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    PROCESS FOR THE PREPARATION OF AN N-ALKYL LACTAM WITH IMPROVED COLOUR QUALITY
    33.
    发明申请
    PROCESS FOR THE PREPARATION OF AN N-ALKYL LACTAM WITH IMPROVED COLOUR QUALITY 审中-公开
    制备具有改善颜色质量的N-ALKYL LACTAM的方法

    公开(公告)号：US20090182139A1

    公开(公告)日：2009-07-16

    申请号：US12296115

    申请日：2007-03-29

    Applicant: Tobias Wabnitz ,  Rolf Pinkos ,  Karl Ott

    Inventor： Tobias Wabnitz ,  Rolf Pinkos ,  Karl Ott

    IPC: C07D201/08 ,  C07D207/267 ,  C07D201/02 ,  C07D211/06

    CPC classification number: C07D201/18 ,  C07D207/267 ,  C07D211/76 ,  C07D223/10

    Abstract: A process for preparing an N-alkyllactam with improved color quality, wherein from 0.01 to 10% by weight of a C1-10-alcohol or a compound which releases from 0.01 to 10% by weight of a C1-10-alcohol is added to the N-alkyllactam.A mixture comprising at least 99.0% by weight of an N-alkyllactam and in the range from 100 to 5000 ppm by weight of a C1-10-alcohol or of an acetal, aminal or of an orthoester which releases in the range from 100 to 5000 ppm by weight of a C1-10-alcohol.

    Abstract translation: 一种制备具有改进的颜色质量的N-烷基内酰胺的方法，其中将0.01至10重量％的C 1-10醇或从0.01至10重量％的C 1-10醇释放的化合物加入到 N-烷基内酰胺。 一种混合物，其包含至少99.0重量％的N-烷基内酰胺和100-5000重量ppm的C1-10醇或缩醛，缩醛或原酸酯，其释放范围为100至 5000重量ppm的C 1-10醇。

    Method for making caprolactam from impure 6-aminocapronitrile
    34.
    发明授权
    Method for making caprolactam from impure 6-aminocapronitrile 失效
    从不纯的6-氨基己腈制备己内酰胺的方法

    公开(公告)号：US07390897B2

    公开(公告)日：2008-06-24

    申请号：US11083715

    申请日：2006-02-10

    Applicant: Alan M. Allgeier ,  John J. Ostermaier ,  Sourav K. Sengupta

    Inventor： Alan M. Allgeier ,  John J. Ostermaier ,  Sourav K. Sengupta

    IPC: C07D201/08

    CPC classification number: C07D223/10

    Abstract: The invention relates to the field of production of lactams from aminonitriles, and in particular to the production of ε-caprolactam by the vapor phase hydrolytic cyclization of 6-aminocapronitrile. A crude liquid caprolactam comprising ε-caprolactam (CL), 6-aminocapronitrile (ACN) and water obtained from a vapor phase cyclization reaction of ACN is contacted with hydrogen in the presence of a hydrogenation catalyst to convert the ACN in the crude liquid caprolactam to a product comprising hexamethylenediamine (HMD) and hexamethyleneimine (HMI). Tetrahydroazepine (THA) in the crude liquid caprolactam is converted to HMI during this hydrogenation. The HMD and HMI have lower boiling points compared to ACN and thus they are more easily separated from CL in the subsequent distillation operations. Thus a process to make CL from ACN with fewer distillation stages, and with lower pressure drop and lower base temperature, is accomplished.

    Abstract translation: 本发明涉及由氨基腈生产内酰胺的领域，特别涉及通过6-氨基己腈的气相水解环化生产ε-己内酰胺。 包含ε-己内酰胺（CL），6-氨基己腈（ACN）和由ACN的气相环化反应获得的水的粗液体己内酰胺在氢化催化剂存在下与氢气接触，将粗液体己内酰胺中的ACN转化为 包含六亚甲基二胺（HMD）和六亚甲基亚胺（HMI）的产品。 粗制液体己内酰胺中的四氢吖庚因（THA）在该氢化期间转化为HMI。 与ACN相比，HMD和HMI具有较低的沸点，因此在随后的蒸馏操作中它们更容易与CL分离。 因此，实现了具有较少蒸馏阶段以及较低压降和较低基础温度的来自ACN的CL的方法。

    Preparation of lactams from aliphatic .alpha..omega.-dinitriles
    37.
    发明授权
    Preparation of lactams from aliphatic .alpha..omega.-dinitriles 失效
    从脂肪族αω-二腈制备内酰胺

    公开(公告)号：US6077955A

    公开(公告)日：2000-06-20

    申请号：US108728

    申请日：1998-07-01

    Applicant: Robert Di Cosimo ,  Robert Donald Fallon ,  John Edward Gavagan ,  Frank Edward Herkes

    Inventor： Robert Di Cosimo ,  Robert Donald Fallon ,  John Edward Gavagan ,  Frank Edward Herkes

    IPC: C07C255/19 ,  C07C255/23 ,  C07D201/08 ,  C07D207/26 ,  C07D211/76 ,  C07D223/10 ,  C12N9/78 ,  C12N9/88 ,  C12P13/00 ,  C12P17/10 ,  C07D211/60 ,  C07D207/00

    CPC classification number: C07D211/76 ,  C07C255/19 ,  C07C255/23 ,  C07D201/08 ,  C07D207/26 ,  C07D223/10 ,  C12N9/78 ,  C12N9/88 ,  C12P13/002 ,  C12P13/02 ,  C12P17/10 ,  C12R1/01 ,  Y02P20/52

    Abstract: A process for the preparation of five-membered or six-membered ring lactams from aliphatic .alpha.,.omega.-dinitriles has been developed. In the process an aliphatic .alpha.,.omega.-dinitrile is first converted to an ammonium salt of an .omega.-nitrilecarboxylic acid in aqueous solution using a catalyst having an aliphatic nitrilase (EC 3.5.5.7) activity, or a combination of nitrile hydratase (EC 4.2.1.84) and amidase (EC 3.5.1.4) activities. The ammonium salt of the .omega.-nitrilecarboxylic acid is then converted directly to the corresponding lactam by hydrogenation in aqueous solution, without isolation of the intermediate .omega.-nitrilecarboxylic acid or .omega.-aminocarboxylic acid. When the aliphatic .alpha.,.omega.-dinitrile is also unsymmetrically substituted at the .alpha.-carbon atom, the nitrilase produces the .omega.-nitrilecarboxylic acid ammonium salt resulting from hydrolysis of the .omega.-nitrile group with greater than 98% regioselectivity, thereby producing only one of the two possible lactam products during the subsequent hydrogenation. A heat-treatment process to select for desirable regioselective nitrilase or nitrile hydratase activities while destroying undesirable activities is also provided.

    Abstract translation: 已经开发了从脂肪族α，ω-二腈制备五元或六元环内酰胺的方法。 在该方法中，使用具有脂族腈水解酶（EC 3.5.5.7）活性的催化剂或腈水合酶（EC 4.2）的组合，首先将脂族α，ω-二腈转化为ω-二硝基甲酸的铵盐 .1.84）和酰胺酶（EC 3.5.1.4）活性。 然后通过在水溶液中氢化将ω-二硝基羧酸的铵盐直接转化成相应的内酰胺，而不分离中间体ω-二硝基甲酸或ω-氨基羧酸。 当脂肪族α，ω-二腈在α-碳原子处也不对称取代时，腈水解酶产生由ω-腈基水解产生的ω-亚硝基羧酸铵盐，其具有大于98％的区域选择性，从而仅产生 在随后氢化期间两种可能的内酰胺产物。 还提供了在破坏不期望的活性的同时选择期望的区域选择性腈水解酶或腈水合酶活性的热处理方法。

    Preparation of lactams from aliphatic .alpha., .omega.-dinitriles
    38.
    发明授权
    Preparation of lactams from aliphatic .alpha., .omega.-dinitriles 失效
    从脂肪族α，ω-二腈制备内酰胺

    公开(公告)号：US5908954A

    公开(公告)日：1999-06-01

    申请号：US108445

    申请日：1998-07-01

    Applicant: Robert Di Cosimo ,  Robert Donald Fallon ,  John Edward Gavagan ,  Frank Edward Herkes

    Inventor： Robert Di Cosimo ,  Robert Donald Fallon ,  John Edward Gavagan ,  Frank Edward Herkes

    IPC: C07C255/19 ,  C07C255/23 ,  C07D201/08 ,  C07D207/26 ,  C07D211/76 ,  C07D223/10 ,  C12N9/78 ,  C12N9/88 ,  C12P13/00 ,  C12P17/10 ,  C07C255/03 ,  C12P17/12

    CPC classification number: C07D211/76 ,  C07C255/19 ,  C07C255/23 ,  C07D201/08 ,  C07D207/26 ,  C07D223/10 ,  C12N9/78 ,  C12N9/88 ,  C12P13/002 ,  C12P13/02 ,  C12P17/10 ,  C12R1/01 ,  Y02P20/52

    Abstract: A process for the preparation of five-membered or six-membered ring lactams from aliphatic .alpha.,.omega.-dinitriles has been developed. In the process an aliphatic .alpha.,.omega.-dinitrile is first converted to an ammonium salt of an .omega.-nitrile-carboxylic acid in aqueous solution using a catalyst having an aliphatic nitrilase (EC 3.5.5.7) activity, or a combination of nitrile hydratase (EC 4.2.1.84) and arnidase (EC 3.5.1.4) activities. The ammonium salt of the .omega.-nitrilecarboxylic acid is then converted directly to the corresponding lactam by hydrogenation in aqueous solution, without isolation of the intermediate .omega.-nitrilecarboxylic acid or .omega.-aminocarboxylic acid. When the aliphatic .alpha.,.omega.-dinitrile is also unsymmetrically substituted at the .alpha.-carbon atom, the nitrilase produces the .omega.-nitrilecarboxylic acid ammonium salt resulting from hydrolysis of the .omega.-nitrile group with greater than 98% regioselectivity, thereby producing only one of the two possible lactam products during the subsequent hydrogenation. A heat-treatment process to select for desirable regioselective nitrilase or nitrile hydratase activities while destroying undesirable activities is also provided.

    Abstract translation: 已经开发了从脂肪族α，ω-二腈制备五元或六元环内酰胺的方法。 在该方法中，首先使用具有脂族腈水解酶（EC 3.5.5.7）活性的催化剂或腈水合酶的组合（在水溶液中将ω-腈 - 羧酸的铵盐转化为ω-腈 - 羧酸的铵盐， EC 4.2.1.84）和arnidase（EC 3.5.1.4）活动。 然后通过在水溶液中氢化将ω-二硝基羧酸的铵盐直接转化成相应的内酰胺，而不分离中间体ω-二硝基甲酸或ω-氨基羧酸。 当脂肪族α，ω-二腈在α-碳原子处也不对称取代时，腈水解酶产生由ω-腈基水解产生的ω-亚硝基羧酸铵盐，其具有大于98％的区域选择性，从而仅产生 在随后氢化期间两种可能的内酰胺产物。 还提供了在破坏不期望的活性的同时选择期望的区域选择性腈水解酶或腈水合酶活性的热处理方法。

    Preparation of caprolactam
    39.
    发明授权
    Preparation of caprolactam 失效
    己内酰胺的制备

    公开(公告)号：US5874575A

    公开(公告)日：1999-02-23

    申请号：US725438

    申请日：1996-10-03

    Applicant: Eberhard Fuchs ,  Guenther Achhammer

    Inventor： Eberhard Fuchs ,  Guenther Achhammer

    IPC: C07D201/08 ,  C07D223/10 ,  B01D3/00

    CPC classification number: C07D201/08 ,  Y02P20/52 ,  Y10S203/17 ,  Y10S203/90

    Abstract: An improved process for the preparation of caprolactam by heating 6-aminocapronitrile in the presence of a heterogenous catalyst and water under superatmospheric pressure without rapid deactivation of the catalysts used. The process further includes the addition of a low or high boiling alcohol in the heating phase, after which the products are obtained by distillation. The process further includes a method of working up the top and bottom products of the reactors to achieve higher yields.

    Abstract translation: 通过在异丙烯催化剂和水的存在下，在超大气压下加热6-氨基己腈而不快速失活所用催化剂制备己内酰胺的改进方法。 该方法还包括在加热阶段加入低沸点或高沸点醇，之后通过蒸馏获得产物。 该方法还包括处理反应器的顶部和底部产物以实现更高产率的方法。

    Simultaneous preparation of caprolactam and hexamethylenediamine
    40.
    发明授权
    Simultaneous preparation of caprolactam and hexamethylenediamine 失效
    同时制备己内酰胺和己二胺

    公开(公告)号：US5717090A

    公开(公告)日：1998-02-10

    申请号：US565214

    申请日：1995-11-30

    Applicant: Peter Bassler ,  Hermann Luyken ,  Gunther Achhammer ,  Tom Witzel ,  Eberhard Fuchs ,  Rolf Fischer ,  Werner Schnurr

    Inventor： Peter Bassler ,  Hermann Luyken ,  Gunther Achhammer ,  Tom Witzel ,  Eberhard Fuchs ,  Rolf Fischer ,  Werner Schnurr

    IPC: C07D201/08

    CPC classification number: C07D201/08

    Abstract: Caprolactam and hexamethylenediamine are prepared simultaneously starting from adiponitrile by a process in which (a) adiponitrile is partially hydrogenated to give a mixture containing essentially 6-aminocapronitrile, hexamethylenediamine, ammonia, adiponitrile and hexamethyleneimine, (b) the mixture obtained in (a) is subjected to a distillation to give ammonia as the top product and a bottom product I, (c) the bottom product I containing essentially 6-aminocapronitrile, hexamethylenediamine, adiponitrile, hexamethyleneimine, inert compound A and ammonia, the ammonia content being lower than that of the mixture used in stage (b), is subjected to a second distillation to give a mixture comprising the inert compound A and ammonia as the top product and a bottom product II, (d) the bottom product II is subjected, in a third column, to a distillation to give the inert compound A as the top product and a bottom product III, (e) the bottom product III is subjected, in a fourth column, to a distillation to give a top product KP1, containing essentially hexamethyleneimine and a bottom product IV, (f) the top product KP1 is subjected, in a fifth column, to a distillation to give a top product KP2, which contains essentially hexamethyleneimine, and (g) the bottom product IV containing essentially 6-aminocapronitrile and adiponitrile is subjected, in a sixth column, to a distillation to give 6-aminocapronitrile, and the 6-aminocapronitrile thus obtained is then cyclized to give caprolactam.

    Abstract translation: 己二醇和六亚甲基二胺由己二腈通过以下方法同时制备，其中（a）己二腈部分氢化得到基本上含有6-氨基己腈，六亚甲基二胺，氨，己二腈和六亚甲基亚胺的混合物，（b）将（a）中得到的混合物 进行蒸馏以产生氨作为顶部产物，底部产物I，（c）含有基本上为6-氨基己腈，六亚甲基二胺，己二腈，六亚甲基亚胺，惰性化合物A和氨的底部产物I，氨含量低于 将阶段（b）中使用的混合物进行第二次蒸馏，得到包含惰性化合物A和氨作为顶部产物的混合物和底部产物II，（d）底部产物II经受第三塔 进行蒸馏，得到惰性化合物A作为顶部产物和底部产物III，（e）底部产物III在第四列中经受 蒸馏得到基本上为六亚甲基亚胺和底部产物IV的顶部产物KP1，（f）顶部产物KP1在第五个塔中进行蒸馏，得到基本上含有六亚甲基亚胺的顶部产物KP2，和（g ）将含有基本上6-氨基己腈和己二腈的底部产物IV在第六塔中进行蒸馏以得到6-氨基己腈，然后将所得的6-氨基己腈环化，得到己内酰胺。

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