公开(公告)号：US08278489B2

公开(公告)日：2012-10-02

申请号：US12809653

申请日：2008-12-10

申请人： Petr Kubanek ,  Wolfgang Mägerlein ,  Ekkehard Schwab ,  Johann-Peter Melder ,  Manfred Julius

发明人： Petr Kubanek ,  Wolfgang Mägerlein ,  Ekkehard Schwab ,  Johann-Peter Melder ,  Manfred Julius

IPC分类号： C07C209/16 ,  C07D265/30 ,  C07D295/03 ,  C07D241/04 ,  B01J23/835 ,  B01J37/03 ,  B01J37/18

CPC分类号： B01J23/835 ,  B01J23/002 ,  B01J37/03 ,  B01J37/18 ,  B01J2523/00 ,  C07C209/16 ,  C07C213/02 ,  C07D295/02 ,  C07D295/06 ,  C07C217/08

摘要： Processes for preparing an amine, which processes comprise: reacting a reactant selected from the group consisting of primary alcohols, secondary alcohols, aldehydes, ketones, and mixtures thereof, with hydrogen and a nitrogen compound selected from the group consisting of ammonia, primary amines, secondary amines and mixtures thereof, in the presence of a zirconium dioxide-, copper- and nickel-containing catalyst; wherein the catalyst comprises a catalytically active composition which comprises, before reduction with hydrogen, oxygen compounds of zirconium, copper, nickel and tin, and 0.5 to 8.0% by weight of an oxygen compound of cobalt, calculated as CoO, and wherein the catalytically active composition does not comprise any ruthenium.

摘要翻译： 用于制备胺的方法，该方法包括：将选自伯醇，仲醇，醛，酮及其混合物的反应物与氢和选自以下的氮化合物反应：氨，伯胺， 仲胺及其混合物，在二氧化锆，含铜和镍的催化剂存在下; 其中所述催化剂包含催化活性组合物，所述催化活性组合物在用氢还原之前包括锆，铜，镍和锡的氧化合物和0.5至8.0重量％的作为CoO计算的钴的氧化合物，并且其中催化活性 组合物不包含任何钌。

公开(公告)号：US08246793B2

公开(公告)日：2012-08-21

申请号：US12443563

申请日：2007-09-12

申请人： Helmut Schmidtke ,  Oliver Buβmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

发明人： Helmut Schmidtke ,  Oliver Buβmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

IPC分类号： B01D3/14 ,  C07D295/02

CPC分类号： C07D295/027

摘要： Processes for the continuous fractional distillation of a mixture comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water from a reaction of diethylene glycol (DEG) with ammonia, the process comprising: (i) separating off ammonia from the mixture at a top of a first distillation column K10; (ii) feeding a bottom fraction from the first distillation column to a second distillation column K20, wherein water and an organic product are separated off at a top of the second distillation column at a top temperature of 45 to 198° C. and a pressure in the range from 0.1 to 15 bar; (iii) feeding a bottom fraction from the second distillation column to a third distillation column K30, wherein morpholine and an organic product having a boiling point of 190° C. (1.013 bar) are separated off at a bottom of the third distillation column, and (iv) feeding the morpholine-comprising stream from the third distillation column to a fourth column K40, wherein morpholine is separated off at a side offtake of the fourth column, an organic product having a boiling point of ≦128° C. (1.013 bar) is separated off at a top of the fourth distillation column and an organic product having a boiling point of ≧128° C. (1.013 bar) is separated off at a bottom of the fourth distillation column.

摘要翻译： 用于从二甘醇（DEG）与氨的反应连续分馏含有吗啉（MO），单氨基二甘醇（ADG），氨和水的混合物的方法，该方法包括：（i）在 第一蒸馏塔K10顶部; （ii）将底部馏分从第一蒸馏塔进料到第二蒸馏塔K20，其中在顶部温度为45至198℃的温度下，在第二蒸馏塔的顶部分离出水和有机产物，并将压力 在0.1至15巴的范围内; （iii）将第二蒸馏塔的塔底馏分进料到第三蒸馏塔K30，其中将吗啉和沸点<140℃（1.013巴）的有机产物在选自顶部和 在第三蒸馏塔的底部分离出第三蒸馏塔的侧馏分和单胺二醇和沸点> 190℃（1.013巴）的有机产物，和（iv）将含吗啉 从第三蒸馏塔到第四塔K40的流，其中吗啉在第四塔的出口侧分离出，沸点为＆amp; NlE的有机产物为128℃（1.013巴）在顶部分离 的第四蒸馏塔和沸点为≧128℃的有机产物（1.013巴）在第四蒸馏塔的底部分离。

公开(公告)号：US08197646B2

公开(公告)日：2012-06-12

申请号：US12443573

申请日：2007-09-12

申请人： Helmut Schmidtke ,  Oliver Buβmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

发明人： Helmut Schmidtke ,  Oliver Buβmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

IPC分类号： B01D3/14 ,  C07D295/02

CPC分类号： C07D295/027 ,  Y10S203/20

摘要： Process for the continuous fractional distillation of mixtures including morpholine (MO), monoaminodiglycol (ADG), ammonia and water obtained by reaction of diethylene glycol (DEG) with ammonia, which includes separating off ammonia at the top of a first distillation column K10, feeding the bottoms from K10 to a second distillation column K20 in which water and organic products are separated off at the top at a temperature at the top in the range from 45 to 198° C. and a pressure in the range from 0.1 to 15 bar, feeding the bottoms from K20 to a third distillation column K30 in which MO and organic products having a boiling point of 190° C. (1.013 bar) are separated off at the bottom, feeding the MO including stream which is separated off at the top or at a side offtake of the column K30 to a fourth column K40 in which organic products having a boiling point of ≦128° C. (1.013 bar) are separated off at the top and MO and organic products having a boiling point of ≧128° C. (1.013 bar) are separated off at the bottom and the bottoms from K40 are fed to a fifth distillation column K55 in which MO is separated off at the top and organic products having a boiling point of ≧128° C. (1.013 bar) are separated off at the bottom.

摘要翻译： 用于连续分馏包括吗啉（MO），单氨基二甘醇（ADG），氨和二乙二醇（DEG）与氨反应得到的水的混合物的方法，其包括在第一蒸馏塔K10的顶部分离出氨， 从K10到第二蒸馏塔K20的底部，其中水和有机产物在顶部的温度在45至198℃的范围内分离，压力在0.1至15巴的范围内， 将塔底物从K20进料到第三蒸馏塔K30，其中MO和沸点<140℃（1.013巴）的有机产物在顶部或侧面被分离出来，ADG和具有沸点的有机产物 在底部分离> 190℃（1.013巴）的点，将包含在柱K30的顶部或侧面分离出的MO的MO进料到第四塔K40，其中有机产物具有 沸点 从顶部分离出128℃（1.013巴），在底部分离出MO和沸点为128℃（1.013巴）的有机产物，将来自K40的底部进料至 其中MO在顶部分离出的第五个蒸馏塔K55和沸点为≧128℃（1.013巴）的有机产物在底部分离。

公开(公告)号：US20120024689A1

公开(公告)日：2012-02-02

申请号：US12443581

申请日：2007-09-12

申请人： Helmut Schmidtke ,  Oliver Bußmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

发明人： Helmut Schmidtke ,  Oliver Bußmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

IPC分类号： B01D3/34 ,  B01D3/14

CPC分类号： C07C213/10 ,  C07D295/023 ,  C07C217/08

摘要： Processes for the continuous fractional distillation of a mixture comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water from a reaction of diethylene glycol (DEG) with ammonia, the process comprising: (i) separating off ammonia from the mixture at a top of a first distillation column K10; (ii) feeding a bottom fraction from the first distillation column to a second distillation column K20, wherein water and an organic product are separated off at a top of the second distillation column at a top temperature of 45 to 198° C. and a pressure in the range from 0.1 to 15 bar; (iii) feeding a bottom fraction from the second distillation column to a third distillation column K30, wherein morpholine and an organic product having a boiling point of 190° C. (1.013 bar) are separated off at a bottom of the third ditillation column, and (iv) feeding the morpholine-comprising stream from the third distillation column to a fourth column K40, wherein morpholine is separated off at a side offtake of the fourth column, an organic product having a boiling point of ≦128° C. (1.013 bar) is separated off at a top of the fourth distillation column and an organic product having a boiling point of ≧128° C. (1.013 bar) is separated off at a bottom of the fourth distillation column.

摘要翻译： 用于从二甘醇（DEG）与氨的反应连续分馏含有吗啉（MO），单氨基二甘醇（ADG），氨和水的混合物的方法，该方法包括：（i）在 第一蒸馏塔K10顶部; （ii）将底部馏分从第一蒸馏塔进料到第二蒸馏塔K20，其中在顶部温度为45至198℃的温度下，在第二蒸馏塔的顶部分离出水和有机产物，并将压力 在0.1至15巴的范围内; （iii）将第二蒸馏塔的塔底馏分进料到第三蒸馏塔K30，其中将吗啉和沸点<140℃（1.013巴）的有机产物在选自顶部和 在第三蒸馏塔的底部分离出第三蒸馏塔的侧馏分和单胺二醇和沸点> 190℃（1.013巴）的有机产物，（iv）将含吗啉 从第三蒸馏塔到第四塔K40的流，其中吗啉在第四塔的出口侧分离出，沸点为＆amp; NlE的有机产物为128℃（1.013巴）在顶部分离 的第四蒸馏塔和沸点为≧128℃的有机产物（1.013巴）在第四蒸馏塔的底部分离。

公开(公告)号：US20100274009A1

公开(公告)日：2010-10-28

申请号：US12809665

申请日：2008-12-10

申请人： Petr Kubanek ,  Wolfgang Mägerlein ,  Ekkehard Schwab ,  Johann-Peter Melder ,  Manfred Julius

发明人： Petr Kubanek ,  Wolfgang Mägerlein ,  Ekkehard Schwab ,  Johann-Peter Melder ,  Manfred Julius

IPC分类号： C07D265/30 ,  C07D211/00 ,  C07C209/00 ,  B01J27/185 ,  B01J23/72

CPC分类号： B01J23/825 ,  B01J23/002 ,  B01J23/8474 ,  B01J23/888 ,  B01J37/03 ,  B01J37/18 ,  B01J2523/00 ,  C07C209/16 ,  C07C213/02 ,  C07C213/06 ,  C07D295/02 ,  C07D295/08 ,  B01J2523/17 ,  B01J2523/48 ,  B01J2523/51 ,  B01J2523/847 ,  B01J2523/69 ,  B01J2523/68 ,  B01J2523/32 ,  B01J2523/56 ,  C07C211/10 ,  C07C215/10 ,  C07C217/08 ,  C07C217/28

摘要： Processes for preparing an amine, the processes comprising: reacting a reactant selected from the group consisting of primary alcohols, secondary alcohols, aldehydes, ketones, and mixtures thereof, with hydrogen and a nitrogen compound selected from the group consisting of ammonia, primary amines, secondary amines and mixtures thereof, in the presence of a zirconium dioxide-, copper- and nickel-containing catalyst; wherein the catalyst comprises a catalytically active composition which comprises, before reduction with hydrogen, oxygen compounds of zirconium, copper, nickel, no oxygen compounds of cobalt, and 0.2 to 5.0% by weight of at least one oxygen compound of phosphorus or gallium, calculated as H3PO4 and Ga2O3 respectively.

摘要翻译： 用于制备胺的方法，所述方法包括：将选自伯醇，仲醇，醛，酮及其混合物的反应物与氢和选自以下的氮化合物反应：氨，伯胺， 仲胺及其混合物，在二氧化锆，含铜和镍的催化剂存在下; 其中所述催化剂包含催化活性组合物，其在用氢还原之前包括锆，铜，镍的氧化合物，不含钴的氧化合物和0.2至5.0重量％的至少一种磷或镓的氧化合物，计算 分别为H3PO4和Ga2O3。

公开(公告)号：US20100084258A1

公开(公告)日：2010-04-08

申请号：US12443573

申请日：2007-09-12

申请人： Helmut Schmidtke ,  Oliver Bussmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

发明人： Helmut Schmidtke ,  Oliver Bussmann ,  Ralph Versch ,  Udo Rheude ,  Uwe Leyk ,  Manfred Julius ,  Martin Rudloff ,  Erhard Henkes

IPC分类号： B01D3/14

CPC分类号： C07D295/027 ,  Y10S203/20

摘要： Processes for the continuous fractional distillation of a mixture comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water from a reaction of diethylene glycol (DEG) with ammonia, the processes comprising: (i) separating off ammonia from the mixture at a top of a first distillation column K10; (ii) feeding a bottom fraction from K10 to a second distillation column K20 in which water and organic products are separated off at the top at a temperature at the top in the range from 45 to 198° C. and a pressure in the range from 0.1 to 15 bar; (iii) feeding a bottom fraction from K20 to a third distillation column K30 in which MO and organic products having a boiling point of 190° C. (1.013 bar) are separated off at the bottom, and (iv) feeding the MO-comprising stream which is separated off at the top or at a side offtake of the column K30 to a fourth column K40 in which organic products having a boiling point of ≦128° C. (1.013 bar) are separated off at the top and MO and organic products having a boiling point of ≧128° C. (1.013 bar) are separated off at the bottom and the bottoms from K40 are fed to a fifth distillation column K55 in which MO is separated off at the top and organic products having a boiling point of ≧128° C. (1.013 bar) are separated off at the bottom.

摘要翻译： 由二甘醇（DEG）与氨的反应连续分馏含有吗啉（MO），单氨基二甘醇（ADG），氨和水的混合物的方法，该方法包括：（i）在 第一蒸馏塔K10顶部; （ii）将底部馏分从K10进料至第二蒸馏塔K20，其中水和有机产物在顶部分离出，顶部温度为45-98℃，压力范围为 0.1至15巴; （iii）从K20向第三蒸馏塔K30供应底部馏分，其中MO和沸点<140℃（1.013巴）的有机产物在顶部或侧面被分离，并且ADG和有机物 沸点> 190℃（1.013巴）的产物在底部被分离，并且（iv）将在柱K30的顶部或侧面分离出的含MO的料流送入到 第四列K40，其中沸点为＆nlE的有机产物为128℃（1.013巴），顶部分离出MO，沸点为≧128℃（1.013巴）的有机产物被分离出 在底部，将来自K40的塔底物进料至第五蒸馏塔K55，其中MO在顶部被分离出，沸点为128℃（1.013巴）的有机产物在底部被分离开。

公开(公告)号：US20080200726A1

公开(公告)日：2008-08-21

申请号：US11993891

申请日：2006-06-21

申请人： Frank Haese ,  Joachim Wulff-Doring ,  Ulrich Kohler ,  Peter Gaa ,  Frank-Friedrich Pape ,  Johann-Peter Melder ,  Manfred Julius

发明人： Frank Haese ,  Joachim Wulff-Doring ,  Ulrich Kohler ,  Peter Gaa ,  Frank-Friedrich Pape ,  Johann-Peter Melder ,  Manfred Julius

IPC分类号： C07C211/44

CPC分类号： C07C209/18 ,  Y02P20/582 ,  C07C211/45

摘要： Processes comprising: providing an aromatic alcohol; and reacting the aromatic alcohol with ammonia at a temperature of 80 to 350° C. in the presence of hydrogen and a heterogeneous catalyst to form a crude reaction product comprising a corresponding primary aromatic amine, wherein the heterogeneous catalyst comprises a catalytically active composition which, prior to reduction with hydrogen, comprises 90 to 99.8% by weight of zirconium dioxide (ZrO2), 0.1 to 5.0% by weight of an oxygen-comprising compound of palladium, and 0.1 to 5.0% by weight of an oxygen-comprising compound of platinum.

摘要翻译： 方法包括：提供芳族醇; 并在80至350℃的温度下在氢气和非均相催化剂存在下使芳族醇与氨反应形成包含相应的伯芳族胺的粗反应产物，其中非均相催化剂包含催化活性组合物， 在用氢还原之前，包含90-99.8重量％的二氧化锆（ZrO 2/2），0.1-5.0重量％的含氧化合物的钯和0.1-5.0重量％ 的含氧化合物的铂。

公开(公告)号：US20070270614A1

公开(公告)日：2007-11-22

申请号：US10573185

申请日：2004-09-24

申请人： Werner Reutemann ,  Rolf Wambsganss ,  Frank Poplow ,  Theodor Weber ,  Karl-Heinz Ross ,  Manfred Julius

发明人： Werner Reutemann ,  Rolf Wambsganss ,  Frank Poplow ,  Theodor Weber ,  Karl-Heinz Ross ,  Manfred Julius

IPC分类号： C07C209/14

CPC分类号： C07C209/16 ,  C07C211/04

摘要： The invention relates to a process for preparing methylamines by gas-phase reaction of methanol and ammonia as starting materials at a pressure in the range from 15 to 30 bar in the presence of heterogeneous catalyst. The starting materials are vaporized in one or more heat exchangers (1, 2, 3), superheated to produce a feed gas stream and subsequently fed into a reactor (4), with the mixing of the starting materials being able to be carried out in the feed stream to one of the heat exchangers (1, 2, 3) or at any desired position in a heat exchanger (1, 2, 3). A product gas stream comprising monomethylamine, dimethylamine and trimethylamine and also reaction by-products is taken off from the reactor (4). To control the reactor inlet temperature of the starting materials to a temperature in the range from 360° C. to 370° C., all or some of the feed gas stream or the product gas stream is passed through an adjustable valve (5) in order to vary the pressure and thus the condensation temperature.

摘要翻译： 本发明涉及通过甲醇和氨作为起始原料在非均相催化剂存在下在15至30巴的压力下气相反应制备甲胺的方法。 起始材料在一个或多个热交换器（1,2,3）中蒸发，过热以产生进料气流，并随后进料到反应器（4）中，原料的混合能够进行 到一个热交换器（1,2,3）或在热交换器（1,2,3）中的任何期望位置的进料流。 从反应器（4）中取出包含一甲胺，二甲胺和三甲胺以及反应副产物的产物气流。 为了将原料的反应器入口温度控制在360℃至370℃的温度范围内，所有或一些进料气流或产物气流通过可调节阀（5），其中 以改变压力，从而改变冷凝温度。

公开(公告)号：US07164031B2

公开(公告)日：2007-01-16

申请号：US10487452

申请日：2002-08-30

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

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

IPC分类号： C07D207/267

CPC分类号： C07D207/267 ,  C07D201/08

摘要： 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.

摘要翻译： 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：US20050252761A1

公开(公告)日：2005-11-17

申请号：US10524084

申请日：2003-08-08

申请人： Frank Funke ,  Thomas Hill ,  Jobst Watzdorf ,  Wolfgang Mattmann ,  Wolfgang Harder ,  Erhard Henkes ,  Gerd Littmann ,  Manfred Julius

发明人： Frank Funke ,  Thomas Hill ,  Jobst Watzdorf ,  Wolfgang Mattmann ,  Wolfgang Harder ,  Erhard Henkes ,  Gerd Littmann ,  Manfred Julius

IPC分类号： C07C209/86 ,  B01D3/14 ,  C07C209/84 ,  C07C211/36 ,  B01D3/00

CPC分类号： B01D3/141 ,  B01D3/146 ,  C07C209/84 ,  Y10S203/20 ,  C07C211/36

摘要： The invention relates to a process for recovering 3-aminomethyl-3,5,5-trimethylcyclohexylamine(isophoronediamine, IPDA) having a cis/trans isomer ratio of at least 73/27 by fractional distillation, which comprises the following steps: a) providing IPDA in a cis/trans isomer ratio of

摘要翻译： 本发明涉及通过分馏回收顺式/反式异构体比为73/27的3-氨基甲基-3,5,5-三甲基环己胺（异佛尔酮二胺，IPDA）的方法，其包括以下步骤：a）提供 IPDA以顺式/反式异构体比为<73/27; b）将IPDA进料到具有内部的蒸馏塔的中间区域，并在该蒸馏塔中在5-300℃的温度和10-2000mbar的压力下蒸馏该IPDA; c）任选地通过在至少一个另外的塔中蒸馏来进一步纯化通过步骤b）获得的IPDA; 其中步骤b）和c）将步骤a）中使用的IPDA分离成至少五个分数ia）至iv）：ia）沸点低于tans-IPDA的一部分杂质的有机比例，ib）水分比 的沸点低于反式 - IPDA的杂质的一部分，ii）沸点高于顺式-IPDA的一部分杂质，iii）顺式/反式异构体比为> 73/27的IPDA馏分和iv） 顺式/反式异构体比例<66/34的IPDA级分。