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1. 发明授权

US06489474B1 Process for producing amide compound 失效
标题翻译：酰胺化合物的制备方法
公开(公告)号：US06489474B1
公开(公告)日：2002-12-03
申请号：US09926816
申请日：2001-12-21
申请人： Yuuji Kawaragi , Tohru Setoyama
发明人： Yuuji Kawaragi , Tohru Setoyama
IPC分类号： C07D20104
CPC分类号： C07D201/04
摘要： Object of the present invention is to provide a process for producing an amide compound with high efficiency by subjecting an oxime compound to Beckmann rearrangement in a liquid phase under mild reaction conditions. Namely, the invention relates to a process for producing an amide compound such as &egr;-caprolactam by subjecting an oxime compound such as cyclohexanone oxime to Beckmann rearrangement in a liquid phase, characterized in that the reaction is carried out in the presence of (1) a non-fluorine-containing sulfonic anhydride and an N,N-disubstituted amide compound or (2) at least one compound selected from the group consisting of sulfonic acids and anhydrides thereof, an N,N-disubstituted amide compound, and a carboxylic anhydride.
摘要翻译：本发明的目的是提供一种通过在温和的反应条件下使肟化合物在液相中经受贝克曼重排而高效生产酰胺化合物的方法。即，本发明涉及通过使肟化合物如环己酮肟在液相中进行贝克曼重排来制备ε-己内酰胺的酰胺化合物的方法，其特征在于反应在（1）非含氟磺酸酐和N，N-二取代酰胺化合物或（2）至少一种选自磺酸及其酸酐，N，N-二取代酰胺化合物和羧酸酐的化合物。

2. 发明授权

US06245907B1 Process for producing a high purity caprolactam 有权
标题翻译：生产高纯度己内酰胺的方法
公开(公告)号：US06245907B1
公开(公告)日：2001-06-12
申请号：US09205900
申请日：1998-12-04
申请人： Myung Suk Suh , Seung Eon Park , Chang Hwang Lee , Myeong Hong Lee , Si Geun Lee , Jung Ho Kim
发明人： Myung Suk Suh , Seung Eon Park , Chang Hwang Lee , Myeong Hong Lee , Si Geun Lee , Jung Ho Kim
IPC分类号： C07D20104
CPC分类号： C07D201/04 , C07D223/10
摘要： Disclosed is a process for producing a high purity caprolactam which comprises converting cyclohexene obtained by the partial hydrogenation of benzene into cyclohexanol through hydration, converting the cyclohexanol into cyclohexanone through dehydrogenation, converting the cyclohexanone into cyclohexanone oxime through oximation and converting the cyclohexanone oxime into caprolactam through the Beckman rearrangement, characterized by comprising isolating and purifying the methylcyclopentanol from the cyclohexanol prior to use of such cyclohexanol in dehydrogenation and feeding the isolated methylcyclopentanol directly to oximation in order that the methylcyclopentanol is not fed to dehydrogenation. The process of the invention advantageously provides an economic method for producing a caprolactam with greater purity.
摘要翻译：公开了一种生产高纯度己内酰胺的方法，其包括将通过水合将苯部分氢化得到的环己烯转化为环己醇，通过脱氢将环己醇转化为环己酮，通过肟化将环己酮转化为环己酮肟，并将环己酮肟转化为己内酰胺，贝克曼重排，其特征在于包括在脱氢中使用这种环己醇之前从环己醇中分离和纯化甲基环戊醇，并将分离的甲基环戊醇直接进料到肟化中，以使甲基环戊醇不进行脱氢。本发明的方法有利地提供了一种制备更高纯度的己内酰胺的经济方法。

3. 发明授权

US06265574B1 Process for producing &egr;-caprolactam 有权
标题翻译：生产ε-己内酰胺的方法
公开(公告)号：US06265574B1
公开(公告)日：2001-07-24
申请号：US09500997
申请日：2000-02-09
申请人： Masaru Kitamura , Yasumoto Shimazu , Makoto Yako
发明人： Masaru Kitamura , Yasumoto Shimazu , Makoto Yako
IPC分类号： C07D20104
CPC分类号： B01J38/12 , B01J29/90 , C07D201/04 , Y02P20/52 , Y02P20/584 , Y02P20/588
摘要： A process for producing &egr;-caprolactam is provided which comprises the steps of subjecting cyclohexanone oxime to a gaseous phase Beckmann rearrangement reaction in a fluidized bed system using a solid catalyst and re-generating the catalyst, wherein said process comprises a step of treating the catalyst with an oxygen-containing gas at an elevated temperature in a re-generation step so that the nitrogen content of the catalyst falls within a range of 10 ppm to 2,500 ppm on its way to the reaction step from the re-generating step. According to the present invention, &egr;-caprolactam is produced with a high conversion or a high selectivity without interrupting the rearrangement reaction or the re-generation step.
摘要翻译：提供了一种生产ε-己内酰胺的方法，其包括以下步骤：使用固体催化剂在流化床系统中使环己酮肟进行气相贝克曼重排反应并重新产生催化剂，其中所述方法包括处理催化剂的步骤在再生步骤中在升高的温度下含有氧的气体，使得在从再生步骤到反应步骤的途中，催化剂的氮含量在10ppm至2,500ppm的范围内。根据本发明，在不中断重排反应或重生步骤的情况下，以高转化率或高选择性生产ε-己内酰胺。

4. 发明授权

US06750336B2 Method of production of lactam 失效
标题翻译：内酰胺的生产方法
公开(公告)号：US06750336B2
公开(公告)日：2004-06-15
申请号：US10285571
申请日：2002-11-01
申请人： Osamu Sato , Kiyotaka Hatakeda , Yutaka Ikushima , Kazuo Torii
发明人： Osamu Sato , Kiyotaka Hatakeda , Yutaka Ikushima , Kazuo Torii
IPC分类号： C07D20104
CPC分类号： C07D201/04 , Y02P20/582
摘要： A method for producing a lactam by using an organic solvent as a substrate solution, which makes it possible to introduce a high-concentration oxime into flowing high-temperature and high-pressure water, thereby allowing the high-concentration lactam to be synthesized with a high efficiency. With this method, the lactam is continuously synthesized at a high rate from the oxime under high-temperature and high-pressure water mixture conditions within a temperature range of no less than 250° C. and a pressure range of no less than 15 MPa.
摘要翻译：通过使用有机溶剂作为底物溶液制备内酰胺的方法，可以将高浓度肟引入流动的高温高压水中，从而使高浓度的内酰胺与高效率。通过该方法，在不低于250℃的温度范围和不低于15MPa的压力范围内，在高温和高压水混合条件下，从肟连续合成内酰胺。

5. 发明授权

US06469163B1 Method for production of hydroxylamine sulfate in the conventional process for the synthesis of caprolactam 有权
标题翻译：用于合成己内酰胺的常规方法生产硫酸羟胺的方法
公开(公告)号：US06469163B1
公开(公告)日：2002-10-22
申请号：US09221209
申请日：1998-12-24
申请人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
发明人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
IPC分类号： C07D20104
CPC分类号： C07D201/06 , C07D201/10
摘要： An improvement in the conventional process for the production of caprolactam. The process involves: (a) reacting air with ammonia gas in an ammonia conversion zone to produce nitric oxide; (b) oxidizing a portion of the nitric oxide to nitrogen dioxide to produce an NOx-rich process gas stream; (c) reacting the NOx-rich stream with ammonium carbonate in a nitriting zone to produce ammonium nitrite; (d) reducing the ammonium nitrite to hydroxylamine diammonium sulfate; (e) hydrolyzing the hydroxylamine diammonium sulfate to hydroxylamine sulfate; (f) oximating the hydroxylamine sulfate with cyclohexanone to produce cyclohexanone oxime; and (g) converting the cyclohexanone oxime to caprolactam. The process is improved by adding supplemental oxygen downstream of the ammonia conversion zone to increase the quantity and rate of formation of nitrogen dioxide in the NOx-rich process gas stream.
摘要翻译：制备己内酰胺的常规方法的改进。该方法包括：（a）在氨转化区中使空气与氨气反应以产生一氧化氮;（b）将一部分氧化氮氧化成二氧化氮以产生富含NO x的工艺气流;（c）使在氮化区中用碳酸铵生成富含NO x的物流以产生亚硝酸铵;（d）将亚硝酸铵还原为羟胺二硫酸铵;（e）将羟胺二硫酸铵水解成硫酸羟胺;（f）用环己酮将硫酸羟胺酸化生产环己酮肟; 并且（g）将环己酮肟转化为己内酰胺。通过在氨转化区下游加入补充氧以提高富氮过程气流中二氧化氮形成的数量和速率，从而提高了工艺。

6. 发明授权

US06258949B1 Apparatus and process for producing &egr;-caprolactam 失效
标题翻译：用于生产ε-己内酰胺的装置和方法
公开(公告)号：US06258949B1
公开(公告)日：2001-07-10
申请号：US09526885
申请日：2000-03-16
申请人： Masaru Kitamura , Yasumoto Shimazu
发明人： Masaru Kitamura , Yasumoto Shimazu
IPC分类号： C07D20104
CPC分类号： B01J8/02 , B01J8/24 , B01J2208/00106 , C07D201/04 , Y02P20/52
摘要： An apparatus for the production of &egr;-caprolactam is provided which comprises (i) a fluidized bed reactor having a solid catalyst therein for subjecting cyclohexanone oxime to a rearrangement reaction to obtain a reaction product containing unreacted cyclohexanone oxime and (ii) a fixed bed reactor packed with a solid catalyst for subjecting the unreacted cyclohexanone oxime to a rearrangement reaction to obtain &egr;-caprolactam. Using the apparatus, &egr;-caprolactam is obtained with a high yield.
摘要翻译：提供了一种用于生产ε-己内酰胺的装置，其包括（i）其中具有固体催化剂的流化床反应器，用于使环己酮肟进行重排反应以获得含有未反应的环己酮肟的反应产物和（ⅱ）固定床反应器填充固体催化剂，使未反应的环己酮肟进行重排反应，得到ε-己内酰胺。使用该装置，以高产率获得ε-己内酰胺。

7. 发明授权

US06531595B2 Method for producing &egr;-caprolactam and reactor for the method 失效
标题翻译：用于该方法生产ε-己内酰胺和反应器的方法
公开(公告)号：US06531595B2
公开(公告)日：2003-03-11
申请号：US09963603
申请日：2001-09-27
申请人： Wolfgang F. Hölderich , Gerd Dahlhoff , Hiroshi Ichihashi , Keisuke Sugita
发明人： Wolfgang F. Hölderich , Gerd Dahlhoff , Hiroshi Ichihashi , Keisuke Sugita
IPC分类号： C07D20104
CPC分类号： C07D201/04
摘要： A method is provided for producing &egr;-caprolactam from cyclohexanone oxime by using a zeolite or non-zeolitic material as a catalyst under gas phase reaction conditions. The method comprises a reaction step converting cyclohexanone oxime into &egr;-caprolactam in the presence of the zeolite or non-zeolitic material; and a regeneration step of treating the zeolite or non-zeolitic material with a non-oxidizing gas at a temperature of from about 100°C. to about 600° C.
摘要翻译：提供了一种通过在气相反应条件下使用沸石或非沸石材料作为催化剂从环己酮肟生产ε-己内酰胺的方法。该方法包括在沸石或非沸石材料存在下将环己酮肟转化成ε-己内酰胺的反应步骤; 以及在约100℃的温度下用非氧化性气体处理沸石或非沸石材料的再生步骤。至约600℃

8. 发明授权

US06482945B2 Process for producing epsilon-caprolactam and apparatus for the process 失效
标题翻译：用于生产ε-己内酰胺的方法和该方法的装置
公开(公告)号：US06482945B2
公开(公告)日：2002-11-19
申请号：US09964424
申请日：2001-09-28
申请人： Wolfgang F. Hölderich , Gerd Dahlhoff , Andre Sbresny , Hiroshi Ichihashi
发明人： Wolfgang F. Hölderich , Gerd Dahlhoff , Andre Sbresny , Hiroshi Ichihashi
IPC分类号： C07D20104
CPC分类号： C07D201/06 , C07D201/04
摘要： A process is provided for producing &egr;-caprolactam from cyclohexanone oxime. The process comprises a evaporation step of a mixture of cyclohexanone oxime and a solvent by introducing the mixture into a fluidized bed in which inert particles is fluidized by an inert gas, the particles having heat enough to evaporate the mixture; and a rearrangement step of cyclohexanone oxime in the evaporated mixture into &egr;-caprolactam by a gas phase Beckmann rearrangement reaction using a solid catalyst, excluding a catalyst consisting of a boric acid or a boron oxide.
摘要翻译：提供了从环己酮肟生产ε-己内酰胺的方法。该方法包括通过将混合物引入流化床中的环己酮肟和溶剂的混合物的蒸发步骤，其中惰性颗粒通过惰性气体流化，该颗粒具有足以蒸发混合物的热量; 和通过使用固体催化剂的气相贝克曼重排反应将蒸发的混合物中的环己酮肟重排成ε-己内酰胺，不包括由硼酸或氧化硼组成的催化剂。

9. 发明授权

US06333411B1 Method for production of hydroxylammonium phosphate in the synthesis of caprolactam 失效
标题翻译：己内酰胺合成中磷酸羟铵的生产方法
公开(公告)号：US06333411B1
公开(公告)日：2001-12-25
申请号：US09221211
申请日：1998-12-24
申请人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
发明人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
IPC分类号： C07D20104
CPC分类号： C07D201/06 , C07D201/10
摘要： 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.
摘要翻译：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以产生一氧化氮;（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）使硝酸根离子与脱气区的空气接触，产生富含硝酸盐的含水工艺流;（e）富含硝酸盐的含水流在磷酸存在下用氢气生成磷酸羟铵;（f）用环己酮肟化磷酸羟铵以制备环己酮肟; 并且（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氮过程气流中二氧化氮的形成量和速率。

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