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    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 ionones
    6.
    发明授权
    Process for preparing ionones 失效
    紫罗兰酮的制备方法

    公开(公告)号：US06288282B1

    公开(公告)日：2001-09-11

    申请号：US09567268

    申请日：2000-05-09

    申请人： Udo Rheude ,  Ulrich Hörcher ,  Dietmar Weller ,  Manfred Stroezel

    发明人： Udo Rheude ,  Ulrich Hörcher ,  Dietmar Weller ,  Manfred Stroezel

    IPC分类号： C07C4921

    CPC分类号： C07C403/16 ,  C07C2601/16

    摘要： Process for the continuous preparation of &agr;- and/or &bgr;-ionone or homologous compounds using concentrated sulfuric acid at temperatures from 20 to 90° C., in the presence of organic solvents or diluents with cooling and by subsequent termination of the reaction by hydrolysis of the reaction mixture with water or dilute sulfuric acid, wherein both the cyclization of pseudoionones and the subsequent hydrolysis of the reaction mixture are carried out in a virtually adiabatic reaction in one or more reaction mixing pump(s) which are connected in series and each of which consists essentially of a rotationally symmetrical mixing chamber formed from a peripheral wall and two end walls and of a mixing rotor made of material inert to sulfuric acid and with rotational drive, where the mixing chamber has at least one inlet opening for each component and one outlet opening for the reaction mixture, and annular channels in fluid connection to one another in the end walls, and wherein the heat of the two reactions is in each case partly or wholly removed with the aid of a downstream heat exchanger.

    摘要翻译： 使用浓硫酸在20〜90℃的温度下，在有机溶剂或稀释剂存在下，在冷却下，随后通过水解终止反应，连续制备α-和/或β-紫罗兰酮或同系化合物的方法 反应混合物与水或稀硫酸反应，其中假戊烯酮的环化和随后的反应混合物的水解在一个或多个反应混合泵中实质上绝热的反应中进行，所述反应混合泵串联连接， 其基本上由旋转对称的混合室组成，该混合室由周壁和两个端壁以及由硫酸惰性且具有旋转驱动的材料制成的混合转子，其中混合室具有用于每个部件的至少一个入口， 用于反应混合物的一个出口，以及在端壁中彼此流体连接的环形通道，其中热量 在每种情况下，两个反应在下游热交换器的帮助下部分或全部去除。

    Structured packing for heat exchange and mass transfer
    9.
    发明授权
    Structured packing for heat exchange and mass transfer 失效
    用于热交换和传质的结构填料

    公开(公告)号：US06427985B1

    公开(公告)日：2002-08-06

    申请号：US09625486

    申请日：2000-07-25

    申请人： Gerd Kaibel ,  Manfred Stroezel ,  Achim Stammer

    发明人： Gerd Kaibel ,  Manfred Stroezel ,  Achim Stammer

    IPC分类号： B01F304

    CPC分类号： F28C3/08 ,  B01J19/32 ,  B01J2219/3221 ,  B01J2219/32213 ,  B01J2219/32227 ,  B01J2219/32258 ,  B01J2219/32272 ,  B01J2219/32408 ,  B01J2219/32466 ,  Y10S261/72

    摘要： A structured packing for heat exchange and mass transfer between a liquid and a gas in a column having at least one packing layer with a first, lower end and a second, upper end is described, the packing layer having an internal geometry which varies over its height so that by suitably setting the liquid and gas flow rates in a first, in particular lower, region of the packing layer a bubbling layer having a predominantly disperse gas phase forms in a targeted manner and simultaneously in a second, in particular upper, region of the packing layer a film flow of the liquid having a predominantly continuous gas phase forms in a targeted manner.

    摘要翻译： 描述了一种用于在具有至少一个具有第一，下端和第二上端的填料层的塔中的液体和气体之间的热交换和质量传递的规整填料，所述填料层具有内部几何形状 高度，使得通过适当地将液体和气体流速设定在填料层的第一个，特别是较低的区域中，具有主要分散气相的起泡层以目标方式形成，同时在第二特别是上部区域 的填料层，以目标的方式形成具有主要连续气相的液体的膜流。

    Preparation of C10-C30-alkenes by partial hydrogenation of alkynes over fixed-bed supported palladium catalysts
    10.
    发明授权
    Preparation of C10-C30-alkenes by partial hydrogenation of alkynes over fixed-bed supported palladium catalysts 失效
    通过固定床负载的钯催化剂上的炔进行部分氢化制备C10-C30-烯烃

    公开(公告)号：US06365790B2

    公开(公告)日：2002-04-02

    申请号：US09734024

    申请日：2000-12-12

    申请人： Klaus Reimer ,  Gerd Kaibel ,  Ulrich Kammel ,  Franz Josef Bröcker ,  Andreas Ansmann ,  Heinz Etzrodt ,  Manfred Stroezel ,  Mathias Haake ,  Lothar Laupichler ,  Bernhard Bockstiegel

    发明人： Klaus Reimer ,  Gerd Kaibel ,  Ulrich Kammel ,  Franz Josef Bröcker ,  Andreas Ansmann ,  Heinz Etzrodt ,  Manfred Stroezel ,  Mathias Haake ,  Lothar Laupichler ,  Bernhard Bockstiegel

    IPC分类号： C07C2900

    CPC分类号： C07C29/17 ,  B01J23/44 ,  B01J23/50 ,  B01J35/04 ,  B01J35/06 ,  B01J37/0217 ,  B01J37/0225 ,  B01J37/08 ,  C07C5/09 ,  C07C2523/44 ,  C07C11/02 ,  C07C33/025 ,  C07C33/02

    摘要： Alkenes are prepared by partial hydrogenation of alkynes in the liquid phase at from 20 to 250° C. and hydrogen partial pressures of from 0.3 to 200 bar over fixed-bed supported palladium catalysts which are obtainable by heating the support material in the air, cooling, applying a palladium compound and, if required, additionally other metal ions for doping purposes, molding and processing to give monolithic catalyst elements, by a process in which A) alkynes of 10 to 30 carbon atoms are used as starting compounds, B) the palladium compound and, if required, the other metal ions are applied to the support material by impregnation of the heated and cooled support material with a solution containing palladium salts and, if required, other metal ions and subsequent drying, and C) from 10 to 2000 ppm of carbon monoxide (CO) are added to the hydrogenation gas or a corresponding amount of CO is allowed to form in the liquid phase by slight decomposition of a compound which is added to the reaction mixture and eliminates CO under the reaction conditions. The process is particularly advantageous if the partial hydrogenation is carried out in a tube reactor by the trickle-bed or liquid phase procedure with product recycling at cross-sectional loadings of from 20 to 500 m3/m2*h. The process is particularly suitable for the preparation of 3,7,11,15-tetramethyl-1-hexadecen-3-ol (isophytol), 3,7,11-trimethyl-l-dodecen-3-ol (tetrahydronerolidol), 3,7,11-trimethyl-1,4-dodecadien-3-ol, 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol), 3,7-dimethyloct-1,6-dien-3-ol or 3,7-dimethyloct-1-en-3-ol from the corresponding alkynes.

    摘要翻译： 烯烃通过液相中炔烃在20至250℃的部分氢化和固定床负载的钯催化剂的0.3至200巴的氢分压来制备，其可通过加热空气中的载体材料，冷却 使用钯化合物，另外还需要另外的金属离子用于掺杂目的，通过使用10-30个碳原子的炔烃作为起始化合物的方法，模塑和加工以得到整体式催化剂元素，B）钯 如果需要，另外的金属离子通过用含有钯盐的溶液浸渍加热和冷却的载体材料以及如果需要的话其它金属离子并随后干燥而被施加到载体材料上，C）为10-2000ppm 的一氧化碳（CO）加入到氢化气体中，或者相应量的CO在液相中形成，通过轻微分解添加到真空中的化合物 并且在反应条件下消除CO。如果部分氢化在管式反应器中通过滴流床或液相方法进行，则该方法是特别有利的，其中产物回收的横截面负荷为20-500m 3 / m2 * h。 该方法特别适用于制备3,7,11,15-四甲基-1-十六碳烯-3-醇（异山梨糖醇），3,7,11-三甲基-1-十二碳烯-3-醇（四氢化吗啉醇），3 ，7,11-三甲基-1,4-十二碳二烯-3-醇，3,7,11-三甲基-1,6-十二碳二烯-3-醇（二氢吗啉醇），3,7-二甲基辛-1,6-二烯 - 3-醇或3,7-二甲基辛-1-烯-3-醇。