公开(公告)号：US11884632B2

公开(公告)日：2024-01-30

申请号：US17212530

申请日：2021-03-25

Applicant: ZHEJIANG HENGYI PETROCHEMICAL RESEARCH INSTITUTE CO., LTD.

Inventor： Shibiao Cheng ,  Songlin Wang ,  Xi Li ,  Han Wang ,  Fei Shen ,  Xinping Zhang ,  Zhaobin Jiang ,  Zhimin Hu

IPC: C07D223/10 ,  C07D201/06 ,  C07D201/16 ,  B01J29/70 ,  B01J35/08 ,  B01J37/00 ,  B01J37/04 ,  B01J37/08

CPC classification number: C07D223/10 ,  B01J29/70 ,  B01J35/08 ,  B01J37/0036 ,  B01J37/04 ,  B01J37/08

Abstract: The present disclosure discloses a method for preparing caprolactam including: (1) contacting cyclohexanone oxime with a catalyst to carry out reaction in the presence of ethanol and under the condition of gas phase Beckmann rearrangement reaction of cyclohexanone oxime; (2) separating the reaction product obtained in step (1) to produce an ethanol solution of crude caprolactam, and then separating the ethanol solution of crude caprolactam to obtain ethanol and crude caprolactam; (3) removing impurities with boiling points lower than that of caprolactam in the crude caprolactam to obtain a light component removal product; (4) mixing the light component removal product with a crystallization solvent to carry out crystallization and solid-liquid separation to obtain a crystalline crystal; (5) subjecting the crystalline crystal to a hydrogenation reaction; wherein the crystallization solvent contains 0.1-2 wt % of ethanol.

公开(公告)号：US20180093949A1

公开(公告)日：2018-04-05

申请号：US15562518

申请日：2015-06-04

Applicant: ANTHEA AROMATICS PRIVATE LIMITED

Inventor： Manoj Kumar MOHAPATRA ,  Ramamohanrao BENDAPUDI ,  Paul Vincent MENACHERRY ,  Vincent PAUL

IPC: C07D201/06 ,  C07D201/16 ,  C07D227/087 ,  C01G9/02 ,  C01B21/14

CPC classification number: C07D201/06 ,  B01D3/36 ,  C01B21/14 ,  C01G9/02 ,  C07D201/04 ,  C07D201/16 ,  C07D227/087

Abstract: Disclosed herein is an efficient, economical, industrially advantageous, straight-through process for the preparation of cyclic amides, also referred as lactams, in substantially pure form and high yield, from the corresponding cyclic ketones and a hydroxylammonium salt, using a combination of amphoteric metal oxide or amphoteric masked metal oxide and a base.

公开(公告)号：US20160221943A1

公开(公告)日：2016-08-04

申请号：US14917808

申请日：2014-07-07

Applicant: TECHNIP ZIMMER GMBH

Inventor： Andreas Bormann ,  Manfred Albrecht ,  Franz Samlitschka

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A process for the recovery of ε-caprolactam from extract water of polycaprolactam obtained by hydrolytic polymerization, wherein the extract water is concentrated, subsequently contained oligomers are depolymerized, non-depolymerizable impurities are separated, water and low-boiling impurities are removed, wherein for adjusting the purity of the recovered ε-caprolactam and the energy consumption used for the process a part of the product is removed from the process as intermediate products.

Abstract translation: 从通过水解聚合获得的聚己内酰胺的萃取水中回收ε-己内酰胺的方法，其中提取水浓缩，随后包含的低聚物被解聚，不可解聚的杂质被分离，除去水和低沸点杂质，其中对于 调整回收的ε-己内酰胺的纯度和用于该方法的一部分产品所用的能量消耗作为中间产物。

公开(公告)号：US07576198B1

公开(公告)日：2009-08-18

申请号：US10069999

申请日：2000-08-25

Applicant: Takashi Kawasuji ,  Tomokazu Yoshinaga

Inventor： Takashi Kawasuji ,  Tomokazu Yoshinaga

IPC: C07D201/16 ,  C07D267/02 ,  C07D281/08 ,  C07D515/00 ,  A61K38/00

CPC classification number: C07D213/64 ,  C07D213/55 ,  C07D213/56 ,  C07D213/57 ,  C07D213/65 ,  C07D213/68 ,  C07D215/233 ,  C07D235/16 ,  C07D239/26 ,  C07D239/52 ,  C07D241/12 ,  C07D241/18 ,  C07D241/20 ,  C07D263/32 ,  C07D277/30 ,  C07D285/12 ,  C07D401/06 ,  C07D401/12 ,  C07D403/06 ,  C07D403/12 ,  C07D405/12 ,  C07D413/06 ,  C07D417/06 ,  C07D473/00 ,  C07F9/6512

Abstract: A compound of the formula (I): wherein X is hydroxy or the like; Y is —C(═R2)—R3—R4 wherein R2 and R3 is oxygen atom or the like, R4 is hydrogen, optionally substituted alkyl, optionally substituted heteroaryl or the like; Z is hydrogen or the like; Z1 and Z3 each is independently a bond, alkylene or the like; Z2 is a bond, alkylene, —O— or the like; R1 is optionally substituted aryl, optionally substituted heteroaryl or the like; p is 0 to 2 and ring (A) is optionally substituted aromatic heterocycle, a tautomer of itself, a prodrug thereof, a pharmaceutically acceptable salt thereof or a solvate thereof has an integrase-inhibiting activity.

Abstract translation: 式（I）的化合物：其中X是羟基等; Y是-C（-R 2）-R 3 -R 4，其中R 2和R 3是氧原子等，R 4是氢，任选取代的烷基，任选取代的杂芳基等; Z是氢等; Z 1和Z 3各自独立地为键，亚烷基等; Z2是键，亚烷基，-O-等; R1是任选取代的芳基，任选取代的杂芳基等; p为0至2，环（A）为任选取代的芳族杂环，其本身的互变异构体，其前药，其药学上可接受的盐或其溶剂合物具有整合酶抑制活性。

公开(公告)号：US20080058513A1

公开(公告)日：2008-03-06

申请号：US11897883

申请日：2007-08-31

Applicant: Chien-Hsien Li ,  Shou-Li Luo

Inventor： Chien-Hsien Li ,  Shou-Li Luo

IPC: C07D201/16

CPC classification number: C07D223/10 ,  C07D201/16

Abstract: A system for purifying an aqueous solution of crude caprolactam is provided, which includes a filtration zone (A), an inspection unit (B), a purification zone (C), and a first temporary storage tank (D). The filtration zone (A) contains a filtration apparatus though which an aqueous solution of crude caprolactam is filtered to remove ionic impurities therein, so as to obtain caprolactam-containing filtrate; the inspection unit (B) is used for judging the filtrate from the filtration zone (A) meets the preset inspection standards; the purification zone(C) is used for concentrating and further purifying filtrate meeting the preset inspection standards, thereby forming a final caprolactam product; and the first temporary storage tank (D) is used for receiving the filtrate not meeting the preset inspection standards, which is then mixed with the aqueous solution of crude caprolactam and delivered back to the filtration zone (A).

Abstract translation: 提供了一种用于纯化粗己内酰胺水溶液的体系，其包括过滤区（A），检查单元（B），净化区（C）和第一临时储罐（D）。 过滤区（A）含有过滤装置，通过其过滤粗己内酰胺水溶液以除去其中的离子杂质，得到含己内酰胺的滤液; 检查单元（B）用于判断过滤区域（A）的滤液符合预设的检验标准; 净化区（C）用于浓缩并进一步净化满足预设检查标准的滤液，从而形成最终的己内酰胺产品; 并且第一临时储罐（D）用于接收不符合预设检查标准的滤液，然后将其与粗己内酰胺水溶液混合并输送到过滤区（A）。

公开(公告)号：US07173127B2

公开(公告)日：2007-02-06

申请号：US10457831

申请日：2003-06-09

Applicant: Claus Born ,  Rudolf K{hacek over (a)}mpf ,  Joachim Seelig ,  Reinhard Wolf

Inventor： Claus Born ,  Rudolf K{hacek over (a)}mpf ,  Joachim Seelig ,  Reinhard Wolf

IPC: C07D201/16

CPC classification number: C07D201/12

Abstract: This invention relates to a continuous and efficient method for the manufacture of highly pure caprolactam suitable for the polycondensation of Polyamide 6 (polycaprolactam) from polyamide waste. In particular the invention relates to a method for the manufacture of caprolactam from waste containing polyamides, including the steps a) depolymerisation of the waste containing polyamides, whereby a caprolactam raw material and a flow containing secondary constituents or additives is obtained, b) at least one distillation of the caprolactam raw material, and c) at least one crystallisation of the caprolactam material obtained in step b), by which means caprolactam is obtained, whereby at least part of the caprolactam obtained in step c) with a permanganate number of

Abstract translation: 本发明涉及用于制备适用于聚酰胺废物聚酰胺6（聚己内酰胺）缩聚的高纯度己内酰胺的连续和有效的方法。 具体地说，本发明涉及一种从含有聚酰胺的废物中制造己内酰胺的方法，包括以下步骤：a）对含有废物的聚酰胺进行解聚，由此得到己内酰胺原料和含有二级成分或添加剂的流体，b）至少 己内酰胺原料的一次蒸馏，和c）步骤b）中获得的己内酰胺材料的至少一种结晶，通过该方法获得己内酰胺，由此至少部分步骤c）中获得的己内酰胺的高锰酸盐数目< 10000秒 并且在解聚之前和/或期间，将含有<85％的UV透射率加入到含废物的聚酰胺中。

公开(公告)号：US20040110943A1

公开(公告)日：2004-06-10

申请号：US10468263

申请日：2004-01-14

Inventor： Maria Louisa Christina Dsinter-De Hondt ,  Joannes Albertus Wilhelmus Lemmens

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: Process for recovering caprolactam from a solution comprising caprolactam dissolved in an organic solvent, said process comprising: a) washing the solution with water or an aqueous alkaline solution, resulting in a washed solution comprising caprolactam and organic solvent and in a washing residue, b) evaporating organic solvent from the washed solution, resulting in caprolactam product, c) optionally, hydrogenating the caprolactam product, d) optionally, evaporating water from the caprolactam product, e) distilling the caprolactam product to recover caprolactam and a distillation residue, f) extracting the distillation residue with an organic solvent in the presence of water to obtain (i) an extract comprising caprolactam dissolved in organic solvent and (ii) an aqueous effluent, and g) recycling the extract to step a) or b).

Abstract translation: 从包含溶解在有机溶剂中的己内酰胺的溶液中回收己内酰胺的方法，所述方法包括：a）用水或碱性水溶液洗涤溶液，得到包含己内酰胺和有机溶剂的洗涤溶液，并在洗涤残渣中，b） 从洗涤的溶液中蒸发有机溶剂，得到己内酰胺产物，c）任选地使己内酰胺产物氢化，d）任选地从己内酰胺产物蒸发水，e）蒸馏己内酰胺产物以回收己内酰胺和蒸馏残渣，f） 在水存在下用有机溶剂蒸馏残余物，以获得（i）包含溶解在有机溶剂中的己内酰胺和（ii）含水流出物的提取物，和g）将提取物再循环到步骤a）或b）。

公开(公告)号：US20030143146A1

公开(公告)日：2003-07-31

申请号：US10332585

申请日：2003-01-10

Inventor： Hermann Luyken

IPC: C01C001/00 ,  C07D201/16

CPC classification number: C07C231/24 ,  C07D201/16

Abstract: A process is provided for the separation of ammonia (I) from mixtures (II) containing ammonia (I) and an amide (IV) selected from the group consisting of a lactam (IVa), an oligomer (IVb) and a polymer (IVc) with amide groups in the main chain, said amide (IV) having been obtained by reacting educts (III), selected from the group consisting of nitrites (IIIa), amines (IIIb), amino nitrites (IIIc) and amino amides (IIId), with water, wherein a) the educt (III) is reacted with water in the liquid phase, in the presence of an organic liquid diluent (V), to give a mixture (II) containing the amide (IV) and the ammonia (I), the diluent (V) exhibiting a miscibility gap with water under certain quantity, pressure and temperature conditions, b) the mixture (II) is converted under quantity, pressure and temperature conditions such that the diluent (V) and the water are in liquid form and exhibit a miscibility gap, to give a two-phase system consisting of a phase (VII) containing a higher proportion of diluent (V) than water, and a phase (VIII) containing a higher proportion of water than diluent (V), c) the phase (VII) is separated from the phase (VIII), d) all or part of the ammonia present in the phase (VII) is separated off by extraction (a) with a water-containing mixture (IX) to give an aqueous mixture (X) containing the ammonia which has been separated off, and a mixture (XI) containing less ammonia than the phase (VII), and e) the diluent (V), any residual ammonia and any by-products selected from the group consisting of low-boiling components, high-boiling components and unreacted compounds (III) are separated from the mixture (XI) to give the amide (IV).

Abstract translation: 提供了一种从含有氨（I）和选自内酰胺（IVa），低聚物（IVb）和聚合物（IVc）的酰胺（IV）的混合物（II）中分离氨（I）的方法 所述酰胺（IV）是通过使选自由亚硝酸盐（IIIa），胺（IIIb），氨基亚硝酸盐（IIIc）和氨基酰胺（IIId）组成的组的离析物（III）反应而获得的 ），其中a）在液相中，在有机液体稀释剂（V）的存在下，水解（III）与水反应，得到含有酰胺（IV）和氨的混合物（II） （I）中，稀释剂（V）在一定量，压力和温度条件下表现出与水的混溶性间隙，b）混合物（II）在数量，压力和温度条件下转化，使得稀释剂（V）和水 呈液态并显示混溶性间隙，得到由含有较高比例的相（VII）组成的两相体系 稀释剂（V）比水，和含有比稀释剂（V）更高比例的水的相（VIII），c）相（VII）从相（VIII）分离，d）全部或部分 通过用含水混合物（IX）萃取（a）分离相（VII）中存在的氨，得到含有已分离出的氨的含水混合物（X）和含有较少量的混合物（XI） （VII）中的氨，e）稀释剂（V），任选的残余氨和选自低沸点组分，高沸点组分和未反应化合物（III）的任何副产物与 混合物（Ⅺ），得到酰胺（Ⅳ）。

公开(公告)号：US20020005343A1

公开(公告)日：2002-01-17

申请号：US09226718

申请日：1999-01-07

Inventor： YVONNE FRENTZEN ,  NICOLAAS HAASEN ,  HENRICUS F.W. WOLTERS

IPC: B01D003/38 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: The invention relates to a process for the separation of a ketoxime or aldoxime from a ketoxime- or aldoxime-containing amide mixture in which the ketoxime or aldoxime is separated from the amide mixture by means of distillation. This has proved to be a very simple and direct method for separating the ketoxime and/or aldoxime from the desired amide.

Abstract translation: 本发明涉及从含有酮肟或醛肟的酰胺混合物中分离酮肟或醛肟的方法，其中酮肟或醛肟通过蒸馏与酰胺混合物分离。 已证明这是一种非常简单和直接的方法，用于将酮肟和/或醛肟与所需酰胺分离。

公开(公告)号：US5869654A

公开(公告)日：1999-02-09

申请号：US844539

申请日：1997-04-18

Applicant: Stylianos Sifniades ,  Alan Bart Levy

Inventor： Stylianos Sifniades ,  Alan Bart Levy

IPC: C07D201/12 ,  C07D201/16

CPC classification number: C07D201/16 ,  C07D201/12

Abstract: The present invention provides an improved process for the recovery of caprolactam from polycaprolactam processing waste. The present process for depolymerizing polycaprolactam waste to form caprolactam comprises the step of: in the absence of added catalyst, contacting the polycaprolactam waste with superheated steam at a temperature of about 250.degree. C. to about 400.degree. C. and at a pressure within the range of about 1.5 atm to about 100 atm and substantially less than the saturated vapor pressure of water at the temperature wherein a caprolactam-containing vapor stream is formed.The formed caprolactam may then be used in the production of engineered resins and fibers.

Abstract translation: 本发明提供了从聚己内酰胺处理废物中回收己内酰胺的改进方法。 用于解聚聚己内酰胺废物形成己内酰胺的本发明方法包括以下步骤：在不加入催化剂的情况下，在约250℃至约400℃的温度和 范围为约1.5atm至约100atm，并且在其中形成含己内酰胺的蒸汽流的温度下，基本上小于饱和的水蒸气压。 然后，所形成的己内酰胺可以用于工程化树脂和纤维的生产。