公开(公告)号：US06462220B1

公开(公告)日：2002-10-08

申请号：US09763710

申请日：2001-02-26

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： C07C25525

CPC分类号： C07C253/30 ,  C07C209/48

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 cl) 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，并且将蒸馏除去6-氨基己腈，然后d1）蒸馏除去己二腈，或同时蒸馏除去6-氨基己腈和己二腈 分离的馏分以步骤d1）或c2）中塔温度低于185℃的碱为特征。

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：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：US06265602B1

公开(公告)日：2001-07-24

申请号：US09622800

申请日：2000-08-23

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

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

IPC分类号： C07C25500

CPC分类号： C07C253/30 ,  B01J23/02 ,  B01J23/78 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

摘要： A process for hydrogenation of aliphatic alpha, omega-dinitriles in the presence of a heterogeneous fixed bed catalyst comprises using a reaction mixture comprising from 2 &mgr;mol to 30 mmol NA, K, Rb, Cs, Mg, Ca, Sr, Ba or Mn or mixtures thereof in the form of a basic salt, based on 10 mol of aliphatic alpha, omega-dinitrile used.

摘要翻译： 在异相固定床催化剂存在下，脂肪族α，ω-二腈的氢化方法包括使用包含2μmol-30mmol NA，K，Rb，Cs，Mg，Ca，Sr，Ba或Mn的反应混合物或 基于10摩尔所用的脂肪族α，ω-二腈的碱性盐形式的混合物。

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：US06677486B2

公开(公告)日：2004-01-13

申请号：US09985982

申请日：2001-11-07

申请人： Andreas Ansmann ,  Christoph Benisch ,  Frank Funke ,  Frank Ohlbach ,  Martin Merger

发明人： Andreas Ansmann ,  Christoph Benisch ,  Frank Funke ,  Frank Ohlbach ,  Martin Merger

IPC分类号： C07C2948

CPC分类号： C07D295/13 ,  B01J25/00 ,  B01J37/0018 ,  C07C209/48 ,  C07C211/14 ,  C07C211/36

摘要： Nitriles are hydrogenated to primary amines over an activated, alpha-Al2O3-containing, macroporous Raney catalyst based on an alloy of aluminum and at least one transition metal selected from the group consisting of iron, cobalt and nickel, and, if desired, one or more further transition metals selected from the group consisting of titanium, zirconium, chromium and manganese, which is obtainable by a process comprising the steps in the order (a)-(f): (a) preparing a kneadable composition comprising the alloy, a shaping aid, water and a pore former; (b) shaping the kneadable composition to form a shaped body; (c) calcining the shaped body; (d) activating the calcined shaped body by treatment with aqueous alkali metal hydroxide solution; (e) rinsing the shaped catalyst body with aqueous alkali metal hydroxide solution; (f) rinsing the shaped catalyst body with water.

摘要翻译： 基于铝和至少一种选自铁，钴和镍的过渡金属的合金，并且如果需要，腈在一种活化的含α-Al 2 O 3的大孔阮内催化剂上氢化成伯胺，如果需要， （a） - （f）：（a）制备包含该合金的可捏合组合物的方法可以获得更多的选自钛，锆，铬和锰的过渡金属， 成型助剂，水和成孔剂;（b）使捏合组合物成形以形成成形体;（c）煅烧成形体;（d）用碱金属氢氧化物水溶液处理活化煅烧成形体;（e） 用碱金属氢氧化物水溶液冲洗成型的催化剂体;（f）用水冲洗成型的催化剂体。

公开(公告)号：US6140545A

公开(公告)日：2000-10-31

申请号：US251462

申请日：1999-02-17

申请人： Martin Merger ,  Shelue Liang ,  Rolf Fischer ,  Joachim Wulff-Doring

发明人： Martin Merger ,  Shelue Liang ,  Rolf Fischer ,  Joachim Wulff-Doring

IPC分类号： C07C29/149 ,  C07C37/08

CPC分类号： C07C29/149 ,  C07C2101/14

摘要： In a process for preparing alcohols by gas phase hydrogenation of carboxylic acids or esters thereof at elevated temperature and elevated pressure in the presence of catalysts consisting of or comprising, as hydrogenating components, oxides of main group VI and/or subgroup IV, the hydrogenation is carried outa) at from 250.degree. C. to 400.degree. C. and from 5 bar to 100 bar in the presence ofb) primary or secondary alcohols, the molar hydrogen/alcohol ratio being at most 800.

摘要翻译： 在通过在升高的温度和升高的压力下，在由主要VI族和/或第IV族的氧化物组成或包含氢化组分的催化剂存在下，在羧酸或其酯的气相氢化制备醇的方法中，氢化是 在b）伯醇或仲醇的存在下，在250℃至400℃和5巴至100巴下进行a），氢/醇摩尔比为至多800。

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：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：US06278023B1

公开(公告)日：2001-08-21

申请号：US09622774

申请日：2000-08-23

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： C07C20900

CPC分类号： C07C211/12 ,  B01J23/745 ,  C07C209/48

摘要： A process for preparing aliphatic alpha, omega-diamines by hydrogenation of aliphatic alpha, omega-dinitriles in the presence of a catalyst comprises using a hydrogenation catalyst comprising (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, and also (c) from 0 to 0.3% by weight based on (a) of a compound based on an alkali and/or alkaline earth metal.

摘要翻译： 通过在催化剂存在下通过氢化脂肪族α，ω-二腈制备脂肪族α，ω-二胺的方法包括使用包含（a）铁或基于铁或其混合物的化合物的氢化催化剂，（b）0.001 至（c）基于（a）基于选自铝，硅，锆，钛和钒的2,3,4或5种元素的助催化剂，并且（c）0至0.3％ 基于（a）基于碱金属和/或碱土金属的化合物的重量。