公开(公告)号：US20140171638A1

公开(公告)日：2014-06-19

申请号：US14132082

申请日：2013-12-18

Applicant: BASF SE

Inventor： Rolf-Hartmuth Fischer

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A process is described for preparing purified caprolactam, comprising the steps a) extraction of crude caprolactam, obtained from the Beckmann rearrangement of cyclohexanone oxime, with an organic extractant, b) removal of the organic phase from step a), c) distillative separation of the organic extractant from the organic phase from step b) giving rise to water-containing lactam extract, being preceded by addition of the distillative separation, aqueous alkali metal hydroxide solution in an amount of from 0 to 10 mmol/kg of caprolactam, d) addition of 0 to 30 mmol of alkali metal hydroxide/kg of caprolactam to the water-containing lactam extract from step c), e) distillative removal of water from the water-containing lactam extract treated with alkali metal hydroxide from step d), f) freeing the caprolactam from step e) from by-products lower- and higher-boiling than caprolactam by distillation, with addition in steps c) and d) together of at least 1.5 mmol of alkali metal hydroxide/kg of caprolactam.

Abstract translation: 描述了制备纯化的己内酰胺的方法，其包括以下步骤：a）从有机萃取剂中提取由Beckmann重排环己酮肟得到的粗己内酰胺，b）从步骤a）中除去有机相，c）蒸馏分离 来自步骤b）的来自有机相的有机萃取剂产生含水内酰胺提取物，之前加入蒸馏分离，碱金属氢氧化物水溶液的量为0至10mmol / kg己内酰胺，d） 向来自步骤c）的含水内酰胺提取物中加入0至30mmol碱金属氢氧化物/ kg己内酰胺，e）从碱金属氢氧化物处理的含水内酰胺提取物中蒸馏除去水，步骤d），f ）通过蒸馏将己内酰胺从步骤e）中脱除副产物比己内酰胺更低沸点和更高沸点，在步骤c）和d）中加入至少1.5mmol碱金属氢氧化物/ k g己内酰胺。

公开(公告)号：US08268990B2

公开(公告)日：2012-09-18

申请号：US12274915

申请日：2008-11-20

Applicant: Nicholas J. Bennett ,  Thomas McInally ,  Stephen Thom

Inventor： Nicholas J. Bennett ,  Thomas McInally ,  Stephen Thom

IPC: C07D201/16

CPC classification number: C07D239/48 ,  C07D239/49 ,  C07D401/10 ,  C07D401/12 ,  C07D403/10 ,  C07D403/12 ,  C07D417/12

Abstract: The present invention provides compounds of formula (I) wherein R1, R2, R3 and R4 are as defined in the specification, and pharmaceutically acceptable salts thereof, as well as processes for their preparation, pharmaceutical compositions containing them and their use in therapy.

Abstract translation: 本发明提供式（I）化合物，其中R 1，R 2，R 3和R 4如说明书中所定义，及其药学上可接受的盐，以及其制备方法，含有它们的药物组合物及其在治疗中的用途。

公开(公告)号：US08231765B2

公开(公告)日：2012-07-31

申请号：US12155065

申请日：2008-05-29

Applicant: Daniel Amoros ,  Philippe Leconte ,  Pierre Coqueret

Inventor： Daniel Amoros ,  Philippe Leconte ,  Pierre Coqueret

IPC: B01D3/34 ,  C07D201/02 ,  C07D201/16

CPC classification number: C07D201/16 ,  C07D201/08 ,  Y10S203/90

Abstract: A method and a plant are disclosed for purifying lactams, particularly lactams obtained by cyclizing hydrolysis of aminonitrile. The purification of ε-caprolactam obtained by cyclizing hydrolysis of aminocapronitrile is described which includes eliminating the ammonia from the reaction medium of the hydrolysis, then recovering the lactam from the medium in purified form. The recovery is carried out by performing at least a distillation of the lactam in the presence of a base producing optionally a fronts fraction having compounds more volatile than the lactam, a fraction having the lactam to be recovered to the degree of desired purity and a distillation tails having the lactam and compounds less volatile than the lactam. The distillation tails are treated by various processes such as evaporation in thin layers to recover the major part of the caprolactam and recycling the latter in the purification process.

Abstract translation: 公开了一种用于纯化内酰胺，特别是通过环化氨基腈水解获得的内酰胺的方法和设备。 描述了通过环化氨基腈的水解获得的ε-己内酰胺的纯化，其包括从水解反应介质中除去氨，然后以纯化形式从培养基中回收内酰胺。 回收是通过在碱的存在下进行至少一种蒸馏来进行的，所述碱生产任选地具有比内酰胺更易挥发的化合物的前端部分，具有待回收的内酰胺至具有所需纯度的馏分和蒸馏 尾巴具有内酰胺和化合物比内酰胺更不易挥发。 蒸馏尾部通过各种方法处理，例如在薄层中蒸发以回收大部分己内酰胺并在纯化过程中回收己内酰胺。

公开(公告)号：US08193348B2

公开(公告)日：2012-06-05

申请号：US12474968

申请日：2009-05-29

Applicant: Chien-Hsien Li

Inventor： Chien-Hsien Li

IPC: C07D201/16

CPC classification number: C07D201/16 ,  C07D201/12

Abstract: A system and a method for recovering caprolactam from a rearrangement mixture are provided. The system includes a neutralization unit; a buffering unit for receiving a crude lactam solution containing impurities content below a standard value and being fed from the neutralization unit; a temporary storage unit for receiving a crude lactam solution containing impurities above the standard value and being fed from the neutralization unit; a temporary extraction unit for performing batch extraction to separate out a first lactam solution; an extraction unit for performing continuous extraction to separate out a second lactam solution; and a recovery unit for allowing caprolactam to be recovered. In the present system and method, the crude lactam solution is selectively fed into the extraction unit for continuous extraction or to the temporary extraction unit for batch extraction, thereby maintaining continuity of operation, enhancing separation efficiency, and reducing both material consumption and purification loadings.

Abstract translation: 提供了从重排混合物中回收己内酰胺的体系和方法。 该系统包括中和单元; 缓冲单元，用于接收含有低于标准值的杂质含量的粗内酰胺溶液并从中和单元进料; 临时存储单元，用于接收含有高于标准值的杂质的粗内酰胺溶液并从中和单元进料; 临时提取单元，用于进行分批提取以分离出第一内酰胺溶液; 提取单元，用于进行连续提取以分离第二内酰胺溶液; 和用于使己内酰胺回收的回收单元。 在本系统和方法中，将粗内酰胺溶液选择性地进料到用于连续萃取的提取单元中或者用于批量提取的临时提取单元，从而保持操作的连续性，提高分离效率，并减少材料消耗和净化负荷。

公开(公告)号：US07365195B2

公开(公告)日：2008-04-29

申请号：US10565774

申请日：2004-07-16

Applicant: Joannes Albertus Wilhelmus J. A. W. Lemmens ,  Theodorus Maria T. M. Smeets ,  Paul Maria P. M. Brandts ,  Koen Harry Maria K. H. M. Ceyssens

Inventor： Joannes Albertus Wilhelmus J. A. W. Lemmens ,  Theodorus Maria T. M. Smeets ,  Paul Maria P. M. Brandts ,  Koen Harry Maria K. H. M. Ceyssens

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: The invention relates to a process for purifying caprolactam, said process comprising (a) subjecting the caprolactam to a hydrogenation by treating the caprolactam with hydrogen in the presence of a heterogeneous nickel containing hydrogenation catalyst, (b) distilling at least a portion of the hydrogenated caprolactam in a distillation column containing nickel in an amount sufficiently low such that ΔPANNi≦3, wherein ΔPANNi=ΔPAN−ΔPANNi=0, ΔPAN=increase of the PAN number of caprolactam during distilling, ΔPANNi=0 increase of the PAN number of caprolactam during distilling under the same conditions in a distillation column free of nickel. Nickel is removed from the caprolactam solution prior to the distillation step.

Abstract translation: 本发明涉及一种纯化己内酰胺的方法，所述方法包括（a）在非均相含镍氢化催化剂存在下，用氢处理己内酰胺进行氢化，（b）蒸馏至少一部分氢化 己内酰胺在含有足够低的量的镍的蒸馏塔中，使得ΔPANN 3 =ΔPAN-ΔPANNi = 0 ，DeltaPAN =蒸馏期间己内酰胺的PAN值的增加，在不含镍的蒸馏塔中在相同条件下蒸馏期间PAN己内酰胺的PAN数量的增加。 在蒸馏步骤之前，将镍从己内酰胺溶液中除去。

公开(公告)号：US20060041122A1

公开(公告)日：2006-02-23

申请号：US10534802

申请日：2003-11-11

Applicant: Rolf-Hartmuth Fischer ,  Hermann Luyken ,  Andreas Ansmann ,  Peter Babler ,  Christoph Benisch ,  Stefan Maixner ,  Johann-Peter Melder

Inventor： Rolf-Hartmuth Fischer ,  Hermann Luyken ,  Andreas Ansmann ,  Peter Babler ,  Christoph Benisch ,  Stefan Maixner ,  Johann-Peter Melder

IPC: C07D201/16

CPC classification number: C07D201/16 ,  C07D201/08

Abstract: 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.

Abstract translation: 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％。

公开(公告)号：US06914140B1

公开(公告)日：2005-07-05

申请号：US09546143

申请日：2000-04-10

Applicant: Peter Karl Matzinger ,  Michelangelo Scalone ,  Ulrich Zutter

Inventor： Peter Karl Matzinger ,  Michelangelo Scalone ,  Ulrich Zutter

IPC: C07D223/08 ,  C07D223/12 ,  C07D498/04 ,  C07D201/16

CPC classification number: C07D223/12 ,  C07D223/08

Abstract: A novel process for the manufacture of compounds of the formula wherein R1 and R2 independently represent aroyl. The present invention also concerns novel intermediates used in the novel process for making compounds of formula I.

Abstract translation: 用于制备下式化合物的新方法其中R 1和R 2独立地代表芳酰基。 本发明还涉及用于制备式I化合物的新方法中的新型中间体。

公开(公告)号：US20050029086A1

公开(公告)日：2005-02-10

申请号：US10487673

申请日：2002-08-23

Applicant: Louise Groot Zevert ,  Joseph Bindels ,  Rita Joosten ,  Joannes Lemmens ,  Eelco Mostert

Inventor： Louise Groot Zevert ,  Joseph Bindels ,  Rita Joosten ,  Joannes Lemmens ,  Eelco Mostert

IPC: C07D223/10 ,  C07D201/16 ,  C07D233/10 ,  B01D3/34 ,  C07D307/02

CPC classification number: C07D201/16 ,  C07D223/10

Abstract: The invention relates to a process for distilling alkaline caprolactam product at reduced pressure, said alkaline caprolactam product comprising (i) caprolactam, (ii) organic impurities, and (iii) one or more bases selected from the group consisting of alkali hydroxide and alkali amino caproate, characterized in that the alkalinity of the alkaline caprolactam product is less than 5 meq. per kg of caprolactam.

Abstract translation: 本发明涉及一种在减压下蒸馏碱性己内酰胺产物的方法，所述碱性己内酰胺产物包含（i）己内酰胺，（ii）有机杂质，和（iii）一种或多种选自碱金属氢氧化物和碱性氨基 己酸盐，其特征在于碱性己内酰胺产物的碱度小于5meq。 每公斤己内酰胺。

公开(公告)号：US6069246A

公开(公告)日：2000-05-30

申请号：US297016

申请日：1999-07-27

Applicant: Henri Chiarelli ,  Philippe Leconte

Inventor： Henri Chiarelli ,  Philippe Leconte

IPC: C07D201/08 ,  C07D201/16

CPC classification number: C07D201/08

Abstract: The present invention relates to the treatment of lactams obtained directly from their synthesis process, avoiding the formation of oligomers as far as possible. The invention consists, more precisely, of a process for treating a lactam using the reaction flow obtained from a cyclizing hydrolysis of an aminonitrile, characterized in that the reaction flow leaving the hydrolysis reactor is cooled, over a period of less than or equal to 1 hour, to a temperature below or equal to 150.degree. C. before it is fractionated.

Abstract translation: PCT No.PCT / FR97 / 01903 Sec。 371日期：1999年7月27日 102（e）1999年7月27日PCT 1997年10月23日PCT公布。 公开号WO98 / 17641 日期：1998年04月30日本发明涉及直接从其合成方法获得的内酰胺的处理，尽可能避免形成低聚物。 本发明更准确地说是使用由氨基腈的环化水解获得的反应流程来处理内酰胺的方法，其特征在于，离开水解反应器的反应流在小于或等于1的时间内被冷却 小时，然后分馏至低于或等于150℃的温度。

公开(公告)号：US6045703A

公开(公告)日：2000-04-04

申请号：US94651

申请日：1998-06-15

Applicant: Jay Fingeret Miller

Inventor： Jay Fingeret Miller

IPC: C07D201/16 ,  B01D15/08

CPC classification number: C07D201/16

Abstract: This invention relates to a process for separating epsilon caprolactam from a feed mixture comprising epsilon caprolactam and octahydrophenazine which process comprises contacting under adsorption conditions said mixture with an adsorbent, selectively adsorbing said epsilon caprolactam to substantial exclusion of said octahydrophenazine, removing the non-adsorbed portion of the feed mixture from contact with the adsorbent, and thereafter recovering high purity epsilon caprolactam by desorption under desorption conditions. The process can also be conducted in a batch or semi-batch manner or in a continuous manner using moving bed or simulated moving bed technologies.

Abstract translation: 本发明涉及从含有ε-己内酰胺和八氢吩嗪的进料混合物中分离ε-己内酰胺的方法，该方法包括在吸附条件下将所述混合物与吸附剂接触，选择性吸附所述ε-己内酰胺以显着排除所述八氢吩嗪，除去未吸附部分 的进料混合物与吸附剂接触，然后通过在解吸条件下解吸回收高纯度ε-己内酰胺。 该方法也可以使用移动床或模拟移动床技术以间歇或半间歇的方式或以连续方式进行。