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1. 发明授权

US06554965B1 Rectification column for isolating pure substances from high boiling air-and/or temperature sensitive substances 失效
标题翻译：用于从高沸点空气和/或温度敏感物质中分离纯物质的精馏塔
公开(公告)号：US06554965B1
公开(公告)日：2003-04-29
申请号：US09466844
申请日：1999-12-20
申请人： Horst Hartmann , Wolfram Burst , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
发明人： Horst Hartmann , Wolfram Burst , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
IPC分类号： B01D300
CPC分类号： B01D3/141 , B01D3/008 , B01D3/146 , B01D3/16 , B01J19/32 , B01J2219/3221 , B01J2219/3222 , B01J2219/32227 , B01J2219/32272 , B01J2219/32408 , B01J2219/32416 , B01J2219/326 , C07C17/38 , C07D311/72 , Y10S159/42 , Y10S261/72
摘要： A reflection column which contains liquid distributors having at least 500 drip points/m2, which are arranged at an angle of about 90° C. to cloth layers of packing elements located immediately therebelow; and a combination of insulation and protective heating. The column is advantageously used for the rectification of mixtures of high-boiling air- or temperature-sensitive substances requiring effective separation efficiency.
摘要翻译：一种反射柱，其包含具有至少500个滴点/ m 2的液体分配器，其以约90℃的角度布置在紧邻其下方的包装元件的布层; 并结合绝缘和保护加热。该柱有利地用于需要有效分离效率的高沸点空气或温度敏感物质的混合物的精馏。

2. 发明授权

US6111117A Process for isolation of pure substances from mixtures of high-boiling air and/or temperature-sensitive substances which require a high separation efficiency by rectification under medium vacuum, and columns suitable for this process 失效
标题翻译：从高沸点空气和/或温度敏感物质的混合物中分离纯物质的方法，这些物质需要通过在中等真空下进行精馏才能获得高分离效率，以及适用于该方法的色谱柱
公开(公告)号：US6111117A
公开(公告)日：2000-08-29
申请号：US981491
申请日：1998-01-08
申请人： Horst Hartmann , Wolfram Burst , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
发明人： Horst Hartmann , Wolfram Burst , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
IPC分类号： B01D3/00 , B01D3/10 , B01D3/14 , B01D3/16 , B01D3/26 , B01D3/32 , B01J19/32 , C07C17/38 , C07D311/72
CPC分类号： B01D3/141 , B01D3/008 , B01D3/146 , B01D3/16 , B01J19/32 , C07C17/38 , C07D311/72 , B01J2219/3221 , B01J2219/3222 , B01J2219/32227 , B01J2219/32272 , B01J2219/32408 , B01J2219/32416 , B01J2219/326 , Y10S159/42 , Y10S261/72
摘要： Process for isolating pure substances from of mixtures of high-boiling air- and/or temperature-sensitive substances which require a high separation efficiency, by rectification under medium vacuum in columns containing metal cloth packings with ordered structure using channel liquid distributors with 500 or more drip points/m.sup.2, which are arranged at an angle of 90.degree. to the cloth layers of the packing elements located immediately below the distributors, in which two or more of the packing elements underneath the liquid distributors have only a very small height, which ensure virtual exclusion of air and are designed so that no heat exchange through the column wall can take place during the rectification. The patent also relates to packed columns which can be used for this process and to the use of this process and these columns for the final purification of vitamin E acetate by distillation.
摘要翻译： PCT No.PCT / EP96 / 02852 Sec。 371日期1998年1月8日 102（e）1998年1月8日PCT PCT 1996年6月29日PCT公布。出版物WO97 / 02880 日期1997年1月30日从需要高分离效率的高沸点空气和/或温度敏感物质的混合物中分离纯物质的过程，通过在含有有序结构的金属布填料的柱中在中等真空下进行精馏，使用通道液具有500个或更多滴点/ m2的分配器，其布置成与位于分配器正下方的包装元件的布层成90°的角度，其中液体分配器下方的两个或更多个包装元件仅具有非常小高度，确保虚拟排除空气，并设计成在整流期间不会通过柱壁进行热交换。该专利还涉及可用于该方法的填充柱和该方法的使用，并且这些柱用于通过蒸馏最终纯化维生素E乙酸酯。

3. 发明授权

US5950454A Cloth or cloth-like packing which is subject to low pressure losses and has an ordered structure for use in material-exchange columns and rectification method using such packing 失效
标题翻译：承受低压损失的布或布状包装，具有用于材料交换柱的有序结构和使用这种包装的精馏方法
公开(公告)号：US5950454A
公开(公告)日：1999-09-14
申请号：US973875
申请日：1998-01-07
申请人： Wolfram Burst , Horst Hartmann , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
发明人： Wolfram Burst , Horst Hartmann , Wulf Kaiser , Harald Laas , Paul Grafen , Bernhard Bockstiegel , Kai-Uwe Baldenius
IPC分类号： B01D3/00 , B01D3/10 , B01D3/14 , B01D3/16 , B01D3/26 , B01D3/32 , B01D53/86 , B01D53/94 , B01J19/32 , B01J23/63 , B01J23/656 , B01J23/89 , C07C17/38 , C07D311/72 , B01D47/00
CPC分类号： B01J23/8913 , B01D3/008 , B01D3/141 , B01D3/146 , B01D3/16 , B01D53/864 , B01D53/8659 , B01D53/8662 , B01D53/8668 , B01J19/32 , B01J23/63 , B01J23/6562 , C07C17/38 , C07D311/72 , B01D2255/102 , B01D2255/20715 , B01D2257/2062 , B01J2219/3221 , B01J2219/3222 , B01J2219/32227 , B01J2219/32272 , B01J2219/32408 , B01J2219/32416 , B01J2219/326 , Y02P20/154 , Y10S62/906
摘要： Packing elements with a low pressure drop for mass transfer column internals of the internal diameter of the column and of a height of from 40 to 300 mm made of dimensionally stable layers, which have an ordered structure and are in mutual contact, of cloth material or cloth-like material with a specific surface area of from 100 to 2000 m.sup.2 /m.sup.3, whereina) the shaped layers of cloth material or cloth-like material, preferably made of metal cloth, which are in mutual contact are arranged so that they form a multiplicity of narrow flow channels, preferably virtually triangular, virtually rectangular or else virtually equilateral hexagonal flow channels, in which the angle of inclination of the serration of the individual cloth layers of the packing to the column axis is only 0 to 25.degree., preferably 3 to 14.degree., andb) to ensure mechanical stability of the packing elements, if necessary wires or thin rods are fixed in suitable arrangement between the cloth layers, or else the cloth layers are firmly connected at some points of contact, and processes for obtaining pure substances from substance mixtures by rectification using the novel packing elements.
摘要翻译： PCT No.PCT / EP96 / 02851 Sec。 371日期：1998年1月7日 102（e）1998年1月7日PCT PCT 1996年6月29日PCT公布。出版物WO97 / 02890 日期1997年1月30日对于具有有序结构并且相互接触的由尺寸稳定的层制成的用于内部直径的柱的内径的质量传递柱内部和40至300mm的高度的低压降的元件的比表面积为100〜2000m 2 / m 3的布料或布状材料，其中a）相互接触的优选由金属布制成的布料或布状材料的成形层是排列成使得它们形成多个窄流动通道，优选实际上为三角形，实质上为矩形或虚拟的等边六边形流动通道，其中填料的单个布层与柱轴线的锯齿形倾斜角仅为0° 至25°，优选3至14°，以及b）确保包装元件的机械稳定性，如有必要，线或细杆以合适的布置固定在布层之间，或els 布层在某些接触点处牢固连接，并且通过使用新的包装元件通过整流从物质混合物中获得纯物质的过程。

4. 发明授权

US6005122A Preparation of .alpha.-tocopherol or .alpha.-tocopheryl acetate by reacting trimethylhydroquinone and phytol or isophytol, with recycling of the zinc halide condensation catalyst 失效
标题翻译：通过三甲基对苯二酚和植物醇或异植醇反应制备α-生育酚或α-生育酚乙酸酯，再加上卤化锌缩合催化剂
公开(公告)号：US6005122A
公开(公告)日：1999-12-21
申请号：US990092
申请日：1997-12-12
申请人： Kai-Uwe Baldenius , Wulf Kaiser , Bernhard Bockstiegel , Harald Laas , Bernhard Schulz , Peter Schmitt , Helmut Glietenberg
发明人： Kai-Uwe Baldenius , Wulf Kaiser , Bernhard Bockstiegel , Harald Laas , Bernhard Schulz , Peter Schmitt , Helmut Glietenberg
IPC分类号： B01J27/138 , C07D311/72
CPC分类号： C07D311/72 , B01J27/138
摘要： A process for preparing .alpha.-tocopherol or .alpha.-tocopheryl acetate by reacting 2,3,5-trimethylhydroquinone with isophytol or phytol in the presence of a zinc halide condensation catalyst and a proton donor in a solvent with or without subsequent esterification with acetic anhydride, which comprisesA. carrying out the reaction in a nonpolar solvent which is only slightly water-miscible, if at all andB. introducing the required zinc halide into the reaction in the form of a mixture of from 1 to 4 mol of water per mol of zinc halide.The possibility of introducing the zinc halide required in the process according to the invention in the form of a mixture of zinc halide and water which can be readily handled and metered at from 50 to 200.degree. C. without impairing the yield and purity of the tocopherol opens the way to an advantageous recycling of the zinc halide after the reaction by separating off or extracting and recycling the zinc halide in the form of a from 60 to 90% strength by weight solution or pumpable magma.
摘要翻译：在卤化锌缩合催化剂和质子供体存在下，使2,3,5-三甲基氢醌与异麦芽糖醇或植物醇在溶剂中反应制备α-生育酚或α-生育酚乙酸酯的方法，其中或不用随后用乙酸酐酯化，其包括A.在非极性溶剂中进行反应，所述非极性溶剂仅仅是轻微的水混溶性的，如果有的话，则B.将所需的卤化锌以每摩尔1至4摩尔水的混合物的形式引入反应中的卤化锌。将本发明方法中所需的卤化锌以卤化锌和水的混合物的形式引入卤化物的可能性，其可以在50-200℃下容易地处理和计量，而不损害生育酚的产率和纯度打开通过分离或提取和重新使用60至90％重量浓度的溶液或可泵送岩浆形式的卤化锌，从而在反应之后有效地再循环卤化锌。

5. 发明授权

US5994589A Process for preparing 2,5,6-trimethyl-2-cyclohexen-1-one 失效
标题翻译：制备2,5,6-三甲基-2-环己烯-1-酮的方法
公开(公告)号：US5994589A
公开(公告)日：1999-11-30
申请号：US265695
申请日：1999-03-10
申请人： Detlef Ruff , Wolfram Burst , Wulf Kaiser , Manfred Stroezel
发明人： Detlef Ruff , Wolfram Burst , Wulf Kaiser , Manfred Stroezel
IPC分类号： C07C45/72 , C07C45/74 , C07C49/603 , C07C45/75
CPC分类号： C07C45/74
摘要： A process for preparing 2,5,6-trimethyl-2-cyclohexen-1-one by reacting diethyl ketone with crotonaldehyde or a compound which is converted under the chosen reaction conditions into crotonaldehyde, in the presence of basic agents at elevated temperature, which comprisesa) simultaneously pumping one mole of crotonaldehyde or one mole of a compound which is converted under the reaction conditions into crotonaldehyde, about 5 to 30 moles of diethyl ketone and the aqueous solution or suspension of a strong base, through separate lines or at least partly in the form of a suitable mixture, continuously into a pressure vessel, which is heated where appropriate and which ensures vigorous mixing, in such a way thatb) the reaction temperature is between 150.degree. C. and 350.degree. C., and the average residence time in the pressure vessel is only about 0.1 second to 20 minutes.
摘要翻译：一种通过使二乙基酮与巴豆醛或在选择的反应条件下转化成巴豆醛的化合物在高温下在碱性试剂存在下制备2,5,6-三甲基-2-环己烯-1-酮的方法，包括a）同时泵送一摩尔巴豆醛或1摩尔在反应条件下转化为巴豆醛的化合物，约5至30摩尔二乙基酮和强碱的水溶液或悬浮液，通过分开的管线或至少部分以合适混合物的形式，连续地进入压力容器，其在适当时被加热并且确保剧烈混合，使得b）反应温度在150℃和350℃之间，并且在压力容器中的平均停留时间仅为约0.1秒至20分钟。

6. 发明授权

US06184420B2 Preparation of unsaturated ketones 失效
标题翻译：不饱和酮的制备
公开(公告)号：US06184420B2
公开(公告)日：2001-02-06
申请号：US09150925
申请日：1998-09-10
申请人： Joaquim Henrique Teles , Norbert Rieber , Klaus Breuer , Dirk Demuth , Hartmut Hibst , Stefan Kaeshammer , Heinz Etzrodt , Wulf Kaiser
发明人： Joaquim Henrique Teles , Norbert Rieber , Klaus Breuer , Dirk Demuth , Hartmut Hibst , Stefan Kaeshammer , Heinz Etzrodt , Wulf Kaiser
IPC分类号： C07C49203
CPC分类号： C07C45/513 , Y02P20/582 , C07C49/203
摘要： Unsaturated ketones of the formulae Ia and Ib are prepared by a process consisting of the combination of the following reactions: a) The conventional reaction of an allyl alcohol of the formula IIa or a propargyl alcohol of the formula IIb with an isopropenyl ether of the formula III with formation of a ketal of the formula IV as a byproduct, b) preparation of the isopropenyl ether of the formula III by reacting a ketal of the formula IV with propyne or allene, or a mixture thereof in the gas phase at elevated temperatures in the presence of a heterogeneous catalyst containing zinc or cadmium together with silicon or oxygen, and c) feeding the ketal of the formula IV formed in the reaction (a) into stage (b) for the preparation of the isopropenyl ether of the formula III again.
摘要翻译：式Ia和Ib的不饱和酮通过由以下反应的组合组成的方法制备：a）式IIa的烯丙醇或式IIb的炔丙醇与式III的异丙烯基醚的常规反应，形成的式I的缩酮化合物是一种副产物，b）通过使式IV的缩酮与丙炔或丙烯或其混合物在升高的温度下在存在下进行反应来制备式III的异丙烯基醚含有锌或镉以及硅或氧的非均相催化剂，和c）将反应（a）中形成的式IV的缩酮进料到步骤（b）中，以再次制备式III的异丙烯基醚。

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