公开(公告)号：US07893255B2

公开(公告)日：2011-02-22

申请号：US11472024

申请日：2006-06-21

Applicant: Eric Lacroix ,  Serge Hub ,  Wolfgang Holderich ,  Wilm Eickelberg ,  Francois Fajula ,  Francesco DiRenzo ,  Markus Brandhorst

Inventor： Eric Lacroix ,  Serge Hub ,  Wolfgang Holderich ,  Wilm Eickelberg ,  Francois Fajula ,  Francesco DiRenzo ,  Markus Brandhorst

IPC: C07D225/02 ,  B01J29/06

CPC classification number: C07D201/04

Abstract: The present invention relates to a process for the preparation of lauryllactam in which a Beckmann rearrangement of cyclododecanone oxime is carried out. Said process is carried out in the gas phase at a temperature of between 180 and 450° C. in the presence of a microporous material having a three-dimensional inorganic main structure composed of tetrahedra connected via a common edge, called zeolite.

Abstract translation: 本发明涉及一种制备十二烷基内酰胺的方法，其中进行了环十二烷酮肟的贝克曼重排。 所述方法在气相中，在具有三维无机主体结构的微孔材料的存在下，在180-450℃的温度下进行，所述三维无机主体结构由通过共同边缘连接的四面体称为沸石。

公开(公告)号：US20100324283A1

公开(公告)日：2010-12-23

申请号：US12526494

申请日：2008-02-08

Applicant: Kazuaki Ishihara ,  Junichi Kugimoto ,  Joji Kawai

Inventor： Kazuaki Ishihara ,  Junichi Kugimoto ,  Joji Kawai

IPC: C07D225/02

CPC classification number: C07D201/04 ,  C07D225/02 ,  Y02P20/582

Abstract: Disclosed is a method for producing laurolactam from cyclododecanone and hydroxylamine in a simple process and with high efficiency. The method comprises the following steps (a) to (e): (a) reacting cyclododecanone with hydroxylamine in an aqueous solution in the presence of an excess amount of cyclododecanone or a solvent to produce cyclododecanone oxime; (b) separating the reaction mixture obtained after the oxime-forming step into an oil and an aqueous phases and collecting a solution of cyclododecanone oxime of the oil phase as; (c) removing dissolved water from the solution of cyclododecanone oxime which is collected as an oily phase in the oil/aqueous phase separation step; (d) producing laurolactam from cyclododecanone oxime by rearrangement reaction using an aromatic-ring containing compound as a rearrangement catalyst; and (e) separating the produced laurolactam from the reaction mixture after the rearrangement step and purifying the laurolactam.

Abstract translation: 公开了一种以简单的工艺和高效率从环十二酮和羟胺制备月桂内酰胺的方法。 该方法包括以下步骤（a）至（e）：（a）在过量的环十二烷酮或溶剂存在下，使环十二酮与羟胺在水溶液中反应，生成环十二酮肟; （b）将在肟形成步骤后获得的反应混合物分离成油和水相，并收集油相的环十二酮肟溶液; （c）从在油/水相分离步骤中以油相收集的环十二酮肟溶液中除去溶解的水; （d）使用含芳环的化合物作为重排催化剂，通过重排反应从环十二酮肟生产月桂内酰胺; 和（e）在重排步骤之后将所生产的月桂内酰胺与反应混合物分离并纯化十二内酰胺。

公开(公告)号：US20090093628A1

公开(公告)日：2009-04-09

申请号：US12224660

申请日：2007-02-27

Applicant: Yasutaka Ishii ,  Tatsuya Nakano ,  Takahiro Iwahama

Inventor： Yasutaka Ishii ,  Tatsuya Nakano ,  Takahiro Iwahama

IPC: C07D403/04

CPC classification number: C07D201/04 ,  C07C231/10 ,  C07D223/10 ,  C07D225/02

Abstract: An amide or lactam is produced by conducting a rearrangement of a corresponding oxime compound in the presence of a cyclic compound containing a structure represented by following Formula (1) as a ring constituent and a fluorinated alcohol: wherein Z represents a halogen atom or an —OR group, where R represents an organic group.Z is preferably chlorine atom. Exemplary fluorinated alcohols include fluorine-containing branched-chain aliphatic alcohols represented by following Formula (3): wherein Rf1 and Rf2 may be the same as or different from each other and each represent a perfluoroalkyl group having one to eight carbon atoms; and “n” denotes an integer of 0 to 8.According to this process, amides or lactams can be simply produced in high yields without causing large amounts of by-products.

Abstract translation: 酰胺或内酰胺通过在含有下式（1）表示的结构的环状化合物作为环成分和氟化醇的存在下进行相应的肟化合物的重排而制备：其中Z表示卤素原子或 - OR基，其中R表示有机基团。 Z优选为氯原子。 示例性的氟化醇包括由下式（3）表示的含氟支链脂族醇：其中Rf1和Rf2可以相同或不同，并且各自表示具有1-8个碳原子的全氟烷基; “n”表示0〜8的整数。根据该方法，可以高产率地简单地制造酰胺或内酰胺而不会产生大量的副产物。

公开(公告)号：US07238803B2

公开(公告)日：2007-07-03

申请号：US10883822

申请日：2004-07-06

Applicant: Masashi Yokota ,  Yoshinori Kobayashi ,  Masaru Kitamura

Inventor： Masashi Yokota ,  Yoshinori Kobayashi ,  Masaru Kitamura

IPC: C07D201/04

CPC classification number: C07D201/04 ,  Y02P20/52

Abstract: ε-Caprolactam is produced by the method comprising the step of introducing a gas comprising cyclohexanone oxime into a layer of solid catalyst particles through a plurality of holes of a gas diffusion plate so that the solid catalyst particles are brought into contact with the gas, while fluidizing the catalyst layer, wherein the holes have an average diameter of about 3 mm or smaller. In accordance with the production method, ε-caprolactam can be produced from a raw material gas comprising cyclohexanone oxime with a high conversion of cyclohexanone oxime and a high selectivity to ε-caprolactam.

Abstract translation: ε-己内酰胺通过包括以下步骤的方法制备：包括环己酮肟的气体通过气体扩散板的多个孔引入固体催化剂颗粒层中，使得固体催化剂颗粒与气体接触，同时 使催化剂层流化，其中孔的平均直径为约3mm或更小。 根据制造方法，ε-己内酰胺可以由包含环己酮肟的高转化率和对ε-己内酰胺的高选择性的环己酮肟的原料气体制备。

公开(公告)号：US20070149778A1

公开(公告)日：2007-06-28

申请号：US11614726

申请日：2006-12-21

Applicant: Stacey Zones ,  Allen Burton

Inventor： Stacey Zones ,  Allen Burton

IPC: C07D201/04

CPC classification number: C07D201/04 ,  B01J29/035 ,  B01J29/70

Abstract: The present invention relates to new crystalline molecular sieve SSZ-74 prepared using a hexamethylene-1,6-bis-(N-methyl-N-pyrrolidinium) dication as a structure-directing agent, and its use in catalysts for Beckmann rearrangement.

Abstract translation: 本发明涉及使用六亚甲基-1,6-双 - （N-甲基-N-吡咯烷鎓）双键作为结构导向剂制备的新型结晶分子筛SSZ-74及其用于贝克曼重排用催化剂。

公开(公告)号：US07060645B2

公开(公告)日：2006-06-13

申请号：US11165538

申请日：2005-06-24

Applicant: Masahiro Hoshino ,  Masaru Kitamura ,  Keisuke Sugita

Inventor： Masahiro Hoshino ,  Masaru Kitamura ,  Keisuke Sugita

IPC: B01J29/40 ,  C07D201/04

CPC classification number: C07D201/04 ,  B01J29/035 ,  B01J37/06 ,  B01J2229/38 ,  B01J2229/40 ,  C01B37/02

Abstract: The present invention provides a method for manufacturing a zeolite comprising following steps of: (1): calcining crystals obtained by hydrothermal synthesis reaction of a silicon compound; (2): contact treating a calcined product obtained by the step (1) with an aqueous solution including an amine and/or a quaternary ammonium compound; (3): calcining a treated product obtained by the step (2); and (4): contact treating the calcined product obtained by the step (3) with an aqueous solution including ammonia and/or an ammonium salt. According to the present invention, a method is also provided wherein ε-caprolactam is manufactured by Beckmann rearrangement reaction of cyclohexanone oxime in a gaseous phase in the presence of the zeolite manufactured by the above-described method.

Abstract translation: 本发明提供一种制造沸石的方法，包括以下步骤：（1）：煅烧通过硅化合物的水热合成反应获得的晶体; （2）：用包含胺和/或季铵化合物的水溶液接触步骤（1）得到的煅烧产物; （3）：煅烧通过工序（2）得到的处理物; 和（4）：用包含氨和/或铵盐的水溶液接触处理由步骤（3）获得的煅烧产物。 根据本发明，还提供了一种方法，其中ε-己内酰胺通过在通过上述方法制造的沸石存在下，在气相中通过环己酮肟的贝克曼重排反应制造。

公开(公告)号：US07026474B2

公开(公告)日：2006-04-11

申请号：US11055101

申请日：2005-02-11

Applicant: Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

Inventor： Keisuke Sugita ,  Masaru Kitamura ,  Masahiro Hoshino

IPC: C07D201/04

CPC classification number: B01J38/08 ,  B01J29/90 ,  B01J38/12 ,  B01J38/66 ,  C07D201/04 ,  Y02P20/52 ,  Y02P20/584

Abstract: A method for producing ε-caprolactam and a method for reactivating a zeolite catalyst for the production are provided. In the reactivation step, a zeolite catalyst is allowed to contact a gas containing a carboxylic acid, water and a compound selected from ammonia and amines. In accordance with the present invention, the catalytic activities of a zeolite catalyst used for the Beckmann rearrangement reaction of cyclohexanone oxime can be effectively restored. Consequently, ε-caprolactam may be produced with a high production yield for a long period of time by reusing the catalyst by the method described above.

Abstract translation: 提供了制备ε-己内酰胺的方法和用于再生催化剂的方法。 在再活化步骤中，使沸石催化剂与含有羧酸，水和选自氨和胺的化合物的气体接触。 根据本发明，可以有效地恢复用于环己酮肟的贝克曼重排反应的沸石催化剂的催化活性。 因此，通过上述方法重新使用催化剂，可以长期生产ε-己内酰胺。

公开(公告)号：US20040059108A1

公开(公告)日：2004-03-25

申请号：US10251335

申请日：2002-09-21

Inventor： Alan Levy ,  Gregory Cleotelis II ,  James Sawyer ,  Nolan Henrich III ,  Mohammed Loya ,  Matthew Warren ,  Gregory Moore

IPC: C07D201/04 ,  C07C231/00

CPC classification number: C07D201/04

Abstract: Methods are disclosed of producing and purifying at least one amide. In accordance with one of the methods disclosed herein, the at least one amide is produced by providing an organic liquid comprising at least one oxime, providing at least one catalyst, adding the at least one catalyst to the organic liquid to form a rearrangement mass, wherein the rearrangement mass comprises at least one amide, at least one impurity, and the at least one catalyst, and heating the rearrangement mass to a temperature of at least about 115null C. for a period of time in order to sulfonate, break down and/or reduce the concentration of some of the at least one impurity in the rearrangement mass.

Abstract translation: 公开了生产和纯化至少一种酰胺的方法。 根据本文公开的方法之一，通过提供包含至少一种肟的有机液体来提供至少一种酰胺，提供至少一种催化剂，将至少一种催化剂加入到有机液体中以形成重排质量， 其中所述重排质量包含至少一种酰胺，至少一种杂质和所述至少一种催化剂，并且将所述重排质量加热至至少约115℃的温度一段时间以便磺化，分解 和/或降低重排质量中的一些至少一种杂质的浓度。

公开(公告)号：US20020040137A1

公开(公告)日：2002-04-04

申请号：US09964424

申请日：2001-09-28

Inventor： Wolfgang F. Holderich ,  Gerd Dahlhoff ,  Andre Sbresny ,  Hiroshi Ichihashi

IPC: C07D223/10

CPC classification number: C07D201/06 ,  C07D201/04

Abstract: A process is provided for producing null-caprolactam from cyclohexanone oxime. The process comprises a evaporation step of a mixture of cyclohexanone oxime and a solvent by introducing the mixture into a fluidized bed in which inert particles is fluidized by an inert gas, the particles having heat enough to evaporate the mixture; and a rearrangement step of cyclohexanone oxime in the evaporated mixture into null-caprolactam by a gas phase Beckmann rearrangement reaction using a solid catalyst, excluding a catalyst consisting of a boric acid or a boron oxide.

公开(公告)号：US06245907B1

公开(公告)日：2001-06-12

申请号：US09205900

申请日：1998-12-04

Applicant: Myung Suk Suh ,  Seung Eon Park ,  Chang Hwang Lee ,  Myeong Hong Lee ,  Si Geun Lee ,  Jung Ho Kim

Inventor： Myung Suk Suh ,  Seung Eon Park ,  Chang Hwang Lee ,  Myeong Hong Lee ,  Si Geun Lee ,  Jung Ho Kim

IPC: C07D20104

CPC classification number: C07D201/04 ,  C07D223/10

Abstract: Disclosed is a process for producing a high purity caprolactam which comprises converting cyclohexene obtained by the partial hydrogenation of benzene into cyclohexanol through hydration, converting the cyclohexanol into cyclohexanone through dehydrogenation, converting the cyclohexanone into cyclohexanone oxime through oximation and converting the cyclohexanone oxime into caprolactam through the Beckman rearrangement, characterized by comprising isolating and purifying the methylcyclopentanol from the cyclohexanol prior to use of such cyclohexanol in dehydrogenation and feeding the isolated methylcyclopentanol directly to oximation in order that the methylcyclopentanol is not fed to dehydrogenation. The process of the invention advantageously provides an economic method for producing a caprolactam with greater purity.

Abstract translation: 公开了一种生产高纯度己内酰胺的方法，其包括将通过水合将苯部分氢化得到的环己烯转化为环己醇，通过脱氢将环己醇转化为环己酮，通过肟化将环己酮转化为环己酮肟，并将环己酮肟转化为己内酰胺， 贝克曼重排，其特征在于包括在脱氢中使用这种环己醇之前从环己醇中分离和纯化甲基环戊醇，并将分离的甲基环戊醇直接进料到肟化中，以使甲基环戊醇不进行脱氢。 本发明的方法有利地提供了一种制备更高纯度的己内酰胺的经济方法。