公开(公告)号：US20050197504A1

公开(公告)日：2005-09-08

申请号：US10515625

申请日：2003-07-07

申请人： Gerd Kaibel ,  Martin Merger ,  Thomas Domschke ,  Petra Deckert ,  Friedrich Sauer

发明人： Gerd Kaibel ,  Martin Merger ,  Thomas Domschke ,  Petra Deckert ,  Friedrich Sauer

IPC分类号： C07D307/62 ,  C07D305/12

CPC分类号： C07D307/62 ,  Y02P20/582

摘要： The invention relates to a method for the separation of ascorbic acid from a mixture containing ascorbic acid and 2-keto-L-gulonic acid in a polar, preferably aqueous solvent, by means of liquid/liquid extraction using an amide. The method preferably also comprises steps for the back-extraction of the ascorbic acid, recycling of the extraction solvent and/or the back extraction solvent and for isolation of the ascorbic acid from the back extraction solvent. The invention further relates to a method for the production of ascorbic acid from KGA and isolation of the ascorbic acid so produced.

摘要翻译： 本发明涉及通过使用酰胺的液/液萃取从抗坏血酸和2-酮-L-古洛糖酸的混合物中分离抗坏血酸在极性，优选水性溶剂中的方法。 该方法优选还包括用于反萃取抗坏血酸的步骤，提取溶剂和/或反萃取溶剂的再循环以及用于从反萃取溶剂中分离抗坏血酸的步骤。 本发明还涉及从KGA生产抗坏血酸并分离如此生产的抗坏血酸的方法。

公开(公告)号：US07696360B2

公开(公告)日：2010-04-13

申请号：US10515625

申请日：2003-07-07

申请人： Gerd Kaibel ,  Martin Merger ,  Thomas Domschke ,  Petra Deckert ,  Friedrich Sauer

发明人： Gerd Kaibel ,  Martin Merger ,  Thomas Domschke ,  Petra Deckert ,  Friedrich Sauer

IPC分类号： C07D307/62

CPC分类号： C07D307/62 ,  Y02P20/582

摘要： The invention relates to a method for the separation of ascorbic acid from a mixture containing ascorbic acid and 2-keto-L-gulonic acid in a polar, preferably aqueous solvent, by means of liquid/liquid extraction using an amide. The method preferably also comprises steps for the back-extraction of the ascorbic acid, recycling of the extraction solvent and/or the back extraction solvent and for isolation of the ascorbic acid from the back extraction solvent. The invention further relates to a method for the production of ascorbic acid from KGA and isolation of the ascorbic acid so produced.

摘要翻译： 本发明涉及通过使用酰胺的液/液萃取在极性优选含水溶剂中从含有抗坏血酸和2-酮-L-古洛糖酸的混合物中分离抗坏血酸的方法。 该方法优选还包括用于反萃取抗坏血酸的步骤，提取溶剂和/或反萃取溶剂的再循环以及用于从反萃取溶剂中分离抗坏血酸的步骤。 本发明还涉及从KGA生产抗坏血酸并分离如此生产的抗坏血酸的方法。

公开(公告)号：US20060149084A1

公开(公告)日：2006-07-06

申请号：US10539960

申请日：2003-12-13

申请人： Thomas Domschke ,  Martin Merger ,  Petra Deckert ,  Friedrich Sauer

发明人： Thomas Domschke ,  Martin Merger ,  Petra Deckert ,  Friedrich Sauer

IPC分类号： C07D307/62 ,  C07C51/245

CPC分类号： C07H1/06 ,  C07H7/027

摘要： The present invention relates to a process for extracting 2-keto-L-gulonic acid (KGA) from a polar, preferably aqueous, solvent, preferably from a solvent which comprises a mixture of ascorbic acid and 2-keto-L-gulonic acid, by means of liquid/liquid extraction using an extractant which comprises a tertiary amine and a polar organic diluent. The process of the invention preferably also comprises steps for back-extraction of the KGA and recycling of the extractant. The present invention likewise relates to a process for preparing ascorbic acid from KGA and isolating the prepared ascorbic acid.

摘要翻译： 本发明涉及一种从极性，优选含水溶剂，优选由包含抗坏血酸和2-酮-L-古洛糖酸的混合物的溶剂中提取2-酮-L-古洛糖酸（KGA）的方法， 通过使用包含叔胺和极性有机稀释剂的萃取剂的液/液萃取。 本发明的方法优选还包括用于反萃取KGA和回收萃取剂的步骤。 本发明同样涉及从KGA制备抗坏血酸并分离制备的抗坏血酸的方法。

公开(公告)号：US07091375B2

公开(公告)日：2006-08-15

申请号：US10534334

申请日：2003-11-07

申请人： Thomas Domschke ,  Martin Merger ,  Georg Grossmann ,  Tillmann Faust

发明人： Thomas Domschke ,  Martin Merger ,  Georg Grossmann ,  Tillmann Faust

IPC分类号： C07D305/12

CPC分类号： C07H7/027 ,  Y02P20/127

摘要： The invention relates to a method for producing 2-keto-L-gulonic acid-C4–C10 alkyl ester by esterifying 2-keto-L-gulonic acid (KGS) with an unsaturated, branched or unbranched C4–C10 alcohol. The inventive method is characterized by the fact that an aqueous KGS solution is reacted with a C4–C10 alcohol up to an esterification degree of 20 to 70 percent in a pre-esterification process carried out under acidic catalysis conditions; and the obtained product is dehydrogenated with an unsaturated, branched or unbranched C4–C10 alcohol in a continuous rectification device, whereby the esterification reaction continues, n-butanol preferably being used as the alkyl alcohol. In a preferred embodiment, the aqueous KGS solution is concentrated up to or beyond the limit of solubility prior to the esterification process, preferably by catalyzing a homogeneous or heterogeneous catalyst, especially sulfonic acid, at temperatures of 50 to 120° C. In another embodiment, the produced KGS ester is reacted in one or several additional steps so as to obtain L-ascorbic acid.

摘要翻译： 本发明涉及通过酯化2-酮-L-古洛糖酸（KGS）制备2-酮-L-古洛糖酸-C 4 -C 10烷基酯的方法 ）与不饱和，支链或非支链C 4 -C 10醇。 本发明的方法的特征在于，将KGS水溶液与C 4 -C 10 - 醇反应，直到酯化程度为20至70％ 在酸性催化条件下进行酯化过程; 并将得到的产物用连续精馏装置中的不饱和支链或非支链C 4 -C 10醇脱氢，由此继续进行酯化反应，正丁醇优选为 用作烷基醇。 在优选的实施方案中，在酯化过程之前，优选通过在50至120℃的温度下催化均相或多相催化剂，特别是磺酸，将KGS水溶液浓缩至或超过溶解度的极限。在另一个实施方案中 ，所制备的KGS酯在一个或几个附加步骤中反应，以获得L-抗坏血酸。

公开(公告)号：US20060058550A1

公开(公告)日：2006-03-16

申请号：US10534334

申请日：2003-11-07

申请人： Thomas Domschke ,  Martin Merger ,  Georg Grobmann ,  Tillmann Faust

发明人： Thomas Domschke ,  Martin Merger ,  Georg Grobmann ,  Tillmann Faust

IPC分类号： C07C69/66

CPC分类号： C07H7/027 ,  Y02P20/127

摘要： The invention relates to a method for producing 2-keto-L-gulonic acid-C4-C10 alkyl ester by esterifying 2-keto-L-gulonic acid (KGS) with an unsaturated, branched or unbranched C4-C10 alcohol. The inventive method is characterized by the fact that an aqueous KGS solution is reacted with a C4-C10 alcohol up to an esterification degree of 20 to 70 percent in a pre-esterification process carried out under acidic catalysis conditions; and the obtained product is dehydrogenated with an unsaturated, branched or unbranched C4-C10 alcohol in a continuous rectification device, whereby the esterification reaction continues, n-butanol preferably being used as the alkyl alcohol. In a preferred embodiment, the aqueous KGS solution is concentrated up to or beyond the limit of solubility prior to the esterification process, preferably by catalyzing a homogeneous or heterogeneous catalyst, especially sulfonic acid, at temperatures of 50 to 120 ° C. In another embodiment, the produced KGS ester is reacted in one or several additional steps so as to obtain L-ascorbic acid.

摘要翻译： 本发明涉及通过酯化2-酮-L-古洛糖酸（KGS）制备2-酮-L-古洛糖酸-C 4 -C 10烷基酯的方法 ）与不饱和，支链或非支链C 4 -C 10醇。 本发明的方法的特征在于，将KGS水溶液与C 4 -C 10 - 醇反应，直到酯化程度为20至70％ 在酸性催化条件下进行酯化过程; 并将得到的产物用连续精馏装置中的不饱和支链或非支链C 4 -C 10醇脱氢，由此继续进行酯化反应，正丁醇优选为 用作烷基醇。 在优选的实施方案中，在酯化过程之前，优选通过在50至120℃的温度下催化均相或多相催化剂，特别是磺酸，将KGS水溶液浓缩至或超过溶解度的极限。在另一个实施方案中 ，所制备的KGS酯在一个或几个附加步骤中反应，以获得L-抗坏血酸。

公开(公告)号：US20070123717A1

公开(公告)日：2007-05-31

申请号：US10582911

申请日：2004-12-10

申请人： Thomas Domschke ,  Martin Merger ,  Frank Haese ,  Peter Resch ,  Tillmann Faust

发明人： Thomas Domschke ,  Martin Merger ,  Frank Haese ,  Peter Resch ,  Tillmann Faust

IPC分类号： C07D307/62

CPC分类号： C07C67/08 ,  C07H7/02 ,  C07H7/027 ,  C07C69/716

摘要： A method for the production of C1-C10-alkyl 2-keto-L-gulonates by esterification of 2-keto-L-gulonic acid anhydrate with an anhydrous C1-C10-alkyl alcohol in the presence of an acidic homogeneous catalyst in a reactor cascade comprising at least two reactors, one of these reactors being a tubular reactor, without the water forming in the esterification being removed from the reaction space.

摘要翻译： 通过2-酮-L-古洛糖酸无水物与无水C的酯化制备C 1 -C 10 - 烷基2-酮-L-古洛糖化物的方法 在酸性均相催化剂存在下，在包含至少两个反应器的反应器级联中，其中一个反应器是管式反应器，没有 酯化反应中形成的水​​从反应空间中除去。

公开(公告)号：US20120232309A1

公开(公告)日：2012-09-13

申请号：US13415174

申请日：2012-03-08

申请人： Thomas SCHAUB ,  Boris Buschhaus ,  Marion Kristina Brinks ,  Mathias Schelwies ,  Rocco Paciello ,  Johann-Peter Melder ,  Martin Merger

发明人： Thomas SCHAUB ,  Boris Buschhaus ,  Marion Kristina Brinks ,  Mathias Schelwies ,  Rocco Paciello ,  Johann-Peter Melder ,  Martin Merger

IPC分类号： C07C209/16 ,  C07C211/02

CPC分类号： C07C213/02 ,  C07C215/08 ,  C07C217/08

摘要： Preparing a primary amine by alcohol amination of alcohol with ammonia and elimination of water includes reacting, in a homogeneously catalyzed reaction, a mixture of alcohol, ammonia, nonpolar solvent, and catalyst, in a liquid phase, to obtain a product mixture. The process then includes phase separating the product mixture into a polar product phase and a nonpolar product phase, and separating off the nonpolar product phase. At least some of the nonpolar phase returns to the homogenously catalyzed reaction. The process further includes separating off amination product from the polar product phase. At least some of the catalyst is in the nonpolar phase, and the catalyst accumulates in the nonpolar phase.

摘要翻译： 通过醇与醇的氨基化反应制备伯胺并除去水包括在均相催化的反应中，将醇，氨，非极性溶剂和催化剂的混合物在液相中反应，得到产物混合物。 然后，该方法包括将产物混合物相分离成极性产物相和非极性产物相，并将非极性产物相分离。 至少一些非极性相返回均匀催化反应。 该方法还包括从极性产物相分离胺化产物。 至少一些催化剂处于非极性相，并且催化剂积聚在非极性相中。

公开(公告)号：US07091153B2

公开(公告)日：2006-08-15

申请号：US10776544

申请日：2004-02-12

申请人： Guido Voit ,  Rolf Fischer ,  Peter Bassler ,  Andreas Ansmann ,  Hermann Luyken ,  Martin Merger ,  Frank Ohlbach ,  Alwin Rehfinger

发明人： Guido Voit ,  Rolf Fischer ,  Peter Bassler ,  Andreas Ansmann ,  Hermann Luyken ,  Martin Merger ,  Frank Ohlbach ,  Alwin Rehfinger

IPC分类号： B01J23/34 ,  B01J21/14

CPC分类号： C07C253/30 ,  B01J23/8892 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

摘要： A material useful as catalyst for the hydrogenation of alpha, omega-dinitriles comprises (a) iron or a compound based on iron or mixtures thereof, (b) from 0.001 to 0.3% by weight based on (a) of a promoter based on 2, 3, 4 or 5 elements selected from the group consisting of aluminum, silicon, zirconium, titanium and vanadium, (c) from 0 to 0.3% by weight based on (a) of a compound based on an alkali and/or alkaline earth metal, and also (d) from 0.001 to 1% by weight based on (a) of manganese.

摘要翻译： 可用作α，ω-二腈的氢化催化剂的材料包括（a）铁或基于铁或其混合物的铁或其混合物，（b）基于（a）基于2的促进剂的0.001至0.3重量％ ，选自铝，硅，锆，钛和钒的3,4或5种元素，（c）基于（a）基于碱和/或碱土金属的化合物，0至0.3重量％ 金属，以及（d）以（a）锰计为0.001〜1重量％。

公开(公告)号：US06815388B1

公开(公告)日：2004-11-09

申请号：US10088406

申请日：2002-03-19

申请人： Frank Ohlbach ,  Rolf Fischer ,  Hermann Luyken ,  Johann-Peter Melder ,  Martin Merger ,  Andreas Ansmann ,  Peter Bassler

发明人： Frank Ohlbach ,  Rolf Fischer ,  Hermann Luyken ,  Johann-Peter Melder ,  Martin Merger ,  Andreas Ansmann ,  Peter Bassler

IPC分类号： B01J3808

CPC分类号： B01J37/18 ,  B01J23/745

摘要： Passivated iron useful as catalytically active component after activation is activated by hydrogen at elevated temperature and elevated pressure in the presence of a nitrile.

摘要翻译： 活化后可用作催化活性组分的钝化铁在高温和高压下在腈的存在下由氢活化。

公开(公告)号：US06346641B1

公开(公告)日：2002-02-12

申请号：US09720882

申请日：2001-01-02

申请人： Hermann Luyken ,  Frank Ohlbach ,  Andreas Ansmann ,  Peter Bassler ,  Rolf Fischer ,  Johann-Peter Melder ,  Martin Merger ,  Alwin Rehfinger ,  Guido Voit ,  Günther Achhammer

发明人： Hermann Luyken ,  Frank Ohlbach ,  Andreas Ansmann ,  Peter Bassler ,  Rolf Fischer ,  Johann-Peter Melder ,  Martin Merger ,  Alwin Rehfinger ,  Guido Voit ,  Günther Achhammer

IPC分类号： C07C25500

CPC分类号： C07C253/30 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

摘要： A process for the coproduction of 6-aminocapronitrile and hexamethylenediamine starting from adiponitrile by a) hydrogenating adiponitrile in the presence of a catalyst comprising an element of the eighth transition group as catalytically active component, to obtain a mixture comprising 6-aminocapronitrile, hexamethylenediamine, adiponitrile and high boilers, b) distillatively removing hexamethylenediamine from the mixture comprising 6-aminocapronitrile, hexamethylenediamine, adiponitrile and high boilers, and either c1) distillatively removing 6-aminocapronitrile, and then d1) distillatively removing adiponitrile, or c2) simultaneously distillatively removing 6-aminocapronitrile and adiponitrile into separate fractions is characterized by base of column temperatures below 185° C. in steps d1) or c2).

摘要翻译： 一种从己二腈开始共生产6-氨基己腈和六亚甲基二胺的方法，其中a）在包含第八过渡基团的元素的催化剂作为催化活性组分的存在下氢化己二腈，得到包含6-氨基己腈，己二胺，己二腈和 高锅炉，b）从包含6-氨基己腈，己二胺，己二腈和高沸点的混合物中蒸馏除去六亚甲基二胺，和c）蒸馏除去6-氨基己腈，然后d1）蒸馏除去己二腈，orc2）同时蒸馏除去6-氨基己腈和己二腈 在步骤d1）或c2）中，单独馏分的特征在于塔温度低于185℃的碱。