公开(公告)号：US20120232309A1

公开(公告)日：2012-09-13

申请号：US13415174

申请日：2012-03-08

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

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

IPC: C07C209/16 ,  C07C211/02

CPC classification number: C07C213/02 ,  C07C215/08 ,  C07C217/08

Abstract: 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.

Abstract translation: 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：US07091375B2

公开(公告)日：2006-08-15

申请号：US10534334

申请日：2003-11-07

Applicant: Thomas Domschke ,  Martin Merger ,  Georg Grossmann ,  Tillmann Faust

Inventor： Thomas Domschke ,  Martin Merger ,  Georg Grossmann ,  Tillmann Faust

IPC: C07D305/12

CPC classification number: C07H7/027 ,  Y02P20/127

Abstract: 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.

Abstract translation: 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

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

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

IPC: B01J23/34 ,  B01J21/14

CPC classification number: C07C253/30 ,  B01J23/8892 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

Abstract: 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.

Abstract translation: 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

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

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

IPC: B01J3808

CPC classification number: B01J37/18 ,  B01J23/745

Abstract: 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.

Abstract translation: 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

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

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

IPC: C07C25500

CPC classification number: C07C253/30 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

Abstract: 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).

Abstract translation: 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。

公开(公告)号：US06265602B1

公开(公告)日：2001-07-24

申请号：US09622800

申请日：2000-08-23

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

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

IPC: C07C25500

CPC classification number: C07C253/30 ,  B01J23/02 ,  B01J23/78 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

Abstract: 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.

Abstract translation: 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：US09193666B2

公开(公告)日：2015-11-24

申请号：US13415409

申请日：2012-03-08

Applicant: Thomas Schaub ,  Boris Buschhaus ,  Marion Kristina Brinks ,  Mathias Schelwies ,  Rocco Paciello ,  Johann-Peter Melder ,  Martin Merger

Inventor： Thomas Schaub ,  Boris Buschhaus ,  Marion Kristina Brinks ,  Mathias Schelwies ,  Rocco Paciello ,  Johann-Peter Melder ,  Martin Merger

IPC: C07C209/66 ,  C07F15/00 ,  C07C209/16 ,  C07C213/02 ,  C07D207/02 ,  C07D207/20 ,  C07D295/027 ,  C07D307/52

CPC classification number: C07C209/16 ,  C07C213/02 ,  C07D207/02 ,  C07D207/20 ,  C07D295/027 ,  C07D307/52 ,  C07C211/09 ,  C07C215/08 ,  C07C217/08 ,  C07C211/10 ,  C07C211/12

Abstract: Process for preparing alkanolamines which have a primary amino group (—NH2) and a hydroxyl group (—OH) by alcohol amination of diols having two hydroxyl groups (—OH) by means of ammonia with elimination of water, wherein the reaction is carried out homogeneously catalyzed in the presence of at least one complex catalyst comprising at least one element selected from groups 8, 9 and 10 of the Periodic Table and also at least one donor ligand.

Abstract translation: 制备具有伯氨基（-NH 2）和羟基（-OH）的链烷醇胺的方法，其通过用氨除去水而具有两个羟基（-OH）的二醇醇胺化，其中反应进行 在包含至少一种选自元素周期表第8,9和10族的元素的复合催化剂的存在下，以及至少一种供体配体均匀催化。

公开(公告)号：US20120232292A1

公开(公告)日：2012-09-13

申请号：US13415412

申请日：2012-03-08

Applicant: Thomas SCHAUB ,  Boris BUSCHHAUS ,  Marion Kristina BRINKS ,  Mathias SCHELWIES ,  Rocco PACIELLO ,  Johann-Peter MELDER ,  Martin MERGER

Inventor： Thomas SCHAUB ,  Boris BUSCHHAUS ,  Marion Kristina BRINKS ,  Mathias SCHELWIES ,  Rocco PACIELLO ,  Johann-Peter MELDER ,  Martin MERGER

IPC: C07D307/52 ,  C07C209/16

CPC classification number: C07C209/16 ,  C07C213/02 ,  C07D207/04 ,  C07D207/20 ,  C07D295/023 ,  C07D307/52 ,  C07C211/07 ,  C07C211/09 ,  C07C215/08 ,  C07C217/08

Abstract: Process for the preparation of primary amines which have at least one functional group of the formula (—CH2—NH2) by alcohol amination of starting materials which have at least one functional group of the formula (—CH2—OH), with ammonia, with the elimination of water, where the alcohol amination is carried out under homogeneous catalysis in the presence of at least one complex catalyst which comprises at least one element selected from groups 8 and 9 of the Periodic Table of the Elements, and also at least one phosphorus donor ligand of the general formula (I).

Abstract translation: 具有至少一个式（-CH 2 -NH 2）官能团的伯胺的方法，其通过具有至少一个式（-CH 2 -OH）官能团的起始原料与氨进行醇胺化反应，与 消除水，其中在均相催化下，在至少一种包含至少一种选自元素周期表第8和9族的元素的复合催化剂的存在下进行醇胺化，以及至少一种磷 通式（I）的供体配体。

公开(公告)号：US20060058550A1

公开(公告)日：2006-03-16

申请号：US10534334

申请日：2003-11-07

Applicant: Thomas Domschke ,  Martin Merger ,  Georg Grobmann ,  Tillmann Faust

Inventor： Thomas Domschke ,  Martin Merger ,  Georg Grobmann ,  Tillmann Faust

IPC: C07C69/66

CPC classification number: C07H7/027 ,  Y02P20/127

Abstract: 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.

Abstract translation: 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

Applicant: Andreas Ansmann ,  Christoph Benisch ,  Frank Funke ,  Frank Ohlbach ,  Martin Merger

Inventor： Andreas Ansmann ,  Christoph Benisch ,  Frank Funke ,  Frank Ohlbach ,  Martin Merger

IPC: C07C2948

CPC classification number: C07D295/13 ,  B01J25/00 ,  B01J37/0018 ,  C07C209/48 ,  C07C211/14 ,  C07C211/36

Abstract: 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.

Abstract translation: 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。