公开(公告)号：US09662643B2

公开(公告)日：2017-05-30

申请号：US14263156

申请日：2014-04-28

Applicant: AdvanSix Resins & Chemicals LLC ,  University of Southampton

Inventor： Alan B. Levy ,  Robert Raja ,  Matthew E. Potter

IPC: C01B39/54 ,  B01J29/85 ,  C07D201/04 ,  B01J35/00 ,  C07D223/10 ,  C07D225/02 ,  C01B37/08

CPC classification number: B01J29/85 ,  B01J35/002 ,  C01B37/08 ,  C01B39/54 ,  C07D201/04 ,  C07D223/10 ,  C07D225/02 ,  Y02P20/52

Abstract: Methods for producing lactams from oximes by performing a Beckmann rearrangement using a silicoaluminophosphate catalyst are provided. These catalysts may be used in gas phase or liquid phase reactions to convert oximes into lactams. High conversion of oxime and high selectivity for the desired lactams are produced using the disclosed methods, including high conversion and selectivity for ε-caprolactam produced from cyclohexanone oxime and high conversion and selectivity for ω-laurolactam produced from cyclododecanone oxime.

公开(公告)号：US09533944B2

公开(公告)日：2017-01-03

申请号：US14655514

申请日：2013-12-12

Applicant: Sumitomo Chemical Company

Inventor： Masahiro Hoshino ,  Yuta Kikuchi ,  Sho Tsujiuchi

IPC: C07C249/04 ,  C07D201/04

CPC classification number: C07C249/04 ,  C07C2601/14 ,  C07D201/04 ,  C07C251/44

Abstract: Provided is a method for producing an oxime compound with satisfactory selectivity. Provide is a method for producing an oxime represented by the following formula (II): wherein R1 and R2 are respectively the same as defined below, the method including oxidizing an amine represented by the following formula (I): wherein R1 and R2 each independently represents a hydrogen atom, an optionally substituted hydrocarbon group, or an optionally substituted heterocyclic group (provided that R1 and R2 are not simultaneously hydrogen atoms), or R1 and R2, together with the carbon atom to which R1 and R2 are attached, form an optionally substituted alicyclic hydrocarbon group having 3 to 12 carbon atoms [hereinafter sometimes referred to as the amine compound (I)], with oxygen in the presence of a layered silicate.

Abstract translation: 提供一种具有令人满意的选择性的肟化合物的制造方法。 提供一种由下述式（II）表示的肟的制造方法，其中R 1和R 2分别与下述定义相同，该方法包括使由下式（I）表示的胺氧化：其中R 1和 R 2各自独立地表示氢原子，任选取代的烃基或任选取代的杂环基（条件是R 1和R 2不同时为氢原子）或R 1和R 2与碳原子一起 在层状硅酸盐存在下，与氧一起形成任选取代的碳原子数为3〜12的脂环族烃基（以下有时称为胺化合物（I））。

公开(公告)号：US09533932B2

公开(公告)日：2017-01-03

申请号：US14814984

申请日：2015-07-31

Applicant: Kevin Micoine ,  Ralf Meier ,  Juergen Herwig ,  Martin Roos ,  Harald Haeger ,  Luca Cameretti ,  Jens Doering

Inventor： Kevin Micoine ,  Ralf Meier ,  Juergen Herwig ,  Martin Roos ,  Harald Haeger ,  Luca Cameretti ,  Jens Doering

IPC: C07C45/58 ,  C07C45/51 ,  C07D201/04 ,  B01J23/44 ,  C07C45/82 ,  C07C249/04 ,  C07D225/02 ,  C07D301/12 ,  C08G69/16 ,  C07C29/52 ,  C07C45/00 ,  C07C45/28 ,  B01J23/38 ,  C07D201/06

CPC classification number: C07C45/512 ,  B01J23/38 ,  B01J23/44 ,  C07C29/52 ,  C07C45/002 ,  C07C45/28 ,  C07C45/58 ,  C07C45/82 ,  C07C249/04 ,  C07C2601/14 ,  C07D201/04 ,  C07D201/06 ,  C07D225/02 ,  C07D301/12 ,  C08G69/16 ,  C07C49/413 ,  C07C35/205

Abstract: Cyclododecanone (CDON) is prepared by epoxidizing cyclododecene (CDEN) to epoxycyclododecane (CDAN epoxide), and rearranging the CDAN epoxide to CDON to obtain a mixture comprising said CDON and cyclododecane (CDAN), wherein CDAN is separated from the CDON-containing mixture and oxidized to CDON.

Abstract translation: 通过环环十二碳烯（CDEN）环氧环十二烷（CDAN环氧化物）制备环十二烷酮（CDON），并将CDAN环氧化物重排为CDON，得到包含所述CDON和环十二烷（CDAN）的混合物，其中CDAN与含CDON的混合物分离， 氧化成CDON。

公开(公告)号：US20160159657A1

公开(公告)日：2016-06-09

申请号：US14899579

申请日：2014-06-20

Applicant: CAP III B.V.

Inventor： Johan Thomas Tinge ,  Geert Ekkelenkamp ,  Robert Geertman

IPC: C01C1/24 ,  B01D9/00

CPC classification number: C01C1/24 ,  B01D9/0022 ,  B01D9/0031 ,  B01D9/004 ,  B01D9/0063 ,  B01D2009/0086 ,  C01C1/248 ,  C07C249/08 ,  C07C2601/14 ,  C07D201/04 ,  C07D201/16 ,  C07C251/44

Abstract: The present invention provides a continuous process for producing ammonium sulfate crystals, wherein said process comprises: (a) feeding to a first group of crystallization sections, which crystallization sections are heat integrated in series, a first aqueous ammonium sulfate solution that contains one or more impurities; (b) feeding to a second group of crystallization sections, which crystallization sections are heat integrated in series, a second aqueous ammonium sulfate solution that contains one or more impurities; (c) crystallizing ammonium sulfate crystals in each crystallization section respectively from each of said solutions of ammonium sulfate that contain one or more impurities; (d) purging a fraction of the ammonium sulfate solution that contains one or more impurities from each of said crystallization sections; and (e) discharging ammonium sulfate crystals from each crystallization section, characterized in that: (i) both the first group of crystallization sections and the second group of crystallization sections are together heat integrated in one series of crystallization sections; wherein the first group of crystallization sections operates at higher temperature than the second group of crystallization sections; and (ii) the composition of the first aqueous ammonium sulfate solution that contains one or more impurities is different to the composition of the second aqueous ammonium sulfate solution that contains one or more impurities. Further provided is apparatus suitable for producing ammonium sulfate crystals.

Abstract translation: 本发明提供了一种用于生产硫酸铵晶体的连续方法，其中所述方法包括：（a）将第一组结晶部分进料到该第一组结晶部分，该结晶部分是串联的热积分法，第一组硫酸铵水溶液含有一种或多种 杂质; （b）将第二组结晶部分进料到该第二组结晶部分，该结晶部分串联加热一体化，含有一种或多种杂质的第二硫酸铵溶液; （c）分别从含有一种或多种杂质的所述硫酸铵溶液中分别在每个结晶段中结晶硫酸铵晶体; （d）从每个所述结晶部分清洗含有一种或多种杂质的硫酸铵溶液的一部分; 和（e）从每个结晶部分排出硫酸铵晶体，其特征在于：（i）第一组结晶部分和第二组结晶部分一起热集成在一系列结晶部分中; 其中所述第一组结晶段在比所述第二组结晶段更高的温度下操作; 和（ii）含有一种或多种杂质的第一硫酸铵水溶液的组成与含有一种或多种杂质的第二硫酸铵水溶液的组成不同。 还提供了适用于生产硫酸铵晶体的装置。

公开(公告)号：US20140246303A1

公开(公告)日：2014-09-04

申请号：US14252610

申请日：2014-04-14

Applicant: ARKEMA FRANCE

Inventor： Thierry AUBERT

IPC: C07D201/04

CPC classification number: C07D201/04 ,  C07C249/06 ,  C07C2601/20 ,  C07D227/087 ,  C07C251/44

Abstract: The invention relates to a method for preparing lactames, according to which a photonitrosation of a cycloalkane is carried out using nitrosyl chloride (NOCI). According to the invention, said photonitrosation is carried out by means of LEDs emitting a monochromatic light. The method according to the invention can also include a step comprising Beckmann transposition/dechlorination of the oxime hydrochloride generated during said phonitrosation, preferably carried out in a glass microreactor.

Abstract translation: 本发明涉及一种制备内酰胺的方法，根据该方法，使用亚硝酰氯（NOCI）进行环烷烃的光子离子化。 根据本发明，所述光子离子化是通过发射单色光的LED进行的。 根据本发明的方法还可以包括一个步骤，该步骤包括贝克曼转移/脱氯在所述发声过程中产生的肟盐酸盐，优选在玻璃微反应器中进行。

公开(公告)号：US20140114061A1

公开(公告)日：2014-04-24

申请号：US14141867

申请日：2013-12-27

Applicant: Ube Industries, Ltd.

Inventor： Junichi Kugimoto ,  Joji Kawai ,  Kazuo Yamato ,  Masahide Okada ,  Tsunemi Sugimoto ,  Hiroshi Matsumoto

IPC: C07D201/04 ,  C07D225/02

CPC classification number: C07D201/06 ,  C07D201/04 ,  C07D225/02

Abstract: A method for producing a high purity, high quality amide compound, particularly a lactam. An amount of each of a halide, an aldehyde compound, an alcohol compound and a nitrile compound contained in a solution recycled into an oxime-forming step is controlled to an amount of 0.4 mol % or less based on the ketone as a starting material. One or more of a ketone, an oxime and an amide compound are purified by hydrogenation and/or crystallization for eliminating impurities containing a double bond. A content of impurities having a cyclic bridge structure is controlled using a cycloalkanone purified by recrystallization.

公开(公告)号：US08552180B2

公开(公告)日：2013-10-08

申请号：US12637190

申请日：2009-12-14

Applicant: Cheng-Fa Hsieh ,  Chien-Chuan Shih ,  Chi-Yuan Chen

Inventor： Cheng-Fa Hsieh ,  Chien-Chuan Shih ,  Chi-Yuan Chen

IPC: C07D201/04

CPC classification number: C07C231/10 ,  B01J31/0279 ,  B01J31/40 ,  C07B63/00 ,  C07C231/24 ,  C07D201/04 ,  C07D201/16 ,  C07D223/10 ,  Y02P20/542 ,  Y02P20/584 ,  C07C233/05 ,  C07C233/07 ,  C07C233/65

Abstract: The present invention provides a method for separating an amide from an amino acid ionic liquid. The method includes the step of providing a polar solvent and an extracting agent to the amino acid ionic liquid, so as to separate the amide from the amino acid ionic liquid. In the method of the present invention, there is no need to add ammonium for neutralization, such that no byproduct, ammonium sulfate, is formed. In addition, after the amide is separated from the amino acid ionic liquid, the amino acid ionic liquid can be recycled.

Abstract translation: 本发明提供了从氨基酸离子液体中分离酰胺的方法。 该方法包括向氨基酸离子液体提供极性溶剂和萃取剂以将酰胺与氨基酸离子液体分离的步骤。 在本发明的方法中，不需要添加用于中和的铵，使得不形成副产物硫酸铵。 此外，在酰胺与氨基酸离子液体分离后，氨基酸离子液体可以循环使用。

公开(公告)号：US20130005960A1

公开(公告)日：2013-01-03

申请号：US13635092

申请日：2011-03-15

Applicant: Junichi Kugimoto ,  Joji Kawai ,  Kazuo Yamato ,  Masahide Okada ,  Tsunemi Sugimoto ,  Hiroshi Matsumoto

Inventor： Junichi Kugimoto ,  Joji Kawai ,  Kazuo Yamato ,  Masahide Okada ,  Tsunemi Sugimoto ,  Hiroshi Matsumoto

IPC: C07D225/02

CPC classification number: C07D201/06 ,  C07D201/04 ,  C07D225/02

Abstract: The present invention relates to a method for producing a high purity, high quality amide compound, particularly, lactam. A first embodiment of the present invention is characterized in that an amount of each of a halide, an aldehyde compound, an alcohol compound and a nitrile compound contained in a solution recycled into an oxime-forming step is controlled to an amount of 0.4 mol % or less based on the ketone as a starting material. A second embodiment of the present invention is characterized in that one or more compounds selected from the group consisting of a ketone, an oxime and an amide compound are purified by hydrogenation and/or crystallization for eliminating impurities containing a double bond. A third embodiment of the present invention is characterized in that a content of impurities having a cyclic bridge structure is controlled by using a cycloalkanone purified by recrystallization.

Abstract translation: 本发明涉及一种生产高纯度，优质酰胺化合物，特别是内酰胺的方法。 本发明的第一实施方案的特征在于，将再循环到肟形成步骤的溶液中所含的卤化物，醛化合物，醇化合物和腈化合物中的每一种的量控制为0.4mol％ 基于酮作为原料。 本发明的第二个实施方案的特征在于，通过氢化和/或结晶纯化一种或多种选自酮，肟和酰胺化合物的化合物，以消除含有双键的杂质。 本发明的第三实施方案的特征在于通过使用通过重结晶纯化的环烷酮来控制具有环状桥结构的杂质的含量。

公开(公告)号：US20110137027A1

公开(公告)日：2011-06-09

申请号：US12993975

申请日：2009-05-14

Applicant: Thierry Aubert

Inventor： Thierry Aubert

IPC: C07D225/02 ,  C07C201/06

CPC classification number: C07D201/04 ,  C07C249/06 ,  C07C2601/20 ,  C07D227/087 ,  C07C251/44

Abstract: The invention relates to a method for preparing lactames, according to which a photonitrosation of a cycloallcane is carried out using nitrosyl chloride (NOCI). According to the invention, said photonitrosation is carried out by means of LEDs emitting a monochromatic light. The method according to the invention can also include a step comprising Beckmann transposition/dechlorination of the oxime hydrochloride generated during said phonitrosation, preferably carried out in a glass microreactor.

Abstract translation: 本发明涉及一种制备内酰胺的方法，根据该方法，使用亚硝酰氯（NOCI）进行环烷烃的光子离子化。 根据本发明，所述光子离子化是通过发射单色光的LED进行的。 根据本发明的方法还可以包括一个步骤，该步骤包括贝克曼转移/脱氯在所述发声过程中产生的肟盐酸盐，优选在玻璃微反应器中进行。

公开(公告)号：US07687621B2

公开(公告)日：2010-03-30

申请号：US11822141

申请日：2007-07-02

Applicant: Keisuke Sugita ,  Masaru Kitamura

Inventor： Keisuke Sugita ,  Masaru Kitamura

IPC: C07D201/04

CPC classification number: B01J29/90 ,  B01J38/66 ,  B01J2229/32 ,  C07D201/04 ,  Y02P20/52 ,  Y02P20/584

Abstract: The present invention provides a process for regenerating a catalyst for producing e-caprolactam comprising the steps of adsorbing a silicon compound on a zeolite catalyst that had been used for a Beckmann rearrangement reaction of cyclohexanone oxime and contacting the catalyst with an aqueous solution containing a compound selected from a quaternary ammonium compound, lower alkylamines and ammonia. The present invention also provides a process for producing e-caprolactam comprising subjecting cyclohexanone oxime to the Beckmann rearrangement reaction in the presence of the catalyst thus regenerated.

Abstract translation: 本发明提供了一种用于再生生产ε-己内酰胺的催化剂的方法，包括以下步骤：将硅化合物吸附在已经用于环己酮肟的贝克曼重排反应的沸石催化剂上，并使催化剂与含有化合物的水溶液接触 选自季铵化合物，低级烷基胺和氨。 本发明还提供一种生产ε-己内酰胺的方法，其包括在由此再生的催化剂存在下使环己酮肟进行贝克曼重排反应。