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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

US5041572A Preparation of 2,3,5-trimethyl-p-benzoquinone 失效
标题翻译：制备2,3,5-三甲基 - 对苯醌
公开(公告)号：US5041572A
公开(公告)日：1991-08-20
申请号：US493103
申请日：1990-03-13
申请人： Ulrich Hoercher , Barbara Jessel , Bernhard Bockstiegel , Paul Grafen , Harald Laas
发明人： Ulrich Hoercher , Barbara Jessel , Bernhard Bockstiegel , Paul Grafen , Harald Laas
IPC分类号： B01J27/122 , C07B61/00 , C07C46/08 , C07C50/02
CPC分类号： C07C46/08
摘要： 2,3,5-Trimethyl-p-benzoquinone is prepared by oxidation of trimethylphenol with oxygen or an oxygen-containing gas in the presence of a catalyst containing a copper(II) halide in a two-phase reaction medium consisting of water and an aliphatic alcohol at elevated temperatures by a process in which the reaction is carried out in a mixture of water and a saturated aliphatic alcohol of 12 to 18 carbon atoms, having a flashpoint greater than 120.degree. C., such as 1-dodecanol, 1-tetradecanol, 1-hexadecanol or 1-octadecanol, in particular 1-dodecanol, and at from 60.degree. to 100.degree. C.Particularly good yields of TMQ are obtained if the reaction is carried out in the presence of a copper(II) halide, such as CuCl.sub.2 or CuBr.sub.2, and of an alkaline earth metal halide, in particular CaCl.sub.2 or MgCl.sub.2, or of an alkali metal halide, in particular LiCl or NaCl, as the catalyst system.
摘要翻译：通过在含有卤化铜（II）的催化剂存在下，用氧或含氧气体氧化三甲基苯酚，制备2,3,5-三甲基对苯醌，所述两相反应介质由水和脂族醇在高温下通过反应在水和12至18个碳原子的饱和脂族醇的混合物中进行的方法进行，其闪点大于120℃，如1-十二醇，1- 十四烷醇，1-十六烷醇或1-十八烷醇，特别是1-十二烷醇，以及60-100℃。如果反应在卤化铜（II）存在下进行，则得到特别好的收率的TMQ，例如CuCl 2或CuBr 2，以及碱土金属卤化物，特别是CaCl 2或MgCl 2，或碱金属卤化物，特别是LiCl或NaCl，作为催化剂体系。

6. 发明授权

US4600799A Preparation of trimethylhydroquinone 失效
标题翻译：三甲基氢醌的制备
公开(公告)号：US4600799A
公开(公告)日：1986-07-15
申请号：US699194
申请日：1985-02-07
申请人： Franz J. Broecker , Peter Tavs , Harald Laas , Wolf-Karlo Aders
发明人： Franz J. Broecker , Peter Tavs , Harald Laas , Wolf-Karlo Aders
IPC分类号： C07C37/07
CPC分类号： C07C37/07
摘要： 2,3,6-Trimethylhydroquinone is prepared by catalytic hydrogenation of 2,3,6-trimethylquinone with hydrogen in the presence of a solvent by a continuous process in which the reaction is carried out over a platinum/alumina catalyst.
摘要翻译： 2,3,6-三甲基氢醌通过在溶剂存在下用氢气将2,3,6-三甲基醌催化氢化，其中反应在铂/氧化铝催化剂上进行的连续方法制备。

7. 发明授权

US4538009A Preparation of substituted phenols 失效
标题翻译：取代苯酚的制备
公开(公告)号：US4538009A
公开(公告)日：1985-08-27
申请号：US599574
申请日：1984-04-12
申请人： Norbert Goetz , Harald Laas , Peter Tavs , Leopold Hupfer , Karl Baer
发明人： Norbert Goetz , Harald Laas , Peter Tavs , Leopold Hupfer , Karl Baer
IPC分类号： C07C37/055 , B01J23/00 , B01J23/42 , B01J23/44 , B01J23/58 , B01J23/60 , B01J23/89 , C07B61/00 , C07C27/00 , C07C37/06 , C07C37/07 , C07C39/06 , C07C67/00
CPC分类号： C07C37/07 , B01J23/005 , B01J23/58 , B01J23/60 , B01J23/89 , C07C37/06
摘要： Substituted phenols of the general formula I ##STR1## where R.sup.1, R.sup.2, R.sup.3, R.sup.4 and R.sup.5 are each hydrogen or an aliphatic or aromatic hydrocarbon radical, are prepared by dehydrogenating a cyclic alcohol of the general formula II ##STR2## or a cyclic ketone of the general formula III ##STR3## where one of the broken lines can be an additional C-C bond, in the gas phase at from 150.degree. to 380.degree. C. over a supported noble metal catalyst, by a process in which the dehydrogenation catalyst used is palladium or platinum on an aluminum spinel carrier, in particular an aluminum spinel which has a BET specific surface area of from 5 to 150 m.sup.2 /g or, for the dehydrogenation of cyclohexenones, preferably from 10 to 50 m.sup.2 /g. Particularly suitable aluminum spinels are those which, in addition to aluminum, contain magnesium, zinc, cobalt or nickel.In the novel process, substituted phenols are obtained in high yields and selectivities, and the catalyst has an extremely long life without a significant decrease in activity.
摘要翻译：通式Ⅰ的取代的酚Ⅰ，其中R 1，R 2，R 3，R 4和R 5各自为氢或脂族或芳族烃基，通过将通式II II的环醇脱氢或环状酮，其中一条虚线可以是额外的CC键，在负载型贵金属催化剂的150〜380℃的气相中，其中，所用的脱氢催化剂是钯尖晶石载体上的钯或铂，特别是BET比表面积为5〜150m 2 / g的尖晶石，或者环己烯酮的脱氢优选为10〜50m2 / g。特别合适的铝尖晶石是除了铝之外还含有镁，锌，钴或镍的铝尖晶石。在新方法中，以高产率和选择性获得取代的酚，并且催化剂具有极长的寿命而没有显着降低活性。

8. 发明授权

US06784303B2 Method for continuously acylating chromanol ester derivatives 失效
标题翻译：连续酰化色氨酸酯衍生物的方法
公开(公告)号：US06784303B2
公开(公告)日：2004-08-31
申请号：US10416468
申请日：2003-05-12
申请人： Carsten Oost , Gerd Kaibel , Harald Laas , Peter Schmitt , Jens von Erden
发明人： Carsten Oost , Gerd Kaibel , Harald Laas , Peter Schmitt , Jens von Erden
IPC分类号： C07D31176
CPC分类号： C07D311/72 , B01D1/22 , B01D3/009 , B01D3/146 , B01D3/322 , Y02P20/127
摘要： A process is described for continuously preparing chromanol ester derivatives, in particular for continuously preparing carboxylic esters of tocopherols and tocotrienols by continuous acylation with carboxylic acids or carboxylic anhydrides.
摘要翻译：描述了连续制备色甘醇酯衍生物的方法，特别是通过用羧酸或羧酸酐连续酰化连续制备生育酚和生育三烯酚的羧酸酯。

9. 发明授权

US06365758B1 Preparation of tocopheral carboxylates or tocotrienyl esters by acid-catalyzed reaction with carboxylic acids 失效
标题翻译：通过与羧酸的酸催化反应制备生育酚羧酸酯或生育三烯基酯
公开(公告)号：US06365758B1
公开(公告)日：2002-04-02
申请号：US09013813
申请日：1998-01-26
申请人： Joanna Linda von dem Bussche-Hünnefeld , Hagen Jaedicke , Guido Harms , Harald Laas
发明人： Joanna Linda von dem Bussche-Hünnefeld , Hagen Jaedicke , Guido Harms , Harald Laas
IPC分类号： C07D31104
CPC分类号： C07D311/72
摘要： A process for preparing tocopheryl esters or tocotrienyl esters by acid-catalyzed esterification of a tocopherol or a tocotrienol in a solvent while stirring at elevated temperature, which comprises a) carrying out the esterification with the appropriate carboxylic acid, b) carrying out the esterification with from 2.5 to 6 mol of the carboxylic acid in an aliphatic, cycloaliphatic or aromatic hydrocarbon boiling in the range from 80 to 200° C., or else with from 1.0 to 2.5 mol of the carboxylic acid in a mixture consisting of an aliphatic or cycloaliphatic hydrocarbon boiling in the range from 80 to 200° C. and a cyclic carbonate of the formula II or a &ggr;-lactone of the formula III where R1, R2 and R3 are each H or lower alkyl, and R4 is H, lower alkyl, phenyl or methoxymethyl, as solvent, c) using a nonoxidizing strong inorganic or organic acid, preferably sulfuric acid, boroxalic acid or benzene- or toluenesulfonic acids, in catalytic amounts as acid catalyst, and d) continuously removing the water formed in the reaction by azeotropic distillation during the reaction.
摘要翻译：一种在高温下搅拌下在溶剂中通过酸催化酯化生育酚或生育三烯酚制备生育酚酯或生育三烯基酯的方法，该方法包括a）用合适的羧酸进行酯化，b）进行酯化反应在80至200℃范围内沸腾的脂肪族，脂环族或芳族烃中的羧酸为2.5至6摩尔，或者由脂族或脂环族烃组成的混合物中的1.0至2.5摩尔羧酸沸程在80至200℃的范围内，和式II的环状碳酸酯或式III的γ-内酯，其中R 1，R 2和R 3各自为H或低级烷基，且R 4为H，低级烷基，苯基或甲氧基甲基，作为溶剂，c）使用非氧化的强无机或有机酸，优选硫酸，硼酸或苯或甲苯磺酸，催化量为酸催化剂，并且d）连续重新在反应期间通过共沸蒸馏移动反应中形成的水。

10. 发明授权

US4255333A Preparation of indolenines 失效
标题翻译：吲哚宁的制备
公开(公告)号：US4255333A
公开(公告)日：1981-03-10
申请号：US7773
申请日：1979-01-30
申请人： Hans-Joachim Opgenorth , Horst Scheuermann , Harald Laas , Axel Nissen
发明人： Hans-Joachim Opgenorth , Horst Scheuermann , Harald Laas , Axel Nissen
IPC分类号： C07D209/08 , C07C119/10
CPC分类号： C07D209/08
摘要： A process for the preparation of an indolenine of the formula ##STR1## where R, X and Y are conventional substituents, by thermal rearrangement of a compound of the formula ##STR2## to give a compound of the formula ##STR3## and cyclization of this compound in the presence of an acid catalyst.
摘要翻译：制备式“IMAGE”的吲哚宁的方法，其中R，X和Y是常规取代基，通过下式化合物的热重排，得到式IMA的化合物，并将其环化化合物在酸催化剂存在下。

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