01J31/0211 ,  C07C45/676

    摘要： A process for preparing .gamma.,.delta.-unsaturated ketones of the general formula I ##STR1## by reacting an allyl alcohol of the general formula II ##STR2## in which R.sup.1 is H or a hydrocarbon radical having 1 to 20 carbon atoms, with diketene or an alkyl acetoacetate of the general formula III ##STR3## in which R.sup.2 is alkyl having 1 to 4 carbon atoms in an unmodified or modified Carroll reaction in the presence of an aluminum catalyst, wherein aluminum compounds which are stable liquids at room temperature, or a mixture of such aluminum compounds, which comprise at least one radical formed from an alkyl acetoacetate and 1 or 2 alkoxy radicals, or else comprise exclusively radicals formed from alkyl acetoacetates, which are esterified with sec-butanol or isobutanol, or else are esterified with at least two different alcohols, are used as aluminum catalyst. Also claimed are the novel mixtures of aluminum compounds which comprise radicals which are formed exclusively from alkyl acetoacetates and are esterified with at least two different alkanols, and the batchwise and continuous preparation of the liquid aluminum catalysts.

    摘要翻译： 通过使通式II的烯丙醇（其中R 1为H或具有1至20个碳原子的烃基）的烯丙醇与二烯酮或一般的乙酰乙酸烷基酯反应制备通式I的γ，β-不饱和酮的方法 式III其中R2是在未改性或改性的Carroll反应中在铝催化剂存在下具有1至4个碳原子的烷基，其中在室温下为稳定液体的铝化合物或这种铝化合物的混合物，其包含在 由烷基乙酰乙酸酯和1或2个烷氧基形成的至少一个基团，或者仅由烷基乙酰乙酸酯形成的由仲丁醇或异丁醇酯化的酰基或者由至少两种不同的醇酯化的基团用作铝 催化剂。 还要求的是铝化合物的新型混合物，其包含仅由乙酰乙酸烷基酯形成并且与至少两种不同的链烷醇酯化的基团，以及液体铝催化剂的分批连续制备。

    Process for preparing higher unsaturated ketones
    3.
    发明授权
    Process for preparing higher unsaturated ketones 失效
    制备高级不饱和酮的方法

    公开(公告)号：US06300524B1

    公开(公告)日：2001-10-09

    申请号：US09440281

    申请日：1999-11-15

    申请人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Udo Rheude ,  Gerd Kaibel ,  Thomas Krug ,  Luise Spiske ,  Hagen Jaedicke

    发明人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Udo Rheude ,  Gerd Kaibel ,  Thomas Krug ,  Luise Spiske ,  Hagen Jaedicke

    IPC分类号： C07C4500

    CPC分类号： C07C45/676 ,  Y02P20/582 ,  C07C49/255 ,  C07C49/203

    摘要： The present invention relates to an improved process for preparing higher unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction , in a reactor system with fitted fractionation column, wherein A the &agr;,&bgr;-unsaturated alcohol is introduced into the reaction vessel together with the organic aluminum compound in the absence of effective amounts of a solvent, and the alkyl acetoacetate is metered into this mixture, B a reaction temperature which is as constant as possible at between 175° C. and 220° C., preferably between 180° C. and 200° C., is adjusted and C during the reaction the content of alkyl acetoacetate in the reaction mixture is adjusted to a value which is as constant as possible at between 1 and 3% by weight. It is advantageous in this process for the reaction temperature defined under B to be controlled by suitable variation of the heat input and/or by variation of the rate of addition of the alkyl acetoacetate, and for adequate mixing of the reaction mixture in the reaction vessel to be ensured This can be achieved with the aid of a stirrer, by pumping the reaction mixture through an external liquid circulation, by introducing the alkyl acetoacetate by means of a mixing nozzle or else by passing in a stream of inert gas. The process according to the invention is particularly suitable for the Carroll reaction of higher alcohols such as 3,7-dimethyl-1,6-octadien-3-ol (linalool), 3,7-dimethyl-1-octen-3-ol, 3,7,11-trimethyl-1,6,10-dodecatrien-3-ol (nerolidol), 3,7,11-trimethyl-1-dodecen-3-ol or 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol).

    摘要翻译： 本发明涉及一种改进的制备高级不饱和酮的方法，该方法通过在具有合适分馏塔的反应器系统中，在卡罗尔反应中使相应的α，β-不饱和醇与烷基乙酰乙酸酯反应，其中引入α，β-不饱和醇 在没有有效量的溶剂的情况下，将有机铝化合物与有机铝化合物一起加入到反应容器中，并将乙酰乙酸烷基酯计量加入到该混合物中，B在175℃和220℃之间的反应温度尽可能恒定 在反应过程中，优选在180℃和200℃之间调节和C，将反应混合物中乙酰乙酸烷基酯的含量调节至1至3重量％之间尽可能恒定的值。 在该方法中，通过适当变化的热输入和/或通过烷基的加成速率的变化来控制在B下限定的反应温度， 乙酰乙酸酯，并使反应混合物在反应容器中充分混合以确保这可以借助于搅拌器，通过泵送反应混合物通过外部液体循环，通过引入烷基乙酰乙酸酯通过混合喷嘴 或者通过流入惰性气体流。根据本发明的方法特别适用于高级醇如3,7-二甲基-1,6-辛二烯-3-醇（芳樟醇），3， 7,7-二甲基-1-辛烯-3-醇，3,7,11-三甲基-1,6,10-十二碳三烯-3-醇（橙花叔醇），3,7,11-三甲基-1-十二碳烯-3-醇 或3,7,11-三甲基-1,6-十二碳二烯-3-醇（二氢吗啉醇）。

    Process for preparing unsaturated ketones
    4.
    发明授权
    Process for preparing unsaturated ketones 失效
    制备不饱和酮的方法

    公开(公告)号：US06307106B1

    公开(公告)日：2001-10-23

    申请号：US09440280

    申请日：1999-11-15

    申请人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Gerd Kaibel ,  Hagen Jaedicke

    发明人： Carsten Oost ,  Manfred Stroezel ,  Heinz Etzrodt ,  Dietmar Weller ,  Gerd Kaibel ,  Hagen Jaedicke

    IPC分类号： C07C4500

    CPC分类号： C07C45/68 ,  B01J19/1881 ,  B01J31/0211 ,  B01J2219/00038 ,  Y02P20/582 ,  C07C49/203

    摘要： An improved process for preparing lower unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction in the presence of from 0.1 to 5 mol %, based on the alkyl acetoacetate to be reacted, of an organic aluminum compound as catalyst with elimination and continuous removal by distillation of the alkanol eliminated during the reaction from the alkyl acetoacetate in a reactor system with a fitted fractionation column, wherein A an &agr;,&bgr;-unsaturated alcohol which boils below 140° C. is introduced, in the absence of effective amounts of a solvent, together with the organic aluminum compound into the reaction vessel, B a reaction temperature which is as constant as possible between 170° C. and 250° C. is set under elevated pressure, C at this temperature, the alkyl acetoacetate is metered into the mixture, obtained in A, of the &agr;,&bgr;-unsaturated alcohol and the organic aluminum compound, and D during the reaction the content of alkyl acetoacetate in the reaction mixture is set at a value which is as constant as possible between 0.1 and 10% by weight.

    摘要翻译： 一种改进的制备低级不饱和酮的方法，该方法通过在卡罗尔反应中使相应的α，β-不饱和醇与烷基乙酰乙酸酯在0.1至5摩尔％存在下反应的待反应的乙酰乙酸烷基酯的有机铝化合物 作为催化剂，在具有适合的分馏塔的反应器系统中通过蒸馏从乙酰乙酸烷基酯反应中消除的烷醇消除并连续除去，其中引入沸点低于140℃的α，β-不饱和醇，在 没有有效量的溶剂与有机铝化合物一起进入反应容器B中，在170℃和250℃之间的反应温度一直保持在升高的压力下，在此温度下， 将乙酰乙酸烷基酯计量加入到A，得自α，β-不饱和醇和有机铝化合物的混合物中，并且在反应期间将D 将反应混合物中乙酰乙酸烷基酯的含量设定为0.1至10重量％之间尽可能恒定的值。

    Method and device for carrying out the distillative separation of C5+ cuts
    7.
    发明授权
    Method and device for carrying out the distillative separation of C5+ cuts 有权
    用于进行C5 +切割的蒸馏分离的方法和装置

    公开(公告)号：US07169267B2

    公开(公告)日：2007-01-30

    申请号：US10380551

    申请日：2001-09-19

    申请人： Gerd Kaibel ,  Carsten Oost ,  Manfred Stroezel ,  Gerald Meyer ,  Peter Trübenbach ,  Karl-Heinz Sartor ,  Jürgen Heners

    发明人： Gerd Kaibel ,  Carsten Oost ,  Manfred Stroezel ,  Gerald Meyer ,  Peter Trübenbach ,  Karl-Heinz Sartor ,  Jürgen Heners

    IPC分类号： B01D3/14 ,  B01D3/42

    CPC分类号： B01D3/141 ,  B01D3/14 ,  B01D3/146 ,  B01D3/4238 ,  C10G7/00 ,  C10G7/02 ,  C10G7/12 ,  Y10S203/20

    摘要： A process is proposed for the separation of C5+ cuts by distillation into a low-boiler (A), a medium-boiler (B) and a high-boiler fraction (C) in one or more dividing-wall columns (TK), in which a dividing wall (T) is arranged in the longitudinal direction of the column with formation of an upper, common column region (1), a lower, common column region (6), a feed part (2, 4) with rectifying section (2) and stripping section (4), and a withdrawal part (3, 5) with rectifying section (5) and stripping section (3), with feed of the C5+ cut (A, B, C) into the central region of the feed part (2, 4), discharge of the high-boiler fraction (C) from the bottom of the column, discharge of the low-boiler fraction (A) via the top of the column, and discharge of the medium-boiler fraction (B) from the central region of the withdrawal part (3, 5), wherein the dividing ratio of the liquid reflux at the upper end of the dividing wall (T) is set in such a way that the proportion of high-boiling key components in the liquid reflux over the stripping section (3) of the withdrawal part at the upper end of the dividing wall (T) is from 10 to 80%, preferably from 30 to 50%, of the limit value allowed in the medium-boiler fraction (B), and wherein the heating power in the evaporator at the bottom of the dividing-wall column (TK) is set in such a way that the concentration of the low-boiling key components in the liquid at the lower end of the dividing wall (T) is from 10 to 80%, preferably from 30 to 50%, of the limit value allowed in the medium-boiler fraction (B).

    摘要翻译： 提出了一种通过蒸馏将C 5+ H 3馏分分离成低沸点（A），中等锅炉（B）和高锅炉馏分（C）的方法，其中一个或多个 分隔壁（TK），其中分隔壁（T）沿柱的纵向方向布置，形成上部公共列区域（1），下部公共柱区域（6），进料 具有整流部分（2）和汽提部分（4）的部分（2,4）和具有整流部分（5）和汽提部分（3）的抽出部分（3,5），其中C 5 （A，B，C）进入进料部分（2,4）的中心区域，从塔底排出高沸点馏分（C），排出低沸点 馏分（A），并且从中间部分（3,5）的中心区域排出中间锅炉馏分（B），其中在上部的液体回流的分离比例 分隔壁（T）以这样的方式设置 在分隔壁（T）的上端的取出部分的汽提段（3）上的液体回流中的高沸点关键成分的比例为10〜80％，优选为30〜50％ 在中间锅炉馏分（B）中允许的极限值，并且其中分隔壁塔（TK）底部的蒸发器中的加热功率被设定为使得低沸点关键成分 在分隔壁（T）的下端的液体中的中等锅炉馏分（B）中允许的极限值为10〜80％，优选为30〜50％。