Method for preparing lactames, comprising a photonitrosation step, followed by a Beckmann transposition step
    3.
    发明授权
    Method for preparing lactames, comprising a photonitrosation step, followed by a Beckmann transposition step 有权
    制备内酰胺的方法,包括光子离子化步骤,接着是Beckmann转置步骤

    公开(公告)号:US09499481B2

    公开(公告)日:2016-11-22

    申请号:US14252610

    申请日:2014-04-14

    Applicant: ARKEMA FRANCE

    Inventor: Thierry Aubert

    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。

    Method for producing amide compound
    4.
    发明授权
    Method for producing amide compound 有权
    酰胺化合物的制备方法

    公开(公告)号:US09242931B2

    公开(公告)日:2016-01-26

    申请号:US14141867

    申请日:2013-12-27

    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.

    Abstract translation: 一种生产高纯度,优质酰胺化合物,特别是内酰胺的方法。 以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基于作为起始原料的酮被控制为0.4摩尔%以下的量。 通过氢化和/或结晶来纯化酮,肟和酰胺化合物中的一种或多种,​​以消除含有双键的杂质。 使用通过重结晶纯化的环烷酮控制具有环状桥结构的杂质含量。

    Method for producing amide compound
    5.
    发明授权
    Method for producing amide compound 有权
    酰胺化合物的制备方法

    公开(公告)号:US08530645B2

    公开(公告)日:2013-09-10

    申请号:US13254217

    申请日:2010-03-04

    CPC classification number: C07D225/02 C07D201/04

    Abstract: This invention relates to a process for producing an amide compound by Beckmann rearrangement of an oxime compound using a compound having at least two electron-withdrawing leaving groups as a rearrangement catalyst, the process comprising a pre-preparation step in which the rearrangement catalyst and at least a part of the oxime compound are mixed and reacted; and a rearrangement reaction step in which the oxime compound is rearranged at a temperature higher than that in the pre-preparation step.

    Abstract translation: 本发明涉及通过使用具有至少两个吸电子离去基团的化合物作为重排催化剂的肟化合物的贝克曼重排制备酰胺化合物的方法,该方法包括预制备步骤,其中重排催化剂和 将至少一部分肟化合物混合并反应; 和重排反应步骤,其中肟化合物在比预制备步骤中高的温度下重新排列。

    Method for preparing amide
    6.
    发明授权
    Method for preparing amide 有权
    酰胺的制备方法

    公开(公告)号:US08524895B2

    公开(公告)日:2013-09-03

    申请号:US12501699

    申请日:2009-07-13

    CPC classification number: C07D201/04 C07D223/10

    Abstract: The present invention provides a method for preparing amides, in which an amino acid ionic liquid is used as both a reaction medium and a catalyst to catalyze Beckman rearrangement of a ketoxime, so as to produce an amide. In the method, the rearrangement is conducted by catalyzing a ketoxime with an amino acid ionic liquid having the asymmetric property at a moderate reaction temperature during a short reaction time, so as to produce an amide without adding other catalysts such as concentrate sulfuric acid. The method has advantages such as avoiding corrosion in equipments with pipelines, the high conversion rate of ketoximes and the high selectivity of amides.

    Abstract translation: 本发明提供了一种制备酰胺的方法,其中使用氨基酸离子液体作为反应介质和催化贝克曼重排酮肟的催化剂,以产生酰胺。 在该方法中,通过在短的反应时间内在适度的反应温度下用具有不对称性质的氨基酸离子液体催化酮肟进行重排,从而在不加入其它催化剂如浓硫酸的情况下生成酰胺。 该方法具有避免管道设备腐蚀,酮肟转化率高,酰胺选择性高等优点。

    CATALYST COMPOSITION AND METHOD FOR PREPARING AMIDE USING THE SAME
    7.
    发明申请
    CATALYST COMPOSITION AND METHOD FOR PREPARING AMIDE USING THE SAME 有权
    催化剂组合物及其制备方法

    公开(公告)号:US20120184733A1

    公开(公告)日:2012-07-19

    申请号:US13332834

    申请日:2011-12-21

    Abstract: The present invention provides a method for preparing an amide. The method includes the steps of performing in a reactor including a catalyst composition having a nitrogen-containing heterocyclic compound and sulfuric acid Beckman rearrangement of a ketoxime to form a product stream having the amide, wherein a molar ratio of the nitrogen-containing heterocyclic compound to the sulfuric acid is from 1:1 to 1:8; and separating an organic phase having the amide and an aqueous phase having the catalyst composition from the product stream. The present invention facilitates the regeneration of the catalyst composition with low water content, so as to increase the conversion rate of a ketoxime and the selectivity of an amide.

    Abstract translation: 本发明提供一种制备酰胺的方法。 该方法包括以下步骤:在包括具有含氮杂环化合物的催化剂组合物和酮肟的硫酸贝克曼重排反应器的反应器中进行,以形成具有酰胺的产物流,其中含氮杂环化合物与 硫酸为1:1至1:8; 并从产物流中分离出具有酰胺的有机相和具有催化剂组成的水相。 本发明有助于低水含量的催化剂组合物的再生,从而提高酮肟的转化率和酰胺的选择性。

    Process for preparing caprolactam by Beckmann rearrangement
    8.
    发明授权
    Process for preparing caprolactam by Beckmann rearrangement 失效
    贝克曼重排制备己内酰胺的方法

    公开(公告)号:US07351820B2

    公开(公告)日:2008-04-01

    申请号:US10557771

    申请日:2004-05-17

    Abstract: The invention relates to a process for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime by feeding cyclohexanone oxime to a reaction mixture comprising (i) sulfuric acid (ii) SO3 and (iii) caprolactam , wherein the SO3 content of the reaction mixture is between 9 and 20 wt. % and the molar ratio M of the reaction mixture defined as (nso3+nH2SO4)/ncap is between 1 and 1.4, wherein nso3=quantity of SO3 in reaction mixture, in mol nso3=quantity of H2SO4 in reaction mixture, in mol ncap=quantity of caprolactam in reaction mixture, in mol.

    Abstract translation: 本发明涉及通过将环己酮肟进料到包含(i)硫酸(ⅱ)SO 3>和(ⅲ)己内酰胺的反应混合物中的贝克曼重排环己酮肟而制备己内酰胺的方法,其中SO 反应混合物的含量为9至20重量%。 %且反应混合物的摩尔比M定义为(n 3 SO 3 H + H 2 SO 4)/ n 在1和1.4之间,其中 在反应混合物中,SO 3 SO 3的量为H 2 SO 3的量,其中n 3 = 在反应混合物中,以摩尔数计,反应混合物中的己内酰胺的量为1摩尔%。

    Continuous process for preparing caprolactam
    9.
    发明授权
    Continuous process for preparing caprolactam 失效
    制备己内酰胺的连续工艺

    公开(公告)号:US07339056B2

    公开(公告)日:2008-03-04

    申请号:US10557753

    申请日:2004-05-17

    Abstract: The invention relates to a continuous process for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime, said process comprising a) feeding (i) oleum and (ii) cyclohexanone oxime into a first reaction mixture comprising caprolactam, sulfuric acid and SO3, b) feeding (iii) a portion of the first reaction mixture and (iv) cyclohexanone oxime into a second reaction mixture comprising caprolactam, sulfuric acid and SO3, c) withdrawing a portion of the second reaction mixture, wherein the process further comprises obtaining the cyclohexanone oxime that is fed to the reaction mixtures by: 1) preparing an organic medium comprising cyclohexanone oxime dissolved in an organic solvent 2) separating, by distillation, cyclohexanone oxime from said organic medium.

    Abstract translation: 本发明涉及通过Beckmann重排环己酮肟制备己内酰胺的连续方法,所述方法包括a)将(i)发烟硫酸和(ii)环己酮肟进料到包含己内酰胺,硫酸和SO 3的第一反应混合物中, b)将(iii)一部分第一反应混合物和(iv)环己酮肟进料到包含己内酰胺,硫酸和SO 3 N的第二反应混合物中,c)将一部分 第二反应混合物,其中所述方法还包括通过以下步骤获得进料到反应混合物中的环己酮肟:1)制备溶解在有机溶剂中的包含环己酮肟的有机介质2)通过蒸馏从所述有机介质中分离出环己酮肟 。

    Continuous process for preparing caprolactam
    10.
    发明申请
    Continuous process for preparing caprolactam 失效
    制备己内酰胺的连续工艺

    公开(公告)号:US20070055061A1

    公开(公告)日:2007-03-08

    申请号:US10557753

    申请日:2004-05-17

    Abstract: The invention relates to a continuous process for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime, said process comprising a) feeding (i) oleum and (ii) cyclohexanone oxime into a first reaction mixture comprising caprolactam, sulfuric acid and SO3, b) feeding (iii) a portion of the first reaction mixture and (iv) cyclohexanone oxime into a second reaction mixture comprising caprolactam, sulfuric acid and SO3, c) withdrawing a portion of the second reaction mixture, wherein the process further comprises obtaining the cyclohexanone oxime that is fed to the reaction mixtures by: 1) preparing an organic medium comprising cyclohexanone oxime dissolved in an organic solvent 2) separating, by distillation, cyclohexanone oxime from said organic medium.

    Abstract translation: 本发明涉及通过Beckmann重排环己酮肟制备己内酰胺的连续方法,所述方法包括a)将(i)发烟硫酸和(ii)环己酮肟进料到包含己内酰胺,硫酸和SO 3的第一反应混合物中, b)将(iii)一部分第一反应混合物和(iv)环己酮肟进料到包含己内酰胺,硫酸和SO 3 N的第二反应混合物中,c)将一部分 第二反应混合物,其中所述方法还包括通过以下步骤获得进料到反应混合物中的环己酮肟:1)制备溶解在有机溶剂中的包含环己酮肟的有机介质2)通过蒸馏从所述有机介质中分离出环己酮肟 。

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