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1. 发明授权

US4206153A Treatment of methanolic-aqueous residues from syntheses employing triphenylphosphonium salts 失效
标题翻译：使用三苯基鏻盐从合成处理甲醇 - 水残余物
公开(公告)号：US4206153A
公开(公告)日：1980-06-03
申请号：US969665
申请日：1978-12-15
申请人： Paul Grafen , Hans-Ulrich Scholz , Bernhard Schulz
发明人： Paul Grafen , Hans-Ulrich Scholz , Bernhard Schulz
IPC分类号： C07C29/76 , C07C27/00 , C07C29/80 , C07C29/84 , C07C31/04 , C07C43/30 , C07C67/00 , C07C401/00 , C07C403/00 , C07C403/08 , C07C403/12 , C07F9/53
CPC分类号： C07C403/12 , C07C29/84 , C07F9/5325 , C07C2101/16
摘要： A process for treating residues which result from the Wittig synthesis of olefins and which consist principally of methanol, triphenylphosphine oxide, salts and organic by-products, by steam-stripping the volatile constituents, with partial condensation of the steam, and separating the resulting aqueous-organic mixture at 80.degree.-100.degree. C. into a saline aqueous phase and an organic phase containing principally triphenylphosphine oxide. Using this process provides a simple method of freeing, from triphenylphosphine oxide and other organic impurities, the effluent from syntheses which result in the formation of triphenylphosphine oxide, and thereby on the one hand substantially facilitates the purification of the effluent and on the other hand provides a simple method of recovering the triphenylphosphine oxide. The latter compound, which is easily purified by distillation or recrystallization, can then be used, for example, to prepare the triphenylphosphine required for Wittig syntheses or to prepare the triphenylphosphine dichloride required for the synthesis of pesticides.
摘要翻译：用于处理由Wittig合成烯烃产生的残余物的方法，其主要由甲醇，三苯基氧化膦，盐和有机副产物组成，通过汽提汽提挥发性成分，蒸汽部分冷凝，并将所得水溶液 - 有机混合物在80°-100℃下进入盐水水相和主要含有三苯基氧化膦的有机相。使用该方法提供了从三苯基氧化膦和其它有机杂质释放导致形成三苯基氧化膦的合成流出物的简单方法，从而一方面大大有利于流出物的纯化，另一方面提供回收三苯基氧化膦的简单方法。然后可以通过蒸馏或重结晶容易地纯化的后者化合物，例如，制备Wittig合成所需的三苯基膦或制备合成农药所需的三苯基膦二氯化物。

2. 发明授权

US4519961A Production of dry powders of substances which are sensitive to oxidation 失效
标题翻译：生产对氧化敏感的物质的干粉
公开(公告)号：US4519961A
公开(公告)日：1985-05-28
申请号：US413085
申请日：1982-08-30
申请人： Horst Schumacher , Paul Grafen
发明人： Horst Schumacher , Paul Grafen
IPC分类号： A61K9/14 , A23L1/00 , A23L1/302 , A23P1/04 , A23P1/06 , A61K9/16 , A61J5/00 , B01J13/02 , B05D7/00
CPC分类号： A61K9/1658 , A23L33/15 , A23P10/30 , A23P10/43 , A61K9/1694 , A61K9/1623 , A61K9/1652
摘要： A process for pulverizing substances which are sensitive to oxidation, in particular oily substances, by dispersing oil-soluble substances, e.g. vitamins, carotinoids, pharmaceutically active compounds or aromas, in an aqueous solution of a film-forming colloid, which constitutes the continuous phase of the dispersion, with the addition of one or more substances from the group comprising the mono-, di- and polysaccharides, atomizing the dispersion, in a spray tower, in the presence of a spraying assistant and collecting the resulting particles in a fluidized bed, wherein, as the spraying auxiliary, a hydrophobic silica or a metal salt of a higher fatty acid is introduced above the fluidized bed and distributed uniformly in the spraying space, at a temperature at which the colloid of the atomized particles has not yet solidified, and the assistant-laden particles, colloid material of which essentially has not yet gelatinized, is collected in a fluidized bed, and dried therein in a conventional manner.
摘要翻译：通过分散油溶性物质，例如粉碎对氧化敏感的物质，特别是油性物质的方法。维生素，类胡萝卜素，药物活性化合物或香气，在构成分散体的连续相的成膜胶体的水溶液中，加入一种或多种包含单糖，二糖和多糖的物质，在喷雾塔中，在喷雾助剂的存在下雾化分散体，并将所得颗粒收集在流化床中，其中，作为喷雾助剂，将疏水性二氧化硅或高级脂肪酸的金属盐引入到流化床，并且在雾化颗粒的胶体尚未固化的温度下均匀地分布在喷雾空间中，并且其主要尚未凝胶化的助粘剂颗粒（其胶体材料基本上尚未凝胶化）被收集在流化床中，并以常规方式在其中干燥。

3. 发明授权

US4191692A Manufacture of tocopherol 失效
标题翻译：生育酚生产
公开(公告)号：US4191692A
公开(公告)日：1980-03-04
申请号：US896479
申请日：1978-04-14
申请人： Paul Grafen , Henning Kroesche , Bernhard Schulz , Joachim Paust , Sigberg Pfohl
发明人： Paul Grafen , Henning Kroesche , Bernhard Schulz , Joachim Paust , Sigberg Pfohl
IPC分类号： C07D311/72
CPC分类号： C07D311/72
摘要： In the manufacture of tocopherol (vitamin E) by reaction of isophytol with trimethylhydroquinone in the presence of zinc chloride and acid in a hydrocarbon solvent one of the starting compounds, isophytol, is pretreated with small amounts of ammonia or an amine.Tocopherol is obtained in higher yield and purity.
摘要翻译：在氯化锌和酸在烃溶剂存在下，通过异山梨醇与三甲基对苯二酚的反应制造生育酚（维生素E），其中一种起始化合物异山梨醇，用少量的氨或胺进行预处理。以更高的产率和纯度获得生育酚。

4. 发明授权

US4182731A Preparation of aqueous solutions or fine aqueous dispersions of polyenyltriarylphosphonium salts 失效
标题翻译：多烯基三芳基鏻盐的水溶液或细水分散体的制备
公开(公告)号：US4182731A
公开(公告)日：1980-01-08
申请号：US912356
申请日：1978-06-05
申请人： Bernhard Schulz , Paul Grafen , Hans-Ulrich Scholz , Hans Grassner , Werner Reif
发明人： Bernhard Schulz , Paul Grafen , Hans-Ulrich Scholz , Hans Grassner , Werner Reif
IPC分类号： C07F9/54
CPC分类号： C07C403/24 , C07F9/5428 , C07F9/5442
摘要： Aqueous solutions of polyenyltriarylphosphonium salts are prepared from solutions of the corresponding polyenyltriarylphosphonium salts in organic solvents by driving off the solvent with steam, part of the steam being allowed to condense. Some of the said triarylphosphonium salts may be used directly as pesticides while others are used as intermediates for organic syntheses, especially in the carotinoid field.
摘要翻译：聚烯丙基三芳基鏻盐的水溶液由相应的多烯基三芳基鏻盐在有机溶剂中的溶液通过用蒸汽驱除溶剂，一部分蒸汽被冷凝来制备。所述三芳基鏻盐中的一些可以直接用作杀虫剂，而其它的用作有机合成的中间体，特别是在类胡萝卜素领域。

5. 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。

6. 发明授权

US5290567A Pulverulent products composed of a water-insoluble core substance and of a protective covering 失效
标题翻译：由水不溶性核心物质和保护性覆盖物组成的粉状产品
公开(公告)号：US5290567A
公开(公告)日：1994-03-01
申请号：US894126
申请日：1992-06-04
申请人： Joachim U. Schneider , Gerhard Schwarz , Paul Grafen , Wolfgang Bewert , Horst Schumacher
发明人： Joachim U. Schneider , Gerhard Schwarz , Paul Grafen , Wolfgang Bewert , Horst Schumacher
IPC分类号： A61J3/02 , A23P1/04 , A61K9/16 , A61K9/36 , B01J2/00 , B01J2/04 , B01J13/04 , B01J13/12 , A61K9/14
CPC分类号： A61K9/1658 , A61K9/1611 , A61K9/1652 , B01J13/043
摘要： Pulverulent products composed of a water-insoluble core substance and of a protective covering, are obtainable bydispersing the core substance in an aqueous solution of amylose or a starch with an amylose content of more than 40% by weight as film-forming polymer for the protective covering,spraying this dispersion using hydrophobic silica as auxiliary andsubsequently drying the sprayed particles.
摘要翻译：通过将核心物质分散在直链淀粉含量大于40重量％的直链淀粉或淀粉的水溶液中，作为成膜聚合物，可以获得由水不溶性核心物质和保护性覆盖物组成的粉状产物使用疏水性二氧化硅作为助剂喷雾该分散体，随后干燥喷雾的颗粒。

7. 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。

8. 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。

9. 发明授权

US5523420A Preparation of alpha-tocopherol and alpha-tocopheryl acetate in liquid or supercritical carbon dioxide 失效
标题翻译：在液体或超临界二氧化碳中制备α-生育酚和乙酸α-生育酚
公开(公告)号：US5523420A
公开(公告)日：1996-06-04
申请号：US439762
申请日：1995-05-12
申请人： Rainer Lowack , Joachim Meyer , Manfred Eggersdorfer , Paul Grafen
发明人： Rainer Lowack , Joachim Meyer , Manfred Eggersdorfer , Paul Grafen
IPC分类号： C07B61/00 , C07D311/72
CPC分类号： C07D311/72 , Y02P20/544
摘要： A process for preparing .alpha.-tocopherol or tocopheryl acetate by cyclocondensation of trimethylhydroquinone with phytol or isophytol in the presence of an acid catalyst and of a solvent and, where appropriate, subsequent acetylation, which comprises carrying out the cyclocondensation and, where appropriate, the subsequent acetylation in liquid or supercritical carbon dioxide as solvent.
摘要翻译：在酸催化剂和溶剂的存在下，以及适当的情况下，随后的乙酰化反应，由三甲基对苯二酚与植物醇或异戊醇共环化缩合制备α-生育酚或生育酚乙酸酯的方法，其中包括进行环缩合，在液体或超临界二氧化碳中的乙酰化作为溶剂。

10. 发明授权

US5468883A Preparation of vitamin E 失效
标题翻译：维生素E的制备
公开(公告)号：US5468883A
公开(公告)日：1995-11-21
申请号：US302743
申请日：1994-09-09
申请人： Paul Grafen , Hans Kiefer , Hagen Jaedicke
发明人： Paul Grafen , Hans Kiefer , Hagen Jaedicke
IPC分类号： B01J31/04 , C07B61/00 , C07D311/72
CPC分类号： C07D311/72
摘要： A process for preparing dl-.alpha.-tocopherol or dl-.alpha.-tocopheryl acetate by acid-catalyzed reaction of 2,3,5-trimethylhydroquinone (TMH) with phytol or isophytol in a solvent at elevated temperature, with or without subsequent esterification of the resulting tocopherol with acetic anhydride, entails the reaction being carried out in the presence of a mixture of ortho-boric acid and certain aliphatic di- or tricarboxylic acids, preferably in the presence of a mixture of ortho-boric acid and oxalic acid.
摘要翻译： PCT No.PCT / EP93 / 00498 Sec。 371日期1994年9月9日 102（e）1994年9月9日PCT 1993年3月5日PCT公布。第WO93 / 19057号公报日本1993年9月30日。一种通过2,3,5-三甲基氢醌（TMH）与植物醇或异植醇在溶剂中在升高的温度下酸催化反应制备dl-α-生育酚或dl-α-生育酚乙酸酯的方法，随着或不用所得到的生育酚与乙酸酐的酯化反应，需要在邻 - 硼酸和某些脂肪族二 - 或三羧酸的混合物存在下进行反应，优选在邻 - 硼酸酸和草酸。

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