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    Purification of caprolactam
    1.
    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 amine and a nitrile
    3.
    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。

    Method for reducing the content of an unsaturated amine in a mixture containing an amino nitrile, a diamine, a dinitrile or mixtures thereof
    4.
    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 reducing the content of an unsaturated amine in a mixture containing an amino nitrile, a diamine, a dinitrile or mixtures thereof
    6.
    发明授权
    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：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。

    Method for purifying caprolactam
    7.
    发明申请
    Method for purifying caprolactam 失效
    己内酰胺纯化方法

    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。

    Method for purifying caprolactam
    9.
    发明申请
    Method for purifying caprolactam 有权
    己内酰胺纯化方法

    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％。