公开(公告)号：EP1013644A1

公开(公告)日：2000-06-28

申请号：EP99125633.0

申请日：1999-12-22

Applicant: PRAXAIR TECHNOLOGY, INC.

Inventor： Echegaray, Diego Fernandez ,  Velloso, Antonio Augusto M. ,  Wagner, Matthew Lincoln

IPC: C07D201/06 ,  C07D201/10

CPC classification number: C07D201/06 ,  C07D201/10

Abstract: A method for production of caprolactam. The method involves:

(a) reacting air with ammonia gas in an ammonia conversion zone to produce nitric oxide;
(b) oxidizing at least a portion of the nitric oxide to nitrogen dioxide to produce an NO x -rich process gas stream;
(c) reactively absorbing the NO x -rich gas stream with phosphoric acid containing solution in an absorption zone to form nitrate ions;
(d) contacting the nitrate ions with air in a degassing zone to produce a nitrate-rich aqueous process stream;
(e) reducing the nitrate-rich aqueous stream with hydrogen in the presence of phosphoric acid to produce hydroxylammonium phosphate;
(f) oximating the hydroxylammonium phosphate with cyclohexanone to produce cyclohexanone oxime; and
(g) converting the cyclohexanone oxime to caprolactam.
According to the invention, supplemental oxygen is added downstream of the ammonia conversion zone to increase the quantity and rate of formation of nitrogen dioxide in the NO x -rich process gas stream.

Abstract translation: 一种生产己内酰胺的方法。 该方法包括：（a）在氨转化区中使空气与氨气反应产生一氧化氮; （b）将至少一部分一氧化氮氧化成二氧化氮以产生富含NO x的工艺气流; （c）在吸收区中用含磷酸溶液反应性吸收富含NO x的气流，形成硝酸根离子; （d）将硝酸根离子与脱气区的空气接触以产生富含硝酸盐的含水工艺物流; （e）在磷酸存在下用氢还原富硝酸盐的水流以产生磷酸羟铵; （f）用环己酮肟化磷酸羟铵，制得环己酮肟; 和（g）将环己酮肟转化为己内酰胺。 根据本发明，在氨转化区的下游添加补充氧以增加富含NOx的工艺气流中二氧化氮的形成量和速率。

公开(公告)号：US11208380B2

公开(公告)日：2021-12-28

申请号：US17000116

申请日：2020-08-21

Applicant: AquafilSLO d.o.o.

Inventor： Anacleto Dal Moro ,  Michele Cecchetto ,  Denis Jahic ,  Vid Margon

IPC: B01D3/10 ,  C07D201/16 ,  B01D3/14 ,  B01D11/04 ,  C07D201/06 ,  C07D223/10

Abstract: The present invention relates to a process for purifying caprolactam from solutions of crude caprolactam by a direct treatment with one or more alkaline compounds of polyvalent metals, preferably bivalent and trivalent, without resorting to organic solvent extraction as used in the usual purification process.
A further subject of the present invention is a facility devoid of a unit for organic solvent extraction and designed to carry out the caprolactam purification process described herein.

公开(公告)号：US10093622B2

公开(公告)日：2018-10-09

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

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：US08962826B2

公开(公告)日：2015-02-24

申请号：US14141916

申请日：2013-12-27

Applicant: Ube Industries, Ltd.

Inventor： Junichi Kugimoto ,  Joji Kawai ,  Kazuo Yamato ,  Masahide Okada ,  Tsunemi Sugimoto ,  Hiroshi Matsumoto

IPC: C07D225/02 ,  C07D201/04 ,  C07D201/06

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。

公开(公告)号：US20140114062A1

公开(公告)日：2014-04-24

申请号：US14141916

申请日：2013-12-27

Applicant: Ube Industries, Ltd.

Inventor： Junichi Kugimoto ,  Joji Kawai ,  Kazuo Yamato ,  Masahide Okada ,  Tsunemi Sugimoto ,  Hiroshi Matsumoto

IPC: C07D201/06 ,  C07D225/02

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。

公开(公告)号：US5599987A

公开(公告)日：1997-02-04

申请号：US414677

申请日：1995-03-31

Applicant: Guy L. Crocco ,  John C. Jubin, Jr. ,  John G. Zajacek

Inventor： Guy L. Crocco ,  John C. Jubin, Jr. ,  John G. Zajacek

IPC: C07C249/04 ,  C07D201/02 ,  C07D201/04 ,  C07D201/06

CPC classification number: C07C249/04 ,  Y02P20/125

Abstract: An integrated process for producing cyclohexanone oxime, a caprolactam precursor, is provided wherein isopropanol is utilized to generate the hydrogen peroxide oxidizing agent. The acetone produced as a co-product is recycled back to the secondary alcohol by hydrogenation. Ammoximation of cyclohexanone is performed in the presence of water and an alcohol other than isopropanol such as methanol or t-butyl alcohol.

Abstract translation: 提供了一种用于生产环己酮肟，己内酰胺前体的综合方法，其中使用异丙醇生成过氧化氢氧化剂。 作为副产物生产的丙酮通过氢化再循环回到仲醇中。 在水和除异丙醇之外的醇（如甲醇或叔丁醇）的存在下进行环己酮的接近。

公开(公告)号：US5451701A

公开(公告)日：1995-09-19

申请号：US266820

申请日：1994-06-27

Applicant: John G. Zajacek ,  John C. Jubin ,  Guy L. Crocco

Inventor： John G. Zajacek ,  John C. Jubin ,  Guy L. Crocco

IPC: C07C249/04 ,  C07C251/44 ,  C07D201/02 ,  C07D201/04 ,  C07D201/06

CPC classification number: C07C249/04 ,  C07C251/44 ,  Y02P20/125

Abstract: An integrated process for producing cyclohexanone oxime, a caprolactam precursor, is provided wherein a secondary alcohol is utilized to generate the hydrogen peroxide oxidizing agent and as a reaction medium for ammoximation. The ketone produced as a co-product is recycled back to the secondary alcohol by hydrogenation.

Abstract translation: 提供了一种用于生产环己酮肟，己内酰胺前体的综合方法，其中使用仲醇产生过氧化氢氧化剂和作为氨肟化反应的反应介质。 作为副产物生产的酮通过氢化再循环回到仲醇中。

公开(公告)号：US5264571A

公开(公告)日：1993-11-23

申请号：US954731

申请日：1992-09-30

Applicant: Hugo Fuchs ,  Gerald Neubauer ,  Josef Ritz

Inventor： Hugo Fuchs ,  Gerald Neubauer ,  Josef Ritz

IPC: C07D201/04 ,  C07D201/06 ,  C07D223/10 ,  C07D201/16

CPC classification number: C07D201/04 ,  C07D201/06

Abstract: A process for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime with oleum at from 85.degree. to 125.degree. C. in a plurality of rearrangement stages arranged in series entails returning a portion of the reaction mixture leaving the last rearrangement stage to at least one of the preceding rearrangement stages.

Abstract translation: 通过贝克曼重整环己酮肟与发烟硫酸在85℃至125℃下重排排列的多个重排阶段制备己内酰胺的方法需要将离开最后一个重排阶段的一部分反应混合物返回至 以前的重排阶段。

公开(公告)号：PL224406B1

公开(公告)日：2016-12-30

申请号：PL39823212

申请日：2012-02-24

Applicant: INST CHEMII PRZEMYSŁOWEJ IM PROF IGNACEGO MOŚCICKIEGO ,  ZAKŁADY AZOTOWE PUŁAWY SPÓŁKA AKCYJNA

Inventor： ZIMOWSKI ANDRZEJ ,  ZYLBERSZTEJN MICHAŁ ,  BAJDA HENRYK ,  WĘSEK ROBERT ,  KUMOR KAZIMIERZ ,  KANIA ANDRZEJ ,  PIŁAT PAWEŁ

IPC: C07D201/04 ,  B01D11/00 ,  C07D201/06

公开(公告)号：DE69907122D1

公开(公告)日：2003-05-28

申请号：DE69907122

申请日：1999-12-22

Applicant: PRAXAIR TECHNOLOGY INC

Inventor： ECHEGARAY DIEGO FERNANDEZ ,  VELLOSO ANTONIO AUGUSTO M ,  WAGNER MATTHEW LINCOLN

IPC: C07D201/06 ,  C07D201/10

Abstract: A method for production of caprolactam. The method involves: (a) reacting air with ammonia gas in an ammonia conversion zone to produce nitric oxide; (b) oxidizing at least a portion of the nitric oxide to nitrogen dioxide to produce an NOx-rich process gas stream; (c) reactively absorbing the NOx-rich gas stream with phosphoric acid containing solution in an absorption zone to form nitrate ions; (d) contacting the nitrate ions with air in a degassing zone to produce a nitrate-rich aqueous process stream; (e) reducing the nitrate-rich aqueous stream with hydrogen in the presence of phosphoric acid to produce hydroxylammonium phosphate; (f) oximating the hydroxylammonium phosphate with cyclohexanone to produce cyclohexanone oxime; and (g) converting the cyclohexanone oxime to caprolactam. According to the invention, supplemental oxygen is added downstream of the ammonia conversion zone to increase the quantity and rate of formation of nitrogen dioxide in the NOx-rich process gas stream.