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    Method for reducing the content of an unsaturated amine in a mixture containing an amine and a nitrile
    2.
    发明授权
    Method for reducing the content of an unsaturated amine in a mixture containing an amine and a nitrile 失效
    减少含有胺和腈的混合物中不饱和胺含量的方法

    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。

    Preparation of cyclic lactams
    5.
    发明授权
    Preparation of cyclic lactams 有权
    制备环状内酰胺

    公开(公告)号：US06683178B2

    公开(公告)日：2004-01-27

    申请号：US10257877

    申请日：2002-10-17

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

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

    IPC分类号： C07D20108

    CPC分类号： C07D201/08 ,  C07D201/16

    摘要： The invention relates to a method for producing cyclic lactams of formula (II) by reacting a compound (I) of formula (I) with water in the presence of an organic, liquid dilution agent in the liquid phase. In formula (II), n and m respectively can have the values 0, 1, 2, 3, 4, 5, 6, 7, 8 and 9 and the sum of n+m is at least 3, preferably at least 4 and R1 and R2 represent C1-C6 alkyl, C5-C7 cycloalkyl or C6-C12 aryl groups. In formula (I), R1, R2, m and n are defined as above and R represents nitrile, carboxylic acid amide and carboxylic acid groups. The inventive method is characterized in that a) compound (I) is reacted with water in the liquid phase in the presence of an organic, liquid dilution agent (III) to form a mixture (IV) containing a lactam (II) and said mixture (IV) is subjected to an aqueous treatment to obtain a two-phase system.

    摘要翻译： 本发明涉及在液相中有机液体稀释剂存在下使式（I）化合物（I）与水反应制备式（II）的环状内酰胺的方法。 在式（II）中，n和m分别具有0,1,2,3,4,5,6,7,8和9的值，并且n + m的和至少为3，优选至少为4，并且 R 1和R 2代表C 1 -C 6烷基，C 5 -C 7环烷基或C 6 -C 12芳基。 在式（I）中，R 1，R 2，m和n如上定义，R代表腈，羧酸酰胺和羧酸基团。 本发明的方法的特征在于：a）化合物（I）在液相中在有机液体稀释剂（III）的存在下与水反应，形成含有内酰胺（II）的混合物（IV），所述混合物 （IV）进行水处理以获得两相体系。

    Purification of caprolactam
    6.
    发明授权
    Purification of caprolactam 有权
    己内酰胺的纯化

    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％。

    Method for reducing the content of an unsaturated amine in a mixture containing an amino nitrile, a diamine, a dinitrile or mixtures thereof
    8.
    发明申请
    Method for reducing the content of an unsaturated amine in a mixture containing an amino nitrile, a diamine, a dinitrile or mixtures thereof 有权
    降低含氨基腈，二胺，二腈或其混合物的混合物中不饱和胺含量的方法

    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。

    Method for removing 6-aminocapronitrile from mixtures that contain 6-aminocapronitrile, adipodinitrile and hexamethylenediamine
    9.
    发明授权
    Method for removing 6-aminocapronitrile from mixtures that contain 6-aminocapronitrile, adipodinitrile and hexamethylenediamine 失效
    从含有6-氨基己腈，己二胺和六亚甲基二胺的混合物中除去6-氨基己腈的方法

    公开(公告)号：US06972075B2

    公开(公告)日：2005-12-06

    申请号：US10311376

    申请日：2001-06-13

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

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

    IPC分类号： C07C209/48 ,  C07C253/34 ,  C07C255/03 ,  C07C255/24 ,  B01D3/14

    CPC分类号： C07C253/34 ,  C07C209/48 ,  Y10S203/20 ,  C07C255/24

    摘要： The invention relates to a method for removing, by distillation, 6-aminocapronitrile from mixtures that contain 6-aminocapronitrile, adipodinitrile and hexamethylenediamine, by a) removing the hexamethylenediamine from the mixture while obtaining a mixture (I) that has a hexamethylenediamine content of less than 1 wt. -%, b) removing completely or partially the 6-aminocapronitrile from mixture (I) while obtaining a mixture (II) whose content in substances that have a higher boiling point as 6-aminocapronitrile under distillation conditions and that cannot be formed by dimerization reactions when 6-aminocapronitrile is thermally treated is less than 1 wt. -%, and c) completely or partially removing from mixture (II) the hexamethylenediamine that might be present while obtaining a mixture (IV) whose hexamethylenediamine content is higher than that of mixture (II), and a mixture (V) whose hexamethylenediamine content is lower than that of mixture (II).

    摘要翻译： 本发明涉及一种通过以下方法：从含有6-氨基己腈，己二腈和六亚甲基二胺的混合物中蒸馏除去6-氨基己腈，方法是a）从混合物中除去六亚甲基二胺，同时得到六亚甲基二胺含量少的混合物（I） 超过1wt。 - ％，b）从混合物（I）中完全或部分地除去6-氨基己腈，同时得到其在蒸馏条件下具有较高沸点的物质中的含量为6-氨基己腈的混合物（II），并且不能通过二聚反应形成 当6-氨基己腈被热处理时小于1wt。 - ％，和c）在获得六亚甲基二胺含量高于混合物（II）的混合物（Ⅳ）的同时，可能存在的六亚甲基二胺的混合物（II）完全或部分地除去，和（VI）的六亚甲基二胺含量 低于混合物（II）。

    Method for generating catalysts
    10.
    发明授权
    Method for generating catalysts 失效
    生成催化剂的方法

    公开(公告)号：US06905997B2

    公开(公告)日：2005-06-14

    申请号：US10380550

    申请日：2001-09-20

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

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

    IPC分类号： B01J23/86 ,  B01J23/94 ,  B01J38/52 ,  C07B61/00 ,  C07C209/48 ,  C07C211/12 ,  B01J38/50 ,  B01J38/10

    CPC分类号： B01J38/52 ,  B01J23/94 ,  C07C209/48 ,  Y02P20/584

    摘要： A process is provided for the regeneration of a heterogeneous catalyst used for the preparation of compounds containing NH2 groups by the hydrogenation, with hydrogen, of compounds containing at least one unsaturated carbon-nitrogen bond, wherein a) the feed of the compound to be hydrogenated is stopped and b) the heterogeneous catalyst is treated with a compound of the formula R1R2N—CO—R3  (I), in which R1 is hydrogen or C1-C4 alkyl and R2, R3 independently of one another are each hydrogen or C1-C4 alkyl or together are a C3-C6 alkylene group, or mixtures of such compounds, at a pressure ranging from 0.1 to 30 MPa and a temperature ranging from 100 to 300° C., with the proviso that the compound of formula (I) is in liquid form during the treatment.

    摘要翻译： 提供了一种用于通过氢化含有至少一个不饱和碳 - 氮键的化合物再生用于制备含有NH 2基团的化合物的非均相催化剂的再生方法，其中a） 待氢化的化合物的进料停止，b）用式<β的化合物处理非均相催化剂。在线式描述=“In-line Formulas”end =“lead”→> （I），<？in-line-formula description =“In-line Formulas”end =“tail 其中R 1是氢或C 1 -C 4烷基，R 2，R 2，R 3， 各自独立地为氢或C 1 -C 4烷基，或者一起为C 3 -C 3 亚烷基或这些化合物的混合物，在0.1至30MPa的压力和100至300℃的温度范围内，条件是式（I）化合物为 液体 在治疗过程中形成。