公开(公告)号：US07217818B2

公开(公告)日：2007-05-15

申请号：US10534802

申请日：2003-11-11

申请人： Rolf-Hartmuth Fischer ,  Hermann Luyken ,  Andreas Ansmann ,  Peter Bassler ,  Christoph Benisch ,  Stefan Maixner ,  Johann-Peter Melder

发明人： Rolf-Hartmuth Fischer ,  Hermann Luyken ,  Andreas Ansmann ,  Peter Bassler ,  Christoph Benisch ,  Stefan Maixner ,  Johann-Peter Melder

IPC分类号： C07D201/16

CPC分类号： C07D201/16 ,  C07D201/08

摘要： A process for removing high boilers from crude caprolactam which comprises high boilers, caprolactam and in some cases low boilers, and which has been obtained by a) reacting 6-aminocapronitrile with water to give a reaction mixture b) removing ammonia and unconverted water from the reaction mixture to obtain crude caprolactam, which comprises c) feeding the crude caprolactam to a distillation apparatus to obtain a first substream via the top as a product and a second substream via the bottom, by setting the pressure in the distillation in such a way that the bottom temperature does not go below 170° C., and adjusting the second substream in such a way that the caprolactam content of the second substream is not less than 10% by weight, based on the entire second substream.

摘要翻译： 一种从粗己内酰胺中除去高锅炉的方法，其包括高锅炉，己内酰胺，在某些情况下是低锅炉，并且通过以下方法获得：a）使6-氨基己腈与水反应得到反应混合物; b）除去氨和未转化的水 反应混合物以获得粗己内酰胺，其包括c）将粗己内酰胺加入到蒸馏装置中，通过顶部获得第一子流作为产物，通过底部通过设置第二子流，通过将蒸馏中的压力设定为使得 底部温度不低于170℃，并且调节第二子流，使得第二子流的己内酰胺含量基于整个第二子流不小于10重量％。

公开(公告)号：US06828457B2

公开(公告)日：2004-12-07

申请号：US10432385

申请日：2003-05-21

申请人： Frank Ohlbach ,  Christoph Benisch ,  Hermann Luyken ,  Andreas Ansmann ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Peter Bassler ,  Stefan Maixner

发明人： Frank Ohlbach ,  Christoph Benisch ,  Hermann Luyken ,  Andreas Ansmann ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Peter Bassler ,  Stefan Maixner

IPC分类号： C07C25334

CPC分类号： C07C209/84 ,  C07C253/34

摘要： A process is provided for reducing the content of a monounsaturated aliphatic amine (III) in a mixture (IV) containing an aminonitrile (I) or a diamine (II), or mixtures thereof, and the amine (III), wherein a) the mixture (IV) is reacted with an anionic nucleophile (V),  which contains a nucleophilic atom selected from the group comprising oxygen, nitrogen and sulfur,  which is capable of taking up an H+ ion to form an acid with a pKa ranging from 7 to 11, measured in water at 25° C., and  which has a relative nucleophilicity, measured in methyl perchlorate/methanol at 25° C.,  ranging from 3.4 to 4.7 when oxygen is the nucleophilic atom,  ranging from 4.5 to 5.8 when nitrogen is the nucleophilic atom, and  ranging from 5.5 to 6.8 when sulfur is the nucleophilic atom,  in an amount ranging from 0.01 to 10 mol per mole of amine (III) in the mixture (IV), to give a mixture (VI), and b) the aminonitrile (I) or the diamine (II), or mixtures thereof, are distilled from the mixture (VI) at a temperature ranging from 50 to 170° C. and a pressure ranging from 0.5 to 100 kPa.

摘要翻译： 提供了一种降低含有氨基腈（I）或二胺（II）或其混合物的混合物（IV）中的单不饱和脂族胺（III）和胺（III）的含量的方法，其中a）混合物 （IV）与阴离子亲核试剂（V）反应，所述阴离子亲核试剂（V）含有选自氧，氮和硫的亲核原子，其能够吸收H +离子以形成pKa范围从 7至11，在25℃的水中测量，并且当氧是亲核原子时，在25℃的甲基高氯酸甲酯/甲醇中测量的范围为3.4至4.7，当氮气为4.5至5.8时，其具有相对的亲核性 是亲核原子，当硫是亲核原子时，其摩尔数为5.5至6.8，其量为每摩尔混合物（IV）中的胺（III）为0.01至10摩尔，得到混合物（Ⅵ），和b） 氨基腈（I）或二胺（II）或其混合物在温度下从混合物（VI）中蒸馏出 e范围为50至170℃，压力范围为0.5至100kPa。

公开(公告)号：US20050222449A1

公开(公告)日：2005-10-06

申请号：US10515281

申请日：2003-05-21

申请人： Stefan Maixner ,  Christoph Benisch ,  Hermann Luyken ,  Peter Bassler ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Andreas Ansmann

发明人： Stefan Maixner ,  Christoph Benisch ,  Hermann Luyken ,  Peter Bassler ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Andreas Ansmann

IPC分类号： C07C209/84 ,  C07C211/09 ,  C07C211/12 ,  C07C253/34 ,  C07C255/09 ,  C07C255/24

CPC分类号： C07C253/34 ,  C07C255/24

摘要： 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 amine (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).

摘要翻译： 含有氨基腈（I）或二胺（II）或二腈（III）或其混合物以及所述胺（IV）的混合物（V）中的脂肪族单不饱和胺（IV）的水平以及所述胺（IV） a）使所述混合物（V）与含有选自氧，氮和硫的亲核原子的阴离子亲核试剂（VI）反应，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：US07115781B2

公开(公告)日：2006-10-03

申请号：US10493504

申请日：2002-10-18

申请人： Andreas Ansmann ,  Christoph Benisch ,  Peter Bassler ,  Rolf-Hartmuth Fischer ,  Stefan Maixner ,  Johann-Peter Melder ,  Hermann Luyken

发明人： Andreas Ansmann ,  Christoph Benisch ,  Peter Bassler ,  Rolf-Hartmuth Fischer ,  Stefan Maixner ,  Johann-Peter Melder ,  Hermann Luyken

IPC分类号： C07C209/62

CPC分类号： B01J23/745

摘要： An oxidic composition which is suitable as a catalyst having divalent and trivalent iron in an atomic ratio of divalent to trivalent iron in the range from greater than 0.5 to 5.5 and oxygen as a counterion to the divalent and trivalent iron. The catalyst composition is useful in the hydrogenation of nitriles to amines.

摘要翻译： 适合作为具有二价和三价铁的二价和三价铁的氧化组合物，其二价至三价铁的原子比在大于0.5至5.5的范围内，氧与二价和三价铁的相反。 催化剂组合物可用于将腈氢化成胺。

公开(公告)号：US07875740B2

公开(公告)日：2011-01-25

申请号：US10493419

申请日：2002-10-18

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

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

IPC分类号： C07C255/03 ,  C07C209/04

CPC分类号： C07C253/30 ,  B01J23/745 ,  B01J23/8892 ,  C07C209/48 ,  C07C211/12 ,  C07C255/24

摘要： 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.

摘要翻译： 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

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

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

IPC分类号： C07C253/34

CPC分类号： C07C253/34 ,  C07C255/24

摘要： 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).

摘要翻译： 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：US20060090994A1

公开(公告)日：2006-05-04

申请号：US10534822

申请日：2003-11-11

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

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

IPC分类号： B01D3/34 ,  C07C51/44

CPC分类号： C07D201/16

摘要： 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.

摘要翻译： 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：US20060041122A1

公开(公告)日：2006-02-23

申请号：US10534802

申请日：2003-11-11

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

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

IPC分类号： C07D201/16

CPC分类号： C07D201/16 ,  C07D201/08

摘要： A process for removing high boilers from crude caprolactam which comprises high boilers, caprolactam and in some cases low boilers, and which has been obtained by a) reacting 6-aminocapronitrile with water to give a reaction mixture b) removing ammonia and unconverted water from the reaction mixture to obtain crude caprolactam, which comprises c) feeding the crude caprolactam to a distillation apparatus to obtain a first substream via the top as a product and a second substream via the bottom, by setting the pressure in the distillation in such a way that the bottom temperature does not go below 170° C., and adjusting the second substream in such a way that the caprolactam content of the second substream is not less than 10% by weight, based on the entire second substream.

摘要翻译： 一种从粗己内酰胺中除去高锅炉的方法，其包括高锅炉，己内酰胺，在某些情况下是低锅炉，并且通过以下方法获得：a）使6-氨基己腈与水反应得到反应混合物; b）除去氨和未转化的水 反应混合物以获得粗己内酰胺，其包括c）将粗己内酰胺加入到蒸馏装置中，通过顶部获得第一子流作为产物，通过底部通过设置第二子流，通过将蒸馏中的压力设定为使得 底部温度不低于170℃，并且调节第二子流，使得第二子流的己内酰胺含量基于整个第二子流不小于10重量％。

公开(公告)号：US07501047B2

公开(公告)日：2009-03-10

申请号：US10534822

申请日：2003-11-11

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

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

IPC分类号： B01D3/14 ,  B01D3/34 ,  C07D201/08 ,  C07D201/16

CPC分类号： C07D201/16

摘要： The disclosure relates to a process for purifying crude caprolactam. The process involves converting a first mixture of 6-amino capronitrile and water to a second mixture of caprolactam ammonia, water, high boilers and low boilers using a catalyst. The ammonia is removed from the second mixture to obtain a third mixture. Water is removed from the third mixture to give crude caprolactam, high boiler and low boilers. Purified caprolactam is then obtained by a series of distillation steps.

摘要翻译： 本公开涉及纯化己内酰胺的方法。 该方法包括使用催化剂将6-氨基己腈和水的第一混合物转化成己内酰胺氨，水，高锅炉和低锅炉的第二混合物。 从第二混合物中除去氨以获得第三混合物。 从第三混合物中除去水，得到粗己内酰胺，高锅炉和低锅炉。 然后通过一系列蒸馏步骤获得纯化的己内酰胺。

公开(公告)号：US06896772B2

公开(公告)日：2005-05-24

申请号：US10297051

申请日：2001-06-02

申请人： Hermann Luyken ,  Frank Ohlbach ,  Stefan Maixner ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Peter Bassler ,  Andreas Ansmann

发明人： Hermann Luyken ,  Frank Ohlbach ,  Stefan Maixner ,  Rolf-Hartmuth Fischer ,  Johann-Peter Melder ,  Peter Bassler ,  Andreas Ansmann

IPC分类号： C07D223/10 ,  B01D3/00 ,  C01C1/10 ,  C07D201/08 ,  C07D201/16 ,  B01D5/00 ,  C01C1/00

CPC分类号： C01C1/10 ,  C07D201/08 ,  C07D201/16

摘要： A process for distillative removal of ammonia from solutions (I) which include a lactam and ammonia comprises effecting said removal in a distillation apparatus (a) at an absolute pressure of less than 10 bar.

摘要翻译： 从包括内酰胺和氨的溶液（I）中蒸馏除去氨的方法包括在绝对压力小于10巴的蒸馏装置（a）中进行所述除去。