公开(公告)号：US20040097726A1

公开(公告)日：2004-05-20

申请号：US10469533

申请日：2003-09-08

Inventor： Kiyotaka Hatakeda ,  Osamu Sato ,  Yutaka Ikushima ,  Kazuo Torii

IPC: C07D223/10

CPC classification number: C07D201/06 ,  C07D201/04 ,  C07D223/10

Abstract: It is an object of the present invention to provide a method of continuously producing a lactam in high-temperature high-pressure water, and the present invention relates to a method for producing a lactam characterized by selectively synthesizing the lactam without bringing about hydrolysis by introducing an oxime into flowing high-temperature high-pressure water, wherein the lactam is continuously synthesized at a high rate from the oxime in water at a high temperature of at least 250null C. and a high pressure of at least 12 MPa.

Abstract translation: 本发明的目的是提供一种在高温高压水中连续生产内酰胺的方法，本发明涉及一种制备内酰胺的方法，其特征在于，通过引入不引起水解而选择性合成内酰胺 将肟流入高温高压水中，其中在至少250℃的高温和至少12MPa的高压下，从肟在水中以高速连续合成内酰胺。

公开(公告)号：US20040054169A1

公开(公告)日：2004-03-18

申请号：US10466888

申请日：2003-07-22

Inventor： Takashi Tsunoda ,  Kenji Akagishi ,  Mitsuhiro Sekiguchi

IPC: C07D201/04

CPC classification number: C07D201/04 ,  B01J21/16 ,  B01J29/035 ,  B01J29/40 ,  Y02P20/52 ,  Y02P20/584

Abstract: In the production of null-caprolactam by contacting cyclohexanone oxime with a solid acid catalyst in the gaseous phase to effect a rearrangement reaction of the cyclohexanone oxime, wherein the solid acid catalyst is produced by calcining a dried catalyst precursor: in a first aspect, the catalyst precursor comprises a zeolite, a crystalline clay mineral and at least one substance selected from the group consisting of an inorganic oxide and a compound which forms the inorganic oxide by calcination, wherein the inorganic oxide comprises an oxide of at least one element selected from the group consisting of elements belonging to Groups 4, 13 and 14 of the Periodic Table and wherein the inorganic oxide is other than oxides contained in a crystalline form in the zeolite and the crystalline clay mineral; or in a second aspect, the rearrangement reaction is effected in the presence of a polyhydric alcohol derivative represented by the following formula: R1nullOnullR2nullOH (wherein: R1 represents a C1-C5 alkyl group or a phenyl group, and R2 represents a C2-C5 alkylene group).

Abstract translation: 在ε-己内酰胺的制备中，使环己酮肟与气相中的固体酸催化剂接触，进行环己酮肟的重排反应，其中固体酸催化剂是通过煅烧干燥的催化剂前体制备的：在第一方面， 催化剂前体包括沸石，结晶粘土矿物和选自无机氧化物和通过煅烧形成无机氧化物的化合物中的至少一种物质，其中无机氧化物包含选自以下的至少一种元素的氧化物： 由元素周期表第4,13和14族元素组成的组，其中无机氧化物不同于在沸石和结晶粘土矿物中结晶形式的氧化物; 或者在第二方面，重排反应在下式表示的多元醇衍生物的存在下进行：R 1 -OR 2 -OH（其中：R 1表示C 1 -C 5烷基 或苯基，R 2表示C 2 -C 5亚烷基）。

公开(公告)号：US06703501B1

公开(公告)日：2004-03-09

申请号：US10088785

申请日：2002-06-11

Applicant: Myunghun Kim ,  Sunjin Kim ,  Youngsun Uh ,  Younghee Kim

Inventor： Myunghun Kim ,  Sunjin Kim ,  Youngsun Uh ,  Younghee Kim

IPC: B01J2320

CPC classification number: B01J29/049 ,  C07D201/04 ,  Y02P20/52

Abstract: The present invention relates to porous catalysts comprising layered silicate and metal oxides, and a method of preparing &egr;-caprolactam from cyclohexanone oxime using the catalyst. This new catalyst can resolve the environmental and safety problems arising from conventional liquid acid process. Also the present catalyst solves the problem of short lifetime of current solid acid catalysts. Moreover, the present catalyst provides higher selectivity and yield.

Abstract translation: 本发明涉及包含层状硅酸盐和金属氧化物的多孔催化剂，以及使用该催化剂由环己酮肟制备ε-己内酰胺的方法。 这种新的催化剂可以解决常规液体酸处理中产生的环境和安全问题。 本催化剂还解决了目前固体酸催化剂寿命短的问题。 此外，本催化剂提供更高的选择性和产率。

公开(公告)号：US20030139596A1

公开(公告)日：2003-07-24

申请号：US10345548

申请日：2003-01-16

Applicant: UBE INDUSTRIES, LTD.

Inventor： Nobuyuki Kuroda ,  Joji Kawai ,  Hideo Shimomura

IPC: C07D225/02

CPC classification number: C07D201/06 ,  C07D201/04

Abstract: Laurolactam having high quality is produced by reacting cyclododecanone with a hydroxylamine salt of a mineral acid, and converting the resultant cyclododecanoneoxime to laurolactam through the Beckmann rearrangement reaction, wherein a content of each of oxygen atom-containing C12 organic compounds, for example, cyclododecenone or epoxycyclododecane, and cycloaliphatic unsaturated C12 hydrocarbon compounds, contained, as an impurity, in the staring cyclododecanone material, is controlled to 1,000 ppm or less.

公开(公告)号：US20030088093A1

公开(公告)日：2003-05-08

申请号：US10285571

申请日：2002-11-01

Applicant: National Inst. of Advanced Ind. Science and Tech.

Inventor： Osamu Sato ,  Kiyotaka Hatakeda ,  Yutaka Ikushima ,  Kazuo Torii

IPC: C07D201/04 ,  C07D211/36

CPC classification number: C07D201/04 ,  Y02P20/582

Abstract: 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 250null C. and a pressure range of no less than 15 MPa.

Abstract translation: 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。

公开(公告)号：US20020042509A1

公开(公告)日：2002-04-11

申请号：US09963603

申请日：2001-09-27

Inventor： Wolfgang F. Holderich ,  Gerd Dahlhoff ,  Hiroshi Ichihashi ,  Keisuke Sugita

IPC: C07D223/10

CPC classification number: C07D201/04

Abstract: A method is provided for producing null-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 null-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 100null C. to about 600null C.

Abstract translation: 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℃至约600℃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。

公开(公告)号：US06344557B1

公开(公告)日：2002-02-05

申请号：US09674164

申请日：2000-10-27

Applicant: Masami Fukao ,  Kan Takamine ,  Tomokazu Nakamura

Inventor： Masami Fukao ,  Kan Takamine ,  Tomokazu Nakamura

IPC: C07D20116

CPC classification number: C07D201/04

Abstract: The present invention provides a method for producing &egr;-caprolactam which comprises the step of treating, with water, a reaction product containing 1-aza-2-alkoxy-1-cycloheptene, which is obtained by gas phase Beckmann rearrangement reaction of cyclohexanone oxime using a solid catalyst in the presence of alcohol, to eliminate the 1-aza-2-alkoxy-1-cycloheptene. The resulting &egr;-caprolactam usually has a 1-aza-2-alkoxy-1-cycloheptene content of 100 ppm or less, preferably 25 ppm or less, more preferably 10 ppm or less and, therefore, has low free basicity and good qualities.

Abstract translation: 本发明提供一种ε-己内酰胺的制造方法，其包括用水处理含有1-氮杂-2-烷氧基-1-环庚烯的反应产物的步骤，该反应产物是通过环己酮肟的气相贝克曼重排反应得到的，使用 在醇存在下的固体催化剂，以除去1-氮杂-2-烷氧基-1-环庚烯。 所得的ε-己内酰胺通常具有100ppm以下的1-氮杂-2-烷氧基-1-环庚烯含量，优选为25ppm以下，更优选为10ppm以下，因此具有低的游离碱度和良好的品质。

公开(公告)号：US06265574B1

公开(公告)日：2001-07-24

申请号：US09500997

申请日：2000-02-09

Applicant: Masaru Kitamura ,  Yasumoto Shimazu ,  Makoto Yako

Inventor： Masaru Kitamura ,  Yasumoto Shimazu ,  Makoto Yako

IPC: C07D20104

CPC classification number: B01J38/12 ,  B01J29/90 ,  C07D201/04 ,  Y02P20/52 ,  Y02P20/584 ,  Y02P20/588

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US5354859A

公开(公告)日：1994-10-11

申请号：US981476

申请日：1992-11-25

Applicant: Hiroshi Ichihashi ,  Masaru Kitamura ,  Hiroshi Kajikuri ,  Eiji Tasaka

Inventor： Hiroshi Ichihashi ,  Masaru Kitamura ,  Hiroshi Kajikuri ,  Eiji Tasaka

IPC: B01J29/06 ,  C07D201/04

CPC classification number: B01J29/06 ,  C07D201/04 ,  Y02P20/52

Abstract: .epsilon.-Caprolactam is prepared by bringing cyclohexanone oxime into contact in gas phase with solid catalysts such as a zeolite catalyst in the presence of at least one nitrogen-containing compound selected from the group consisting of ammonia, methylamines and .epsilon.-caprolactam.

Abstract translation: 在选自氨，甲胺和ε-己内酰胺的至少一种含氮化合物的存在下，使环己酮肟与气相与固体催化剂如沸石催化剂接触来制备ε-己内酰胺。

公开(公告)号：US5242676A

公开(公告)日：1993-09-07

申请号：US881282

申请日：1992-05-11

Applicant: Minas R. Apelian ,  Anthony S. Fung

Inventor： Minas R. Apelian ,  Anthony S. Fung

IPC: B01J29/40 ,  B01J29/65 ,  B01J29/70 ,  C07D201/04

CPC classification number: B01J29/7034 ,  B01J29/40 ,  B01J29/65 ,  B01J29/70 ,  B01J29/7038 ,  B01J29/7046 ,  C07D201/04 ,  B01J2229/123 ,  B01J2229/16 ,  B01J2229/37 ,  Y10S423/22 ,  Y10S423/23 ,  Y10S423/29 ,  Y10S423/30 ,  Y10S423/35 ,  Y10S423/36

Abstract: A process for the selective surface dealumination of a zeolite having a Constraint Index greater than 1 by contacting the zeolite with dicarboxylic acid, such as oxalic acid.

Abstract translation: 通过使沸石与二羧酸如草酸接触来选择性表面脱铝约束指数大于1的沸石的方法。