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：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：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：US5763665A

公开(公告)日：1998-06-09

申请号：US765214

申请日：1997-01-03

申请人： Kaspar Bott ,  Thomas Domschke ,  Michael Bohn

发明人： Kaspar Bott ,  Thomas Domschke ,  Michael Bohn

IPC分类号： B01J19/18 ,  C07C231/08 ,  C07C233/20 ,  C07C209/02

CPC分类号： B01J19/1862 ,  C07C231/08 ,  C07C233/20 ,  B01J2219/00094 ,  B01J2219/182

摘要： In a process for the preparation of crystalline N-methylol(meth)acrylamide from (meth)acryamide and paraformaldehyde, the reaction of the solid reactants to give a product melt and the subsequent crystallization thereof in a reactor while subjecting the reaction mixture to mechanical shear load is preferably carried out in a self-purging screw reactor or a disk reactor. The reaction of the reactants and the crystallization of the product melt are preferably carried out without added solvent. A catalyst, in particular an alkali metal carbonate or a trialkylamine, can be used for the reaction of the reactants.

摘要翻译： PCT No.PCT / EP95 / 02594 371日期1997年1月3日 102（e）日期1997年1月3日PCT提交1995年7月5日PCT公布。 第WO96 / 01251号公报 日期1996年1月18日在从（甲基）丙烯酰胺和多聚甲醛制备结晶N-羟甲基（甲基）丙烯酰胺的方法中，固体反应物的反应产生产物熔体，随后在反应器中结晶， 反应混合物至机械剪切载荷优选在自净式螺杆反应器或盘式反应器中进行。 反应物的反应和产物熔融物的结晶优选在不加入溶剂的情况下进行。 催化剂，特别是碱金属碳酸盐或三烷基胺可用于反应物的反应。

公开(公告)号：US06716937B2

公开(公告)日：2004-04-06

申请号：US10312851

申请日：2003-01-02

申请人： Gerd Bohner ,  Thomas Domschke ,  Rolf-Hartmuth Fischer ,  Martin Haubner ,  Christoph Sigwart ,  Ulrich Steinbrenner ,  Christian Tragut

发明人： Gerd Bohner ,  Thomas Domschke ,  Rolf-Hartmuth Fischer ,  Martin Haubner ,  Christoph Sigwart ,  Ulrich Steinbrenner ,  Christian Tragut

IPC分类号： C08F244

CPC分类号： C08G65/30 ,  C08G65/20

摘要： A process for the single-stage preparation of polytetrahydrofuran and/or tetrahydrofuran copolymers having a mean molecular weight of from 650 to 5000 dalton by polymerization of tetrahydrofuran over a heterogeneous acid catalyst in the presence of at least one telogen and/or comonomer selected from the group consisting of alpha,omega-diols, water, polytetrahydrofuran having a molecular weight of from 200 to 700 dalton and cyclic ethers comprises a) separating off the catalyst and/or downstream products of the catalyst suspended and/or dissolved in the output from the polymerization, b) fractionating the resulting catalyst-free output from the polymerization in at least one distillation step to give a distillation residue comprising the polymerization product and at least one tetrahydrofuran fraction and returning at least part of the tetrahydrofuran fraction to the polymerization and c) separating low molecular weight polytetrahydrofuran and/or tetrahydrofuran copolymers having a mean molecular weight of from 200 to 700 dalton from the distillation residue from work-up step b) and isolating polytetrahydrofuran and/or tetrahydrofuran copolymers having a mean molecular weight of from 650 to 5000 dalton.

摘要翻译： 一种通过在多相酸催化剂的存在下，在四氢呋喃和/或共聚单体的存在下，通过四氢呋喃聚合，单分级制备平均分子量为650-5000道尔顿的聚四氢呋喃和/或四氢呋喃共聚物的方法，该共聚单体选自 由α，ω-二醇，水，分子量为200至700道尔顿的聚四氢呋喃和环醚组成的组包括：a）将催化剂和/或催化剂的下游产物分离出悬浮和/或溶解在聚合物的输出中 b）在至少一个蒸馏步骤中将所得无催化剂的产物从聚合中分馏，得到包含聚合产物和至少一种四氢呋喃馏分的蒸馏残余物，并将至少部分四氢呋喃馏分返回到聚合反应中， 分子量的四氢呋喃和/或四氢呋喃共聚物 来自后处理步骤b）的蒸馏残余物的200至700道尔顿的颗粒重量，并分离平均分子量为650-5000道尔顿的聚四氢呋喃和/或四氢呋喃共聚物。

公开(公告)号：US07074944B2

公开(公告)日：2006-07-11

申请号：US10485685

申请日：2002-07-26

申请人： Ulrich Steinbrenner ,  Martin Haubner ,  Achim Gerstlauer ,  Thomas Domschke ,  Christoph Sigwart ,  Stefan Käshammer

发明人： Ulrich Steinbrenner ,  Martin Haubner ,  Achim Gerstlauer ,  Thomas Domschke ,  Christoph Sigwart ,  Stefan Käshammer

IPC分类号： C07D307/77

CPC分类号： C08G65/2696 ,  C08G65/20 ,  C08G65/2666

摘要： In a process for the single-stage preparation of polytetrahydrofuran and/or tetrahydrofuran copolymers having a mean molecular weight of from 650 to 5000 dalton by polymerization of tetrahydrofuran over an acid catalyst in the presence of at least one telogen and/or comonomer, the telogen and/or comonomer is added at at least two addition points in different segments of the polymerization apparatus.

摘要翻译： 在通过四氢呋喃在酸性催化剂的存在下，在至少一种停用的和/或共聚单体的存在下，通过四氢呋喃的聚合，单阶段制备平均分子量为650-5000道尔顿的聚四氢呋喃和/或四氢呋喃共聚物的方法， 和/或共聚单体在聚合装置的不同部分中的至少两个添加点加入。

公开(公告)号：US06234092B1

公开(公告)日：2001-05-22

申请号：US09456515

申请日：1999-12-08

申请人： Thomas Domschke ,  Andreas Joa ,  Klaus Steinebrunner

发明人： Thomas Domschke ,  Andreas Joa ,  Klaus Steinebrunner

IPC分类号： F23G704

CPC分类号： C02F1/72 ,  C02F1/10 ,  F23C9/006 ,  F23C2900/99001 ,  F23D17/002 ,  F23G7/001 ,  F23L7/00 ,  F23L7/007 ,  Y02E20/342 ,  Y02E20/344

摘要： A process for the thermal treatment of incombustible liquids in a combustion space of a combustion apparatus by contacting the incombustible liquid with a supplementary fuel in the combustion space in the presence of at least one reactive gas. The process of the invention comprises feeding the incombustible liquid and the supplementary fuel into the combustion space (1) at different points, mixing the incombustible liquid with at least one reactive gas and the supplementary fuel with at least one inert gas prior to the contacting, and vaporizing the incombustible liquid and supplementary fuel prior to the contacting in the combustion space. The advantage of this invention is that environmentally harmful waste waters in particular are disposed of by burning these using a supplementary fuel. The required amounts of supplementary fuel are minimal in the process and only small amounts of nitrogen oxides, carbon monoxide and soot are generated.

摘要翻译： 一种用于在燃烧装置的燃烧空间中热处理不燃性液体的方法，该方法是在至少一种反应气体的存在下使不燃性液体与辅助燃料在燃烧空间中接触。 本发明的方法包括在不同的点将不燃性液体和辅助燃料进料到燃烧空间（1）中，在接触之前将不燃性液体与至少一种反应性气体和补充燃料与至少一种惰性气体混合， 以及在燃烧空间中接触之前使不燃性液体和补充燃料蒸发。 本发明的优点是特别是通过使用补充燃料燃烧这些废物来处理对环境有害的废水。 所需量的补充燃料在该过程中是最小的，并且仅产生少量的氮氧化物，一氧化碳和烟灰。