公开(公告)号：US5245029A

公开(公告)日：1993-09-14

申请号：US792413

申请日：1991-11-15

Applicant: Yukio Inaba ,  Yasuhiro Kurokawa ,  Takafumi Hirakawa ,  Kanji Oyama

Inventor： Yukio Inaba ,  Yasuhiro Kurokawa ,  Takafumi Hirakawa ,  Kanji Oyama

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

CPC classification number: C07D201/16

Abstract: Disclosed is an ion exchange purification method of an aqueous caprolactam solution in a process for producing caprolactam and laurolactam by subjecting a mixture of cyclohexanone oxime and cyclododecanone oxime to Beckmann rearrangement in the presence of sulfuric acid and fuming sulfuric acid, which comprises, after neutralization of the rearrangement reaction products, and first extraction thereof with an organic solvent and second extraction of the first extract with water to obtain a second extract of an aqueous caprolactam solution, treating the aqueous caprolactam solution obtained by extraction with an organic solvent immiscible with water with a strongly acidic cation exchange resin, and subsequently with a weakly basic anion exchange resin or further with a strongly basic anion exchange resin.

Abstract translation: 公开了在硫酸和发烟硫酸的存在下，使环己酮肟和环十二烷酮肟的混合物进行贝克曼重排以制备己内酰胺和月桂内酰胺的方法中的己内酰胺水溶液的离子交换纯化方法， 重排反应产物，首先用有机溶剂萃取，用水萃取第二提取物，得到第二次己内酰胺水溶液，用与水不混溶的有机溶剂萃取得到的己内酰胺水溶液 强酸性阳离子交换树脂，随后用弱碱性阴离子交换树脂或强碱性阴离子交换树脂。

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。

公开(公告)号：US4968793A

公开(公告)日：1990-11-06

申请号：US468935

申请日：1990-01-23

Applicant: Masaru Kitamura ,  Hiroshi Ichihashi ,  Gohfu Suzukamo ,  Yasuo Nakamura

Inventor： Masaru Kitamura ,  Hiroshi Ichihashi ,  Gohfu Suzukamo ,  Yasuo Nakamura

IPC: C07D201/04

CPC classification number: C07D201/04

Abstract: .epsilon.-caprolactam is produced by gas phase reaction of cyclohexanone oxime using a solid acid as a catalyst in the presence of a compound represented by the formula (I): R.sub.1 --O--R.sub.2 (wherein R.sub.1 represents a lower alkyl group which may be substituted with a fluorine atom and R.sub.2 represents a hydrogen atom, a lower alkyl group or a phenyl group) such as a lower alcohol or an ether compound. The solid acid includes a crystalline metallosilicate or a crystalline silicate.

公开(公告)号：US4883915A

公开(公告)日：1989-11-28

申请号：US35868

申请日：1987-04-08

Applicant: Patrick E. McMahon

Inventor： Patrick E. McMahon

IPC: C07D201/04

CPC classification number: C07D201/04

Abstract: A process for the catalyzed conversion fo oximes such as cyclohexanone oxime to amides such as caprolactam via a high conversion, high selectivity, long catalyst lifetime reaction over a HAMS-1B crystalline borosilicate-based catalyst composition.

Abstract translation: 通过HAMS-1B结晶硼硅酸盐基催化剂组合物的高转化率，高选择性，长的催化剂寿命反应，催化转化如环己酮肟向酰胺如己内酰胺转化的方法。

公开(公告)号：US4806638A

公开(公告)日：1989-02-21

申请号：US109405

申请日：1987-10-19

Applicant: Uwe Brand ,  Ruediger Schmitz ,  Ernst Deuker ,  Hugo Fuchs

Inventor： Uwe Brand ,  Ruediger Schmitz ,  Ernst Deuker ,  Hugo Fuchs

IPC: C07D201/04 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: Reaction mixtures obtained by Beckmann rearrangement of cyclohexanone oxime with sulfuric acid or oleum are neutralized by a process which comprises the following steps:(a) mixing the reaction mixture with recycled ammonium sulfate mother liquor whose concentration is chosen so that no solid ammonium sulfate is precipitated during the neutralization,(b) neutralization by feeding gaseous ammonia which contains water or an aqueous ammonium sulfate solution in finely divided liquid form through a plurality of nozzle orifices into the solution of the reaction mixture in the ammonium sulfate mother liquor at elevated temperatures,(c) separation of crude lactam from the aqueous ammonium sulfate solution,(d) evaporation of the ammonium sulfate solution under reduced pressure and with separation of the crystalline ammonium sulfate from the ammonium sulfate mother liquor and(e) recycling of the ammonium sulfate mother liquor to stage a).

Abstract translation: 通过包含以下步骤的方法中和通过Beckmann重排环己酮肟与硫酸或发烟硫酸得到的反应混合物：（a）将反应混合物与其浓度选择为不使固体硫酸铵沉淀的再循环硫酸铵母液混合 在中和期间，（b）通过将高分子液体形式的含有水或硫酸铵水溶液的气态氨通过多个喷嘴孔送入反应混合物在硫酸铵母液的溶液中，在升高的温度下中和（b） c）将粗内酰胺与硫酸铵水溶液分离，（d）在减压下蒸发硫酸铵溶液，并从硫酸铵母液中分离结晶硫酸铵，和（e）将硫酸铵母液 到a）。

公开(公告)号：US4789741A

公开(公告)日：1988-12-06

申请号：US165234

申请日：1988-03-07

Applicant: Francesco Cellini ,  Vittorio Gervasutti ,  Raffaele Tancorra ,  Sergio Tonti

Inventor： Francesco Cellini ,  Vittorio Gervasutti ,  Raffaele Tancorra ,  Sergio Tonti

IPC: B01J19/26 ,  C07D201/04

CPC classification number: C07D201/04 ,  B01J19/26 ,  B01J2219/00119

Abstract: The invention concerns a two-step process for the synthesis of caprolactam by reaction of cylcohexanone-oxime with an excess of oleum, carried out in a first step with only a portion of the oxime and in the presence of liquid SO.sub.2, according to usual "cold" techniques, the amount of free SO.sub.3 in the oleum being equal to or greater than 50% by weight, wherein said "cold" step is completed by a second "hot" step, by adding a second portion of oxime, the ratio between said second portion and said first portion ranging from 0.5 to 1.2.

公开(公告)号：US4709024A

公开(公告)日：1987-11-24

申请号：US896008

申请日：1986-08-13

Applicant: Hiroshi Sato ,  Kenichi Hirose ,  Norio Ishii ,  Youichi Umada

Inventor： Hiroshi Sato ,  Kenichi Hirose ,  Norio Ishii ,  Youichi Umada

IPC: B01J25/00 ,  B01J29/035 ,  B01J29/40 ,  B01J29/70 ,  C07B61/00 ,  C07D201/04

CPC classification number: C07D201/04 ,  Y02P20/52

Abstract: .epsilon.-caprolactam is prepared by gas phase catalytic synthesis in which cyclohexanone oxime is brought into contact with crystalline alluminosilicate, for example, ZSM-5 H.sup.+ form) having 1-12 of constraint index, 500 or more, preferably 1000 or more, of Si/Al atomic ratio and 5.mu. equivalent/g or less, preferably 2.mu. equivalent/g, of external acid amount.

Abstract translation: ε-己内酰胺通过气相催化合成法制备，其中环己酮肟与具有1-12约束指数的结晶二硅铝酸盐例如ZSM-5 H +形式接触，其中500重量％以上，优选1000个以上的Si /原子比，5当量/ g以下，优选为2当量/ g的外部酸量。

公开(公告)号：US4472516A

公开(公告)日：1984-09-18

申请号：US467214

申请日：1983-02-17

Applicant: Petrus M. G. Frenken

Inventor： Petrus M. G. Frenken

IPC: C07D201/04 ,  B01J21/16 ,  B01J29/04 ,  B01J29/40 ,  B01J29/86 ,  B01J37/30 ,  C07B61/00 ,  C07C1/00 ,  C07C2/00 ,  C07C2/76 ,  C07C15/00 ,  C07C67/00 ,  C07D201/06 ,  B01J29/06 ,  B01J21/02

CPC classification number: C07D201/06 ,  B01J29/40 ,  B01J29/86 ,  B01J37/30 ,  C07C2/00 ,  C07C2529/06 ,  C07C2529/86

Abstract: Disclosed is a method for selectively deactivating catalytically active sites which occur only on the surface of a zeolite of boralite catalyst. Active sites occurring on the interior of the pores are masked by saturating the catalyst with an organic compound which fills substantially the whole of the catalyst pore volume. The catalyst so treated is then exposed to a deactivating agent, such as a solution of an alkali metal salt which is substantially immiscible with, substantially insoluble in, and which is otherwise unreactive to said pore-filling compound. The catalyst is then treated to drive off the pore-filling compound, yielding a catalyst selectively deactivated only on the external surface, but which is not deactivated within the pores. The treatment enables the catalyst to be used for e.g. hydrocarbon conversion for long time periods without carbon buildups around the pore entrances, which buildup would otherwise either restrict entry into the pores by reactants or exit therefrom by product.

Abstract translation: 公开了一种选择性地使仅发生在硼石催化剂的沸石表面上的催化活性位点的方法。 通过用充满基本上整个催化剂孔体积的有机化合物使催化剂饱和来掩盖在孔内部发生的活性位点。 然后将如此处理的催化剂暴露于钝化剂，例如碱性金属盐的溶液，其基本上不混溶，基本上不溶于，并且否则对所述孔填充化合物是不反应的。 然后处理催化剂以排出孔隙填充化合物，产生仅在外表面上选择性地失活的催化剂，但在孔内未失活。 该处理使得催化剂可以用于例如 碳氢化合物转化长时间没有在孔入口周围的碳积累，否则这些积聚将限制通过反应物进入孔或通过产物从其中排出。

公开(公告)号：US3991115A

公开(公告)日：1976-11-09

申请号：US633208

申请日：1975-11-19

Applicant: Richard Lynn Purgason

Inventor： Richard Lynn Purgason

IPC: C07D201/04 ,  C07D201/00 ,  C07C131/04

CPC classification number: C07C249/08

Abstract: This invention relates to a process for the production of cyclohexanone oxime by reacting cyclohexanone with excess aqueous hydroxylamine in the presence of excess ammonia. More specifically, the invention relates to improving yields of the oxime while reducing undesirable by-product formation by use of two or more stages of reaction with correlated adjustment of reaction conditions in each stage. The invention also involves improved recovery of the unreacted hydroxylamine reactant for recycle in the process.

Abstract translation: 本发明涉及通过在过量氨的存在下使环己酮与过量的羟胺反应生产环己酮肟的方法。 更具体地说，本发明涉及提高肟的产率，同时通过使用两阶段或更多阶段的反应，同时在每个阶段的反应条件的相关调整来减少不希望的副产物形成。 本发明还涉及在该方法中回收未反应的羟胺反应物以进行再循环。

公开(公告)号：US3835124A

公开(公告)日：1974-09-10

申请号：US32556373

申请日：1973-01-22

Applicant: SNIA VISCOSA

Inventor： GIUFFRE L ,  SIOLI G ,  MATTONE R

IPC: C07D201/02 ,  C07C67/00 ,  C07C201/00 ,  C07C207/00 ,  C07C239/00 ,  C07C251/46 ,  C07D201/04 ,  C07D201/10 ,  C07D205/08 ,  C07D207/263 ,  C07D223/02 ,  C07D41/06

CPC classification number: C07D201/10

Abstract: A method for the preparation of omega lactams is disclosed, more particularly epsilon caprolactam or a precursor thereof (such as cyclohexanone oxime), using as the starting material a cyclomethylene ketene, with the simultaneous formation of side products such as cyclohexanecarboxylic acid, wherein an adduct is preliminarly formed between cyclomethylene ketene and sulphur dioxide. The adduct is then reacted with a nitrosating agent so as to obtain, under the appropriate reaction conditions, the expected lactam, more specifically epsilon caprolactam.

Abstract translation: 公开了制备ω内酰胺的方法，更特别的是ε己内酰胺或其前体（例如环己酮肟），其以起始材料为环亚甲基乙烯酮，同时形成副产物如环己烷羧酸，其中加合物 在环亚甲基乙烯酮和二氧化硫之间初步形成。 然后将加合物与亚硝化剂反应，以在适当的反应条件下获得预期的内酰胺，更具体地是ε己内酰胺。