公开(公告)号：US07384518B2

公开(公告)日：2008-06-10

申请号：US10296512

申请日：2001-05-28

Applicant: Daniel Amoros ,  Philippe Leconte ,  Pierre Coqueret

Inventor： Daniel Amoros ,  Philippe Leconte ,  Pierre Coqueret

IPC: B01D3/34 ,  C07D201/08 ,  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 said 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 comprising compounds more volatile than the lactam, a fraction comprising the lactam to be recovered to the degree of desired purity and a distillation tails comprising 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. The method and plant enables a high rate of recovery of the caprolactam contained in the hydrolysis medium, while observing required criteria of purity.

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己腈水解获得的ε-己内酰胺的纯化，其包括从水解反应介质中除去氨，然后以纯化形式从所述介质中回收内酰胺。 回收是通过在碱的存在下至少进行内消旋而进行的，所述碱生产任选地含有比内酰胺更易挥发的化合物的前列馏分，包含待回收的内酰胺至所需纯度的馏分和蒸馏 尾部包含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。 该方法和设备能够在观察所需的纯度标准的同时使包含在水解介质中的己内酰胺的回收率高。

公开(公告)号：US20050011744A1

公开(公告)日：2005-01-20

申请号：US10486727

申请日：2002-08-23

Applicant: Arnold Jetten ,  Nicolaas Haasen ,  Gerardus Hangx

Inventor： Arnold Jetten ,  Nicolaas Haasen ,  Gerardus Hangx

IPC: C07D223/10 ,  C07D201/16 ,  C07D233/10 ,  B01D3/42 ,  C07C51/44

CPC classification number: C07D201/16 ,  C07D223/10

Abstract: The invention relates to a continuous process for recovering caprolactam from aqueous caprolactam product, said aqueous caprolactam product comprising (i) caprolactam, (ii) impurities, and (iii) water, said process comprising: adding alkali hydroxide to the aqueous caprolactam product, in an amount of not more than 100 mmol alkali hydroxide per kg of caprolactam; reacting at least part of the added alkali hydroxide to form alkali amino caproate, to obtain a caproate-enriched caprolactam product; and distilling the caproate-enriched caprolactam product at reduced pressure.

Abstract translation: 本发明涉及从己内酰胺产物水中回收己内酰胺的连续方法，所述含水己内酰胺产品包括（i）己内酰胺，（ii）杂质和（iii）水，所述方法包括：向含水己内酰胺产物中加入碱金属氢氧化物 每公斤己内酰胺不超过100mmol碱金属氢氧化物; 使至少部分加入的碱金属氢氧化物反应形成碱式氨基己酸酯，得到富含己酸的己内酰胺产物; 并在减压下蒸馏富含己内酰胺的己内酰胺产物。

公开(公告)号：US06841666B2

公开(公告)日：2005-01-11

申请号：US10473077

申请日：2002-03-22

Applicant: Wim Buijs ,  Henricus Franciscus Wilhelmus Wolters

Inventor： Wim Buijs ,  Henricus Franciscus Wilhelmus Wolters

IPC: C07D201/08 ,  C07D201/12 ,  C07D201/16 ,  C08G69/16 ,  C08L77/00

CPC classification number: C08G69/16 ,  C07D201/08

Abstract: The invention relates to a process for the preparation ε-caprolactam starting from 6-aminocapronitrile by hydrolysis/oligomerisation followed by de-oligomerisation/cyclisation using superheated steam characterized in that the hydrolysis/oligomerisation is performed with superheated steam converting 6-aminocapronitrile into a molten phase and a gas phase comprising ammonia, ammonia is continuously separated off and the de-oligomerisation/cyclisation is performed by treating the molten phase further with superheated steam. The invention also relates to a process for the preparation of ε-caprolactam starting from 6-aminocapronitrile by hydrolysis/oligomerisation followed by de-oligomerisation/cyclisation characterized in that the preparation is performed in a horizontal scraped-surface reactor, the hydrolysis/oligomerisation is performed with superheated steam converting 6-aminocapronitrile into a molten phase and a gas phase comprising ammonia, ammonia is continuously separated off and the de-oligomerisation/cyclisation is performed by treating the molten phase further with superheated steam.

Abstract translation: 本发明涉及一种从6-氨基己腈开始通过水解/低聚制备ε-己内酰胺，然后使用过热蒸汽进行脱低聚/环化的方法，其特征在于水解/低聚反应用过热蒸汽将6-氨基己腈转化成熔融 相和包含氨的气相，氨被连续分离，并且通过用过热蒸汽进一步处理熔融相进行脱低聚/环化。 本发明还涉及从6-氨基己腈开始制备ε-己内酰胺的方法，其通过水解/低聚，接着进行脱低聚/环化，其特征在于制备在水平刮面反应器中进行，水解/低聚是 使用过热蒸汽将6-氨基己腈转化成熔融相和包含氨的气相，连续分离氨，通过用过热蒸汽进一步处理熔融相进行脱低聚/环化。

公开(公告)号：US6433166B2

公开(公告)日：2002-08-13

申请号：US88736001

申请日：2001-06-25

Applicant: SUMITOMO CHEMICAL CO

Inventor： SHIMAZU YASUMOTO ,  UMIDA HIROYUKI ,  FUKAO MASAMI

IPC: C07D223/10 ,  C07B61/00 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A high purity epsi-caprolactam is prepared by pouring a molten crude epsi-caprolactam and a solvent comprising an aliphatic hydrocarbon and having a lower temperature than that of the crude epsi-caprolactam, into a vessel and mixing them to obtain a first slurry containing a crystallized epsi-caprolactam. The slurry is then subjected to a solid-liquid separation to obtain epsi-caprolactam and a first liquid phase. This process can effectively remove impurities from a crude epsi-caprolactam, which is obtained by for example, subjecting cyclohexanone oxime to the Beckmann rearrangement.

Abstract translation: 通过将熔融的原始ε-己内酰胺和包含脂族烃并且具有比原始ε-己内酰胺低的温度的溶剂倾倒到容器中并混合以制备含有一种高纯度ε-己内酰胺的第一浆料， 结晶的ε-己内酰胺。 然后将浆料进行固液分离以获得ε-己内酰胺和第一液相。 该方法可以有效地除去通过例如使环己酮肟进行贝克曼重排得到的粗ε-己内酰胺的杂质。

公开(公告)号：US06111099A

公开(公告)日：2000-08-29

申请号：US5512

申请日：1998-01-12

Applicant: Yvonne H Frentzen ,  Marcellinus P. G. Thijert ,  Rudolf L. Zwart

Inventor： Yvonne H Frentzen ,  Marcellinus P. G. Thijert ,  Rudolf L. Zwart

IPC: C07D201/12 ,  C07D201/16

CPC classification number: C07D201/12

Abstract: A process for depolymerizing nylon 6 and recovering caprolactam from the depolymerized products by extraction with alkyl phenolic compounds. Process steps include (a) treating a first mixture comprising nylon 6 with water at a temperature between about 200.degree. C. and about 400.degree. C. to yield a second mixture comprising depolymerized nylon 6 components, wherein the second mixture contains caprolactam at a concentration between about 5 wt. % and about 35 wt. %; (b) optionally, separating insoluble material from the second mixture; (c) extracting the second mixture with an extraction agent to yield an aqueous raffinate third mixture and an organic phase fourth mixture comprising caprolactam and the extraction agent, wherein the extraction agent is an alkyl phenol having a boiling point higher than that of the caprolactam; (d) recovering caprolactam from the organic phase fourth mixture by distillation; (e) recycling the aqueous raffinate third mixture to step (a).

Abstract translation: 一种通过用烷基酚类化合物萃取从解聚产物中解聚尼龙6并回收己内酰胺的方法。 工艺步骤包括（a）在约200℃至约400℃之间的温度下处理包含尼龙6的第一混合物与水，以产生包含解聚的尼龙6组分的第二混合物，其中第二混合物含有浓度为的己内酰胺 约5wt。 ％和约35wt。 ％; （b）任选地，从第二混合物中分离不溶物质; （c）用提取剂萃取第二混合物，得到含水萃余液第三混合物和包含己内酰胺和提取剂的有机相第四混合物，其中提取剂是沸点高于己内酰胺的沸点的烷基苯酚; （d）通过蒸馏从有机相第四混合物中回收己内酰胺; （e）将含水萃余液第三混合物再循环到步骤（a）。

公开(公告)号：US6100396A

公开(公告)日：2000-08-08

申请号：US230588

申请日：1999-04-23

Applicant: Hubert Gayet ,  Philippe Leconte ,  Philippe Perrona

Inventor： Hubert Gayet ,  Philippe Leconte ,  Philippe Perrona

IPC: C07D203/16 ,  C07C253/34 ,  C07D201/08 ,  C07D201/16

CPC classification number: C07D201/16 ,  C07C253/34 ,  C07D201/08

Abstract: A method for purifying lactams by liquid-liquid extraction and/or processing with an ion exchange resin is disclosed. The method is useful for purifying lactams produced by the cyclising vapour-phase hydrolysis of an aliphatic aminonitrile, and comprises removing the major part of the ammonia before subjecting the lactam to liquid-liquid extraction by means of a solvent including an acidic solvent and/or contacting said lactam with a cation exchange resin. In most applications of the lactam, it is preferable to carry out a hydrogenation step on the compounds of the lactam solution comprising unsaturations, prior to or in addition to the liquid-liquid extraction step and/or the acidic resin contact step. The purification method may also include an oxidation step in addition to or instead of the hydrogenation step. Said method is preferably combined with a distillation step in the presence of a base.

Abstract translation: PCT No.PCT / FR97 / 01426 Sec。 371日期1999年4月23日第 102（e）1999年4月23日PCT PCT 1997年7月31日PCT公布。 公开号WO98 / 05636 日期1998年2月12日公开了通过液 - 液萃取和/或用离子交换树脂处理来提纯内酰胺的方法。 该方法可用于纯化通过脂族氨基腈的气相汽相水解产生的内酰胺，并且包括在将内酰胺进行液 - 液萃取之前，通过包括酸性溶剂和/或 使所述内酰胺与阳离子交换树脂接触。 在内酰胺的大多数应用中，优选在液 - 液萃取步骤和/或酸性树脂接触步骤之前或之后对包含不饱和的内酰胺溶液的化合物进行氢化步骤。 除了氢化步骤之外或代替氢化步骤，纯化方法还可以包括氧化步骤。 所述方法优选在碱的存在下与蒸馏步骤组合。

公开(公告)号：US6036865A

公开(公告)日：2000-03-14

申请号：US94650

申请日：1998-06-15

Applicant: Jay Fingeret Miller ,  George Ernest Keller, II

Inventor： Jay Fingeret Miller ,  George Ernest Keller, II

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 one or more epsilon caprolactam isomers selected from the group consisting of 4-ethyl-2-pyrrolidinone, 5-methyl-2-piperdinone, 3-ethyl-2-pyrrolidinone and 3-methyl-2-piperdinone which process comprises contacting under adsorption conditions said mixture with an adsorbent, selectively adsorbing said epsilon caprolactam isomers to substantial exclusion of said epsilon caprolactam, removing the non-adsorbed portion of the feed mixture from contact with the adsorbent, and thereafter recovering high purity epsilon caprolactam. The epsilon caprolactam isomers can be recovered by desorption under desorption conditions. The process can 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-己内酰胺和一种或多种ε-己内酰胺异构体的进料混合物中分离ε-己内酰胺的方法，其选自4-乙基-2-吡咯烷酮，5-甲基-2-哌啶酮，3-乙基-2-戊酮， 2-吡咯烷酮和3-甲基-2-哌啶酮，该方法包括在吸附条件下使所述混合物与吸附剂接触，选择性吸附所述ε己内酰胺异构体以显着排除所述ε-己内酰胺，从接触中除去进料混合物的未吸附部分 与吸附剂反应，然后回收高纯度ε己内酰胺。 ε-己内酰胺异构体可以通过在解吸条件下的解吸来回收。 该方法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。

公开(公告)号：US5990351A

公开(公告)日：1999-11-23

申请号：US981572

申请日：1997-12-22

Applicant: Joan Cabre ,  Victor Centellas ,  Jose Diago ,  Asuncion Esteve ,  Joan Serrat

Inventor： Joan Cabre ,  Victor Centellas ,  Jose Diago ,  Asuncion Esteve ,  Joan Serrat

IPC: C07D201/16 ,  C07C51/00 ,  C07C51/42 ,  C07C51/44 ,  C07C53/128 ,  C07C51/60

CPC classification number: C07C51/42

Abstract: A process for recovering 2,2-dimethylpropanoic acid in highly pure form from a mixture of 2,2-dimethylpropanoic acid and impurities which may be obtained in the production of a beta lactam antibiotic, by degrading impurities and separating off the volatile fragments.

Abstract translation: 从2,2-二甲基丙酸和杂质的混合物中回收高纯度的2,2-二甲基丙酸的方法，该方法可通过降解杂质和分离出挥发性片段而制备β-内酰胺抗生素。

公开(公告)号：US5637700A

公开(公告)日：1997-06-10

申请号：US297719

申请日：1994-08-30

Applicant: Hugo Fuchs ,  Gerald Neubauer ,  Claus-Ulrich Priester

Inventor： Hugo Fuchs ,  Gerald Neubauer ,  Claus-Ulrich Priester

IPC: C07B63/02 ,  C07D201/16 ,  C07D201/12

CPC classification number: C07D201/16

Abstract: Caprolactam is purified by oxidative treatment in which mixtures which essentially contain the caprolactam to be purified and unsaturated lactams are treated with oxygen or an oxygen-containing gas mixture in an alkaline medium.

Abstract translation: 通过氧化处理纯化己内酰胺，其中基本上含有要纯化的己内酰胺和不饱和内酰胺的混合物在碱性介质中用氧或含氧气体混合物处理。

公开(公告)号：US5458740A

公开(公告)日：1995-10-17

申请号：US205979

申请日：1994-03-04

Applicant: Thomas P. Losier ,  Donald R. Johnson ,  Hugo Fuchs ,  Gerald Neubauer ,  Josef Ritz

Inventor： Thomas P. Losier ,  Donald R. Johnson ,  Hugo Fuchs ,  Gerald Neubauer ,  Josef Ritz

IPC: C07D201/12 ,  C07D201/16 ,  B01D3/34

CPC classification number: C07D201/12 ,  C07D201/16 ,  Y10S203/90

Abstract: A process for the purification of caprolactam from crude caprolactam by distilling the crude caprolactam in the presence of an anorganic or organic acid.

Abstract translation: 通过在无机或有机酸的存在下蒸馏粗己内酰胺从粗己内酰胺纯化己内酰胺的方法。