公开(公告)号：US08383866B2

公开(公告)日：2013-02-26

申请号：US12953004

申请日：2010-11-23

Applicant: Rolf Pinkos ,  Axel Paul ,  Rolf-Hartmuth Fischer ,  Roman Dostalek

Inventor： Rolf Pinkos ,  Axel Paul ,  Rolf-Hartmuth Fischer ,  Roman Dostalek

IPC: C07C29/156

CPC classification number: C07C29/149 ,  C07C31/20

Abstract: The present invention relates to a process for preparing diols by hydrogenating a mixture comprising carboxylic acid, carboxylic anhydrides and/or carboxylic esters/lactones by means of a cobalt-comprising catalyst, wherein alkali metal and/or alkaline earth metal ions are added to the hydrogenation feed, excluding alkali metal and/or alkaline earth metal ions of mineral acids.

Abstract translation: 本发明涉及通过使含钴催化剂氢化包含羧酸，羧酸酐和/或羧酸酯/内酯的混合物来制备二醇的方法，其中将碱金属和/或碱土金属离子加入到 氢化进料，不含碱金属和/或无机酸的碱土金属离子。

公开(公告)号：US20110224401A1

公开(公告)日：2011-09-15

申请号：US13131790

申请日：2009-11-29

Applicant: Stefan Käshammer ,  Rolf Pinkos ,  Tobias Wabnitz ,  Rolf-Hartmuth Fischer

Inventor： Stefan Käshammer ,  Rolf Pinkos ,  Tobias Wabnitz ,  Rolf-Hartmuth Fischer

IPC: B01D3/14 ,  C08G65/20 ,  C08G63/00

CPC classification number: B01D1/065 ,  B01D1/22 ,  B01D3/06 ,  C08G65/20 ,  C08G65/30

Abstract: The invention relates to an apparatus for separating a liquid substance mixture by distillation, a method for producing a tetrahydrofuran homopolymer and copolymer in which the oligomers in a liquid starting mixture containing oligomers are separated by distillation in such an apparatus, tetrahydrofuran homopolymers and copolymers which can be obtained using said method and have a narrow distribution of the relative molar mass, and the use thereof.

Abstract translation: 本发明涉及一种通过蒸馏分离液体物质混合物的装置，四氢呋喃均聚物和共聚物的制备方法，其中含有低聚物的液体起始混合物中的低聚物在这种装置中通过蒸馏分离，四氢呋喃均聚物和共聚物可以 使用所述方法获得并且具有相对摩尔质量的窄分布及其用途。

公开(公告)号：US07875740B2

公开(公告)日：2011-01-25

申请号：US10493419

申请日：2002-10-18

Applicant: Andreas Ansmann ,  Christoph Benisch ,  Peter Baβler ,  Rolf-Hartmuth Fischer ,  Stefan Maixner ,  Johann-Peter Melder ,  Hermann Luyken

Inventor： Andreas Ansmann ,  Christoph Benisch ,  Peter Baβler ,  Rolf-Hartmuth Fischer ,  Stefan Maixner ,  Johann-Peter Melder ,  Hermann Luyken

IPC: C07C255/03 ,  C07C209/04

CPC classification number: C07C253/30 ,  B01J23/745 ,  B01J23/8892 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

Abstract: The iron-containing catalyst suitable for use as a catalyst contains a) iron or a mixture containing iron and an iron-based compound. The iron has an average crystallite size ranging from 1-35 nm measured by X-ray diffraction.

Abstract translation: 适合用作催化剂的含铁催化剂含有a）铁或含有铁和铁基化合物的混合物。 铁通过X射线衍射测得的平均微晶尺寸为1-35nm。

公开(公告)号：US07385073B2

公开(公告)日：2008-06-10

申请号：US10515281

申请日：2003-05-21

Applicant: Stefan Maixner ,  Christoph Benisch ,  Hermann Luyken ,  Peter Baβler ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Andreas Ansmann

Inventor： Stefan Maixner ,  Christoph Benisch ,  Hermann Luyken ,  Peter Baβler ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Andreas Ansmann

IPC: C07C253/34

CPC classification number: C07C253/34 ,  C07C255/24

Abstract: A process for reducing the level of an aliphatic monounsaturated amine (IV) in a mixture (V) containing an aminonitrile (I) or a diamine (II) or a dinitrile (III) or mixtures thereof as well as said mine (IV) by a) reacting said mixture (V) with an anionic nucleophile (VI) which contains a nucleophilic atom selected from the group consisting of oxygen, nitrogen and sulfur, which is capable of taking up an H+ ion to form an acid having a pKa value in the range from 7 to 11, as measured in water at 25° C., and which has a relative nucleophilicity, as measured in methyl perchlorate/methanol at 25° C., in the range from 3.4 to 4.7 when said nucleophilic atom is oxygen, in the range from 4.5 to 5.8 when said nucleophilic atom is nitrogen, and in the range from 5.5 to 6.8 when said nucleophilic atom is sulfur, in an amount in the range from 0.01 to 10 mol per mole of said amine (IV) in said mixture (V) at a temperature in the range from 50 to 200° C. to obtain a mixture (VII), b) distilling said aminonitrile (I) or said diamine (II) or said dinitrile (III) or mixtures thereof from said mixture (VII) at a temperature in the range from 50 to 200° C. and at a pressure in the range from 0.1 to 100 kPa to obtain a bottom product (VIII), which comprises c) distilling an aminonitrile (I) or diamine (II) or dinitrile (III) or mixtures thereof from said bottom product (VIII) at a temperature which is lower than that chosen in step b).

Abstract translation: 在含有氨基腈（I）或二胺（II）或二腈（III）或其混合物以及所述矿（IV）的混合物（V）中降低脂族单不饱和胺（IV）的水平的方法， a）使所述混合物（V）与阴离子亲核试剂（VI）反应，所述阴离子亲核试剂（VI）含有选自氧，氮和硫的亲核原子，其能够吸收H + 形成在25℃下在水中测量的具有7至11的pK值的酸，其在25℃下在高氯酸甲酯/甲醇中测得的具有相对亲核性 当所述亲核原子为氧时，在3.4至4.7的范围内，当所述亲核原子为氮时，在4.5至5.8的范围内，当所述亲核原子为硫时在5.5至6.8的范围内，其量为 在所述混合物（V）中在50至200℃的温度范围内每摩尔所述胺（IV）为0.01至10摩尔的范围，以获得混合物 （VII）中，b）在50至200℃的温度下，从所述混合物（VII）中蒸馏所述氨基腈（I）或所述二胺（II）或所述二腈（III）或其混合物， 压力为0.1至100kPa，以获得底部产物（VIII），其包括c）在所述底部产物（VIII）中蒸馏氨基腈（I）或二胺（II）或二腈（III）或其混合物， 温度低于步骤b）中选择的温度。

公开(公告)号：US07351311B2

公开(公告)日：2008-04-01

申请号：US10505774

申请日：2003-02-28

Applicant: Gunther Windecker ,  Alexander Weck ,  Rolf-Hartmuth Fischer ,  Markus Rösch ,  Nils Bottke ,  Michael Hesse ,  Stephan Schlitter ,  Holger Borchert

Inventor： Gunther Windecker ,  Alexander Weck ,  Rolf-Hartmuth Fischer ,  Markus Rösch ,  Nils Bottke ,  Michael Hesse ,  Stephan Schlitter ,  Holger Borchert

IPC: B01D3/14 ,  C07D307/08

CPC classification number: B01D3/146 ,  C07D307/08 ,  Y10S203/20

Abstract: Crude water-containing tetrahydrofuran is purified by passing the crude tetrahydrofuran through three distillation columns, withdrawing water from the bottom of the first column, recycling water-containing tetrahydrofuran from the top of the second column into the first column, passing a sidestream of the first column into the second column, recycling the bottom product of the third column into the first column, and withdrawing a distillate at the top of the first column. Additionally, a sidestream of the second column is passed into the third column and the purified tetrahydrofuran is recovered as the top product of the third column.

Abstract translation: 通过将粗四氢呋喃通过三个蒸馏塔，从第一塔的底部排出水，将含水四氢呋喃从第二塔的顶部再循环到第一塔中，将第一个塔 塔进入第二列，将第三塔的底部产物回收到第一塔中，并且抽出第一塔顶部的馏出物。 此外，将第二塔的侧流送入第三塔，回收纯化的四氢呋喃作为第三塔的顶部产物。

公开(公告)号：US07271299B2

公开(公告)日：2007-09-18

申请号：US10516922

申请日：2003-06-11

Applicant: Michael Hesse ,  Stephan Schlitter ,  Holger Borchert ,  Markus Schubert ,  Markus Rösch ,  Nils Bottke ,  Rolf-Hartmuth Fischer ,  Alexander Weck ,  Gunther Windecker ,  Gunnar Heydrich

Inventor： Michael Hesse ,  Stephan Schlitter ,  Holger Borchert ,  Markus Schubert ,  Markus Rösch ,  Nils Bottke ,  Rolf-Hartmuth Fischer ,  Alexander Weck ,  Gunther Windecker ,  Gunnar Heydrich

IPC: C07C31/18

CPC classification number: C07C29/149 ,  C07C31/207

Abstract: Optionally alkyl-substituted 1,4-butanediol is prepared from C4-dicarboxylic acids and/or of derivatives thereof by: a) a gas stream of the C4-dicarboxylic acid or the derivative thereof in a first reactor in the gas phase to obtain a product which contains mainly optionally alkyl-substituted γ-butyro-lactone; b) removing succinic anhydride from the product of step a); c) catalytically hydrogenating the product of step b) in a second reactor in the gas phase to obtain optionally alkyl-substituted 1,4-butanediol; d) removing the desired product from intermediates, by-products and any unconverted reactants; and e) optionally recycling unconverted intermediates into one or both hydrogenation stages. The catalysts employed in each of the hydrogenation stages comprise ≦95% by weight of CuO, and ≦5% by weight of an oxidic support, and the second reactor has a higher pressure than the first reactor.

Abstract translation: 任选地，烷基取代的1,4-丁二醇由C 4-14二羧酸和/或其衍生物通过以下方法制备：a）引入C 4 - 二羧酸或其衍生物在气相中的第一反应器中，以获得主要含有烷基取代的γ-丁内酯的产物; b）从步骤a）的产物中除去琥珀酸酐; c）在气相中的第二反应器中催化氢化步骤b）的产物以获得任选的烷基取代的1,4-丁二醇; d）从中间体，副产物和任何未转化的反应物中除去所需的产物; 和e）任选地将未转化的中间体再循环到一个或两个氢化阶段。 在每个氢化阶段中使用的催化剂包含<95重量％的CuO和<= 5重量％的氧化载体，并且第二反应器具有比第一反应器更高的压力。

公开(公告)号：US07169958B2

公开(公告)日：2007-01-30

申请号：US10516923

申请日：2003-06-10

Applicant: Michael Hesse ,  Stephan Schlitter ,  Holger Borchert ,  Markus Schubert ,  Markus Rösch ,  Nils Bottke ,  Rolf-Hartmuth Fischer ,  Alexander Weck ,  Gunther Windecker ,  Gunnar Heydrich

Inventor： Michael Hesse ,  Stephan Schlitter ,  Holger Borchert ,  Markus Schubert ,  Markus Rösch ,  Nils Bottke ,  Rolf-Hartmuth Fischer ,  Alexander Weck ,  Gunther Windecker ,  Gunnar Heydrich

IPC: C07C29/132 ,  C07C29/149 ,  C07C29/136 ,  C07C29/147

CPC classification number: C07C29/149 ,  C07C31/207

Abstract: The present invention relates to a process for preparing optionally alkyl-substituted 1,4-butanediol by two-stage catalytic hydrogenation in the gas phase of C4-dicarboxylic acids and/or of derivatives thereof having the following steps: a) introducing a gas stream of a C4-dicarboxylic acid or of a derivative thereof at from 200 to 300° C. and from 2 to 60 bar into a first reactor and catalytically hydrogenating it to a product which contains mainly optionally alkyl-substituted γ-butyrolactone; b) converting the product stream into the liquid phase; c) introducing the product stream obtained in this way into a second reactor at a temperature of from 100° C. to 240° C. and a pressure of from 20 to 250 bar and catalytically hydrogenating it in the liquid phase to optionally alkyl-substituted 1,4-butanediol; d) removing the desired product from by-products and any unconverted reactants; e) optionally recycling unconverted intermediates into one or both hydrogenation stages, said hydrogenation stages both using a catalyst which comprises ≦95% by weight, preferably from 5 to 95% by weight, in particular from 10 to 80% by weight, of CuO, and ≧5% by weight, preferably from 5 to 95% by weight, in particular from 20 to 90% by weight, of a support, said second reactor having a higher pressure than said first reactor, and the product mixture removed from said first reactor being introduced without further purification into said second reactor.

Abstract translation: 本发明涉及通过在具有下列物质的C 4 - 二羧酸和/或其衍生物的气相中通过两阶段催化氢化制备任选的烷基取代的1,4-丁二醇的方法 步骤：a）将200-300℃和2-60巴的C 4-14二羧酸或其衍生物的气流引入第一反应器，并将其催化氢化至 主要含烷基取代的γ-丁内酯的产品; b）将产物流转化成液相; c）将以这种方式获得的产物流在100℃至240℃的温度和20至250巴的压力下引入第二反应器，并将其在液相中催化氢化为任选的烷基取代的 1,4-丁二醇 d）从副产物和任何未转化的反应物中除去所需的产物; e）任选地将未转化的中间体再循环到一个或两个氢化阶段中，所述氢化步骤均使用包含<= 95重量％，优选5至95重量％，特别是10至80重量％的CuO ，和> = 5重量％，优选5至95重量％，特别是20至90重量％的载体，所述第二反应器具有比所述第一反应器更高的压力，并将产物混合物从 所述第一反应器不经进一步纯化地引入所述第二反应器。

公开(公告)号：US07164031B2

公开(公告)日：2007-01-16

申请号：US10487452

申请日：2002-08-30

Applicant: Martin Rudloff ,  Peter Stops ,  Erhard Henkes ,  Helmut Schmidtke ,  Rolf-Hartmuth Fischer ,  Manfred Julius ,  Rolf Lebkücher ,  Karl-Heinz Ross

Inventor： Martin Rudloff ,  Peter Stops ,  Erhard Henkes ,  Helmut Schmidtke ,  Rolf-Hartmuth Fischer ,  Manfred Julius ,  Rolf Lebkücher ,  Karl-Heinz Ross

IPC: C07D207/267

CPC classification number: C07D207/267 ,  C07D201/08

Abstract: A process for continuously preparing 2-pyrrolidone by reacting gamma-butyrolactone with ammonia in the liquid phase in the presence of water, wherein the reaction is carried out at a temperature of from 275 to 300° C. and an absolute pressure of from 140 to 180 bar.

Abstract translation: 一种在水存在下使γ-丁内酯与氨在液相中反应连续制备2-吡咯烷酮的方法，其中反应在275-300℃的温度下进行，绝对压力为140〜 180吧。

公开(公告)号：US20060090994A1

公开(公告)日：2006-05-04

申请号：US10534822

申请日：2003-11-11

Applicant: Hermann Luyken ,  Andreas Ansmann ,  Christoph Benisch ,  Peter Babler ,  Rolf-Hartmuth Fischer ,  Stefan Maixner ,  Johann-Peter Melder

Inventor： Hermann Luyken ,  Andreas Ansmann ,  Christoph Benisch ,  Peter Babler ,  Rolf-Hartmuth Fischer ,  Stefan Maixner ,  Johann-Peter Melder

IPC: B01D3/34 ,  C07C51/44

CPC classification number: C07D201/16

Abstract: A process for purifying crude caprolactam which has been obtained by 1) converting a mixture (I) comprising 6-aminocapronitrile and water to a mixture (II) comprising caprolactam, ammonia, water, high boilers and low boilers in the presence of a catalyst, then 2) removing ammonia from mixture (II) to obtain a mixture (III) comprising caprolactam, water, high boilers and low boilers, then 3) completely or partly removing water from mixture (III) to obtain crude caprolactam (IV) comprising caprolactam, high boilers and low boilers, which comprises a) feeding the crude caprolactam and an inorganic acid which has a boiling point above the boiling point of caprolactam under the distillation conditions of the following steps b) to h) to a first distillation apparatus C1, b) distilling the crude caprolactam and the inorganic acid in the first distillation apparatus C1, and removing a first substream in the bottom region and a second substream in the top region of the distillation apparatus C1, c) feeding the second substream from step b) to a second distillation apparatus C2, d) distilling the second substream from step b) in the second distillation apparatus C2, and removing a first substream in the bottom region and a second substream in the top region of the distillation apparatus C2, e) feeding the first substream from step d) to a third distillation apparatus C3, f) distilling the first substream from d) in the third distillation apparatus C3, and removing a first substream in the bottom region and purified caprolactam in the top region of distillation apparatus C3, and g) feeding the first substream from step f) to the first distillation apparatus C1.

Abstract translation: 一种纯化己内酰胺的方法，其通过以下步骤获得：1）在催化剂存在下，将包含6-氨基己腈和水的混合物（I）转化为包含己内酰胺，氨，水，高锅炉和低沸点的混合物（II） 然后2）从混合物（II）中除去氨以获得包含己内酰胺，水，高锅炉和低锅炉的混合物（III），然后3）从混合物（III）中完全或部分除去水，得到包含己内酰胺的粗己内酰胺（IV） ，高沸点锅炉和低锅炉，其包括：a）在第一蒸馏装置C1的下述步骤b）至h）的蒸馏条件下，将粗己内酰胺和沸点高于己内酰胺沸点的无机酸， b）在第一蒸馏装置C1中蒸馏粗己内酰胺和无机酸，并且除去蒸馏装置C1的顶部区域中的第一子流和顶部区域中的第二子流 c）将来自步骤b）的第二子流进料到第二蒸馏装置C2，d）在第二蒸馏装置C2中蒸馏步骤b）中的第二子流，并且除去第二蒸馏装置C2中的第一子流， e）蒸馏装置C2的顶部区域，e）将来自步骤d）的第一子流进料到第三蒸馏装置C3，f）将第一子流从d）蒸馏到第三蒸馏装置C3中，并且除去底部区域中的第一子流 和在蒸馏装置C3的顶部区域中纯化的己内酰胺，并且g）将来自步骤f）的第一子流进料到第一蒸馏装置C1。

公开(公告)号：US20050267318A1

公开(公告)日：2005-12-01

申请号：US10516923

申请日：2003-06-10

Applicant: Michael Hesse ,  Stephan Schlitter ,  Holger Borchert ,  Markus Schubert ,  Markus Rosch ,  Nils Bottke ,  Rolf-Hartmuth Fischer ,  Alexander Weck ,  Gunther Windecker ,  Gunnar Heydrich

Inventor： Michael Hesse ,  Stephan Schlitter ,  Holger Borchert ,  Markus Schubert ,  Markus Rosch ,  Nils Bottke ,  Rolf-Hartmuth Fischer ,  Alexander Weck ,  Gunther Windecker ,  Gunnar Heydrich

IPC: B01J23/80 ,  C07B61/00 ,  C07C29/149 ,  C07C31/20 ,  C07C31/18

CPC classification number: C07C29/149 ,  C07C31/207

Abstract: The present invention relates to a process for preparing optionally alkyl-substituted 1,4-butanediol by two-stage catalytic hydrogenation in the gas phase of C4-dicarboxylic acids and/or of derivatives thereof having the following steps: a) introducing a gas stream of a C4-dicarboxylic acid or of a derivative thereof at from 200 to 300° C. and from 2 to 60 bar into a first reactor and catalytically hydrogenating it to a product which contains mainly optionally alkyl-substituted 7-butyrolactone; b) converting the product stream into the liquid phase; c) introducing the product stream obtained in this way into a second reactor at a temperature of from 100° C. to 240° C. and a pressure of from 20 to 250 bar and catalytically hydrogenating it in the liquid phase to optionally alkyl-substituted 1,4-butanediol; d) removing the desired product from by-products and any unconverted reactants; e) optionally recycling unconverted intermediates into one or both hydrogenation stages, said hydrogenation stages both using a catalyst which comprises ≦95% by weight, preferably from 5 to 95% by weight, in particular from 10 to 80% by weight, of CuO, and ≧5% by weight, preferably from 5 to 95% by weight, in particular from 20 to 90% by weight, of a support, said second reactor having a higher pressure than said first reactor, and the product mixture removed from said first reactor being introduced without further purification into said second reactor.

Abstract translation: 本发明涉及通过在具有下列物质的C 4 - 二羧酸和/或其衍生物的气相中通过两阶段催化氢化制备任选的烷基取代的1,4-丁二醇的方法 步骤：a）将200-300℃和2-60巴的C 4-14二羧酸或其衍生物的气流引入第一反应器，并将其催化氢化至 主要含有烷基取代的7-丁内酯的产物; b）将产物流转化成液相; c）将以这种方式获得的产物流在100℃至240℃的温度和20至250巴的压力下引入第二反应器，并将其在液相中催化氢化为任选的烷基取代的 1,4-丁二醇 d）从副产物和任何未转化的反应物中除去所需的产物; e）任选地将未转化的中间体再循环到一个或两个氢化阶段中，所述氢化步骤均使用包含<= 95重量％，优选5至95重量％，特别是10至80重量％的CuO ，和> = 5重量％，优选5至95重量％，特别是20至90重量％的载体，所述第二反应器具有比所述第一反应器更高的压力，并将产物混合物从 所述第一反应器不经进一步纯化地引入所述第二反应器。