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1. 发明授权

US11459302B2 Refining process and refining system of caprolactam 有权
公开(公告)号：US11459302B2
公开(公告)日：2022-10-04
申请号：US17208073
申请日：2021-03-22
申请人： ZHEJIANG HENGYI PETROCHEMICAL RESEARCH INSTITUTE CO., LTD.
发明人： Shibiao Cheng , Songlin Wang , Fei Shen , Han Wang , Xi Li , Xinping Zhang , Dejia Ma , Xiaokang Hu , Zong Li , Yixuan He
IPC分类号： C07D201/06 , C07D201/16 , C07D223/10
摘要： A refining process includes steps of subjecting crude caprolactam to a first evaporative crystallization and a first solid-liquid separation to obtain a first caprolactam crystal and a first crystallization mother liquor; washing the first caprolactam crystal to obtain a second caprolactam crystal; optionally concentrating the first crystallization mother liquor to perform a second evaporative crystallization and a second solid-liquid separation to obtain a third caprolactam crystal and a second crystallization mother liquor; subjecting the third caprolactam crystal to a second washing to obtain a fourth caprolactam; optionally concentrating the second crystallization mother liquor to perform thermostatic crystallization, performing separation to obtain a fifth caprolactam crystal and a third crystallization mother liquor; washing the fifth caprolactam crystal to obtain a sixth caprolactam crystal; and subjecting the second caprolactam crystal to a hydrogenation reaction.

2. 发明授权

US10787417B2 Process for the purification of caprolactam from a solution of crude caprolactam without organic solvent extraction 有权
公开(公告)号：US10787417B2
公开(公告)日：2020-09-29
申请号：US16488016
申请日：2017-12-15
申请人： AquafilSLO d.o.o.
发明人： Anacleto Dal Moro , Michele Cecchetto , Denis Jahic , Vid Margon
IPC分类号： C07D201/16 , B01D3/10 , B01D3/14 , B01D11/04 , C07D201/06 , C07D223/10
摘要： 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.

3. 发明授权

US09624176B2 Method for preparing caprolactam by using a microreactor under lewis acid catalysis 有权
公开(公告)号：US09624176B2
公开(公告)日：2017-04-18
申请号：US15192869
申请日：2016-06-24
申请人： NANJING TECH UNIVERSITY (CN)
发明人： Kai Guo , Xin Li , Zheng Fang , Kai Zhang , Qi Yu , Pingkai Ouyang
IPC分类号： C07D201/04 , C07D201/06 , C07D223/10
CPC分类号： C07D223/10 , Y02P20/52
摘要： A method for preparing caprolactam by using a microreactor under Lewis acid catalysis, wherein a hydroxyl group in a cyclohexanone oxime is activated to obtain a cyclohexanone oxime sulfonates intermediate, then rearranged under Lewis acid catalysis to prepare the caprolactam. The method of this invention has a simple process and a high operation safety and selectivity, the reaction condition is mild, an efficient reaction can take place even at room temperature, the reaction time is short, the conversion of the cyclohexanone oxime can reach 100% within a short time, the selectivity of the caprolactam can reach 99%, the energy consumption is greatly reduced in the premise of maintaining a high yield, and the production cost is reduced, being an efficient and green and environmentally friendly method of for synthesizing the caprolactam.

4. 发明授权

US3335183A Preparation of oximes 失效
公开(公告)号：US3335183A
公开(公告)日：1967-08-08
申请号：US42181564
申请日：1964-12-29
申请人： STAMICARBON
发明人： DE ROOIJ ABRAHAM H
IPC分类号： C07D201/06
CPC分类号： C07D201/06

5. 发明授权

US09242931B2 Method for producing amide compound 有权
标题翻译：酰胺化合物的制备方法
公开(公告)号：US09242931B2
公开(公告)日：2016-01-26
申请号：US14141867
申请日：2013-12-27
申请人： Ube Industries, Ltd.
发明人： Junichi Kugimoto , Joji Kawai
IPC分类号： C07D201/04 , C07D201/06 , C07D225/02
CPC分类号： C07D201/06 , C07D201/04 , C07D225/02
摘要： 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.
摘要翻译：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。

6. 发明授权

US5525725A Process for producing a high purity caprolactam 失效
公开(公告)号：US5525725A
公开(公告)日：1996-06-11
申请号：US293180
申请日：1994-08-19
申请人： Yasuhiko Higashio , Hiroshi Kajikuri , Keisuke Sugita , Hideki Doi , Masanobu Matsubara
发明人： Yasuhiko Higashio , Hiroshi Kajikuri , Keisuke Sugita , Hideki Doi , Masanobu Matsubara
IPC分类号： C07D201/16 , C07D201/04 , C07D201/06
CPC分类号： C07D201/16
摘要： A process for producing a high purity caprolactam is disclosed in which a crude caprolactam obtained by a catalytic rearrangement of cyclohexanone oxime is subjected(1) to mixing, while stirring, with at least one hydrocarbon selected from the group consisting of aliphatic hydrocarbons and alicyclic hydrocarbons to form a liquid-liquid, two-layer liquid mixture, and then crystallizing caprolactam out of the liquid mixture;(2) to mixing with both at least one hydrocarbon selected from the group consisting of aliphatic hydrocarbons and alicyclic hydrocarbons, and water to form a liquid mixture, separating the liquid mixture into a hydrocarbon layer and a water layer, and then recovering caprolactam from the water layer; or(3) to distillation in the co-presence of at least one aliphatic saturated hydrocarbon of 10 to 18 carbon atoms.

7. 发明授权

US4472516A Process for deactivating catalytically active sites on the external surface of crystalline silicate catalysts, as well as crystalline silicate catalysts the catalytic properties of the external surface of which differ from those of the pore surface 失效
标题翻译：结晶硅酸盐催化剂外表面催化活性位点失活的方法以及结晶硅酸盐催化剂，其外表面的催化性能与孔表面的催化性质不同
公开(公告)号：US4472516A
公开(公告)日：1984-09-18
申请号：US467214
申请日：1983-02-17
申请人： Petrus M. G. Frenken
发明人： Petrus M. G. Frenken
IPC分类号： 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分类号： C07D201/06 , B01J29/40 , B01J29/86 , B01J37/30 , C07C2/00 , C07C2529/06 , C07C2529/86
摘要： 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.
摘要翻译：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。

8. 发明授权

US2754298A Production of lactams and amides 失效
标题翻译：生产内酰胺和酰胺
公开(公告)号：US2754298A
公开(公告)日：1956-07-10
申请号：US37504653
申请日：1953-08-18
申请人： BRITISH CELANESE
发明人： CYRIL BARNETT , JAMES LINCOLN
IPC分类号： C07D201/06
CPC分类号： C07D201/06

9. 发明授权

US11884632B2 Preparation method of caprolactam 有权
公开(公告)号：US11884632B2
公开(公告)日：2024-01-30
申请号：US17212530
申请日：2021-03-25
申请人： ZHEJIANG HENGYI PETROCHEMICAL RESEARCH INSTITUTE CO., LTD.
发明人： Shibiao Cheng , Songlin Wang , Xi Li , Han Wang , Fei Shen , Xinping Zhang , Zhaobin Jiang , Zhimin Hu
IPC分类号： C07D223/10 , C07D201/06 , C07D201/16 , B01J29/70 , B01J35/08 , B01J37/00 , B01J37/04 , B01J37/08
CPC分类号： C07D223/10 , B01J29/70 , B01J35/08 , B01J37/0036 , B01J37/04 , B01J37/08
摘要： 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.

10. 发明申请

US20180093949A1 AN EFFICIENT PROCESS FOR THE SYNTHESIS OF CYCLIC AMIDES 审中-公开
公开(公告)号：US20180093949A1
公开(公告)日：2018-04-05
申请号：US15562518
申请日：2015-06-04
申请人： ANTHEA AROMATICS PRIVATE LIMITED
发明人： Manoj Kumar MOHAPATRA , Ramamohanrao BENDAPUDI , Paul Vincent MENACHERRY , Vincent PAUL
IPC分类号： C07D201/06 , C07D201/16 , C07D227/087 , C01G9/02 , C01B21/14
CPC分类号： C07D201/06 , B01D3/36 , C01B21/14 , C01G9/02 , C07D201/04 , C07D201/16 , C07D227/087
摘要： 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.

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