公开(公告)号：US09908785B2

公开(公告)日：2018-03-06

申请号：US14899579

申请日：2014-06-20

Applicant: CAP III B.V.

Inventor： Johan Thomas Tinge ,  Geert Ekkelenkamp ,  Robert Geertman

IPC: B01D9/00 ,  C01C1/24 ,  C01C1/248 ,  C07D201/16 ,  C07D201/04 ,  C07C249/08

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.

公开(公告)号：US20130211072A1

公开(公告)日：2013-08-15

申请号：US13516296

申请日：2010-12-17

Applicant: Maria Elena Avramescu ,  Johan Thomas Tinge

Inventor： Maria Elena Avramescu ,  Johan Thomas Tinge

IPC: C07D223/10

CPC classification number: C07D223/10 ,  C07D201/16

Abstract: The invention relates to a process for treating an aqueous solution containing ε-caprolactam, ammonium sulphate and one or more other impurities, comprising one or more organic impurities from a caprolactam production process and optionally other salts than ammonium sulphate, by means of a membrane process, thereby obtaining a retentate and a permeate, in which process the membrane used is selected from the group of polyether sulphone membranes, sulphonated polyether sulphone membranes, polyester membranes, polysulphone membranes, aromatic polyamide membranes, polyvinyl alcohol membranes, polypiperazine membranes, cellulose acetate membranes, titanium oxide membranes, zirconium oxide membranes and aluminium oxide membranes, having a molecular weight cut off in the range of 100-1000 g/mol; and wherein more than 60 wt. % of the caprolactam in the aqueous solution is passed through a membrane to the permeate side, to obtain a purified caprolactam containing permeate stream, and wherein at least 50 wt. % of the organic impurities are retained in the retentate solution.

Abstract translation: 本发明涉及一种通过膜方法处理含有ε-己内酰胺，硫酸铵和一种或多种其它杂质的水溶液的方法，其包含一种或多种有机杂质，其由己内酰胺生产方法和任选的除硫酸铵以外的其它盐 从而获得渗余物和渗透物，其中使用的膜选自聚醚砜膜，磺化聚醚砜膜，聚酯膜，聚砜膜，芳族聚酰胺膜，聚乙烯醇膜，聚哌嗪膜，醋酸纤维素膜 ，氧化钛膜，氧化锆膜和氧化铝膜，分子量在100-1000g / mol范围内切断; 并且其中大于60wt。 将水溶液中的己内酰胺的百分比通过膜渗透到一侧，以获得含有纯化的己内酰胺的渗透物流，并且其中至少50wt。 ％的有机杂质保留在渗余液中。

公开(公告)号：US20110218344A1

公开(公告)日：2011-09-08

申请号：US13109450

申请日：2011-05-17

Applicant: Hideto SUGIURA ,  Toru Inaoka ,  Shigeyuki Nozaki ,  Yoshihisa Oka

Inventor： Hideto SUGIURA ,  Toru Inaoka ,  Shigeyuki Nozaki ,  Yoshihisa Oka

IPC: C07D207/273

CPC classification number: C07D207/267 ,  B01D9/0059 ,  C07D201/16

Abstract: A method for producing N-vinyl-2-pyrrolidone by crystallization including: controlling a water content in a feed N-vinyl-2-pyrrolidone solution at an inlet of a crystallizer so as to be not lower than 0.7% by weight and not higher than 10% by weight based on the total weight of the N-vinyl-2-pyrrolidone solution; and supplying the feed N-vinyl-2-pyrrolidone solution to a crystallization process.

Abstract translation: 通过结晶生产N-乙烯基-2-吡咯烷酮的方法包括：将结晶器入口处的进料N-乙烯基-2-吡咯烷酮溶液中的水含量控制在不低于0.7重量％且不高于 基于N-乙烯基-2-吡咯烷酮溶液的总重量的10重量％以上; 并将进料N-乙烯基-2-吡咯烷酮溶液供给至结晶过程。

公开(公告)号：US20110105793A1

公开(公告)日：2011-05-05

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: C07C231/24

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：US20090312542A1

公开(公告)日：2009-12-17

申请号：US12474968

申请日：2009-05-29

Applicant: Chien-Hsien LI

Inventor： Chien-Hsien LI

IPC: C07D201/16 ,  B01J19/00

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：US07615137B2

公开(公告)日：2009-11-10

申请号：US10486727

申请日：2002-08-23

Applicant: Arnold G M Jetten ,  Nicolaas F Haasen ,  Gerardus W A Hangx

Inventor： Arnold G M Jetten ,  Nicolaas F Haasen ,  Gerardus W A Hangx

IPC: B01D3/34 ,  C07D201/16

CPC classification number: C07D201/16 ,  C07D223/10

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

Abstract translation: 提供了一种连续的方法从己内酰胺产物中回收己内酰胺，其中包括（i）己内酰胺，（ii）杂质和（iii）水，通过（a）向己酸内酰胺产物中加入碱金属氢氧化物，其量不超过100 mmol碱金属氢氧化物/ kg己内酰胺; （b）使至少部分加入的碱金属氢氧化物反应形成碱性氨基己酸酯，得到富含己酸的己内酰胺产物; 和（c）在减压下蒸馏富含己内酰胺的己内酰胺产物。

公开(公告)号：US20080230368A1

公开(公告)日：2008-09-25

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

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.

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。

公开(公告)号：US07217818B2

公开(公告)日：2007-05-15

申请号：US10534802

申请日：2003-11-11

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

Inventor： Rolf-Hartmuth Fischer ,  Hermann Luyken ,  Andreas Ansmann ,  Peter Bassler ,  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：US20070060750A1

公开(公告)日：2007-03-15

申请号：US10565774

申请日：2004-07-16

Applicant: Joannes Albertus Wilhelmus Lemmens ,  Theodorus Smeets ,  Paul Brandts ,  Koen Ceyssens

Inventor： Joannes Albertus Wilhelmus Lemmens ,  Theodorus Smeets ,  Paul Brandts ,  Koen 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ΔPANNiN = 3，其中ΔPANNi=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：US07129347B2

公开(公告)日：2006-10-31

申请号：US10897472

申请日：2004-07-23

Applicant: Rudolf Kampf ,  Reinhard Wolf ,  Joachim Seelig

Inventor： Rudolf Kampf ,  Reinhard Wolf ,  Joachim Seelig

IPC: C07D201/12

CPC classification number: C07D201/16 ,  C07D201/12

Abstract: The invention relates to a method for the continuous production of caprolactam from waste containing polyamide, comprising a) depolymerisation of the waste containing polyamide, whereby a caprolactam raw material and, where applicable, a flow containing secondary constituents or additives is obtained, and b) irradiation of the caprolactam raw material with UV radiation.

Abstract translation: 本发明涉及一种从含有聚酰胺的废物中连续生产己内酰胺的方法，其包括：a）含有聚酰胺的废物的解聚，由此得到己内酰胺原料，并且在适用的情况下获得含有二级成分或添加剂的流动，以及b） 紫外线照射己内酰胺原料。