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公开(公告)号：US06392037B1
公开(公告)日：2002-05-21
申请号：US09925730
申请日：2001-08-10
IPC分类号： C07D20108
CPC分类号： C07D201/08
摘要： Process for the preparation of &egr;-caprolactam comprising treating 6-aminocaproic acid 6-aminocaproate ester, 6-aminocaproamide, oligomers or polymers of these compounds or mixtures comprising at least two of these compounds in a cyclisation reactor in the presence of superheated steam in which a gaseous product stream comprising &egr;-caprolactam, lights and heavies is obtained, wherein the product stream, after condensation and at least partial removal of water and lights, is split into a &egr;-caprolactam stream and a heavies stream containing heavies and &egr;-caprolactam and the heavies stream is recycled to a cyclisation reactor.
摘要翻译： 制备ε-己内酰胺的方法，包括在过热蒸汽存在下，在环化反应器中处理6-氨基己酸6-氨基己酸酯，6-氨基己酰胺，这些化合物的低聚物或包含至少两种这些化合物的混合物或其混合物，其中 得到包含ε-己内酰胺，光和重质物的气态产物流，其中在冷凝和至少部分除去水和光之后，产物流被分裂成ε-己内酰胺流和含有重质和ε-己内酰胺的重质流 并将重质物流再循环至环化反应器。
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公开(公告)号：US06323341B1
公开(公告)日：2001-11-27
申请号：US09665592
申请日：2000-09-19
IPC分类号： C07D20116
CPC分类号： C07D201/08 , C07D201/16
摘要： The invention relates to a process for the purification of crude &egr;-caprolactam, wherein crude &egr;-caprolactam prepared by cyclization of alkyl 6-aminocaproate, 6-aminocapronitrile, 6-aminocaproic acid, 6-aminocaproic amide and/or oligomers thereof, is subjected to a crystallization process.
摘要翻译： 本发明涉及纯化ε-己内酰胺的方法，其中将通过6-氨基己酸烷基酯，6-氨基己腈，6-氨基己酸，6-氨基己酰胺和/或其低聚物的环化制备的粗ε-己内酰胺进行 结晶过程。
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公开(公告)号：US06660857B2
公开(公告)日：2003-12-09
申请号：US10210878
申请日：2002-08-02
IPC分类号： C07D20108
CPC分类号： C07D201/12 , C07D201/08
摘要： A process for the preparation of &egr;-caprolactam starting from 6-aminocaproic acid, 6-aminocaproamide, 6-aminocaproic ester, 6-aminocapronitrile, oligomers or polymers of these compounds or mixtures comprising at least two of these compounds, which process is performed in the presence of N-(5-carboxypentyl)-&egr;-caprolactam and/or derivative thereof in an amount of less than 50 wt. % and more than 0.1 wt. % (based on the total reaction mixture).
摘要翻译： 从6-氨基己酸，6-氨基己酰胺，6-氨基己酸酯，6-氨基己腈，这些化合物的低聚物或聚合物或包含这些化合物中的至少两种的混合物制备ε-己内酰胺的方法，该方法在 N-（5-羧基戊基） - 己内酰胺和/或其衍生物的存在量小于50wt。 ％和大于0.1wt。 ％（基于总反应混合物）。
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公开(公告)号：US06194572B1
公开(公告)日：2001-02-27
申请号：US09376310
申请日：1999-08-18
IPC分类号： C07D20108
CPC分类号： C07D201/08
摘要： Process to prepare &egr;-caprolactam by treating 6-aminocaproic acid, 6-aminocaproate ester or 6-aminocaproamide or mixtures comprising at least two of these compounds in the presence of superheated steam in which a gaseous mixture comprising &egr;-caprolactam and steam is obtained, wherein the process is carried out in the absence of a catalyst at a temperature between 250 and 400° C. and at a pressure of between 0.5 and 2 MPa. The invention also encompasses a process to prepare &egr;-caprolactam starting from 6-aminocapronitrile by performing a hydrolysis and a subsequent step as described above.
摘要翻译： 在过热蒸汽的存在下，通过在其中得到包含ε-己内酰胺和蒸汽的气体混合物的情况下，通过处理6-氨基己酸，6-氨基己酸酯或6-氨基己酰胺或包含这些化合物中至少两种的混合物来制备ε-己内酰胺的方法， 其中所述方法在不存在催化剂的情况下在250-400℃和0.5-2MPa的压力下进行。 本发明还包括通过进行如上所述的水解和随后的步骤从6-氨基己腈开始制备ε-己内酰胺的方法。
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公开(公告)号：US06191274B1
公开(公告)日：2001-02-20
申请号：US09134756
申请日：1998-08-17
IPC分类号： C07D20116
CPC分类号： C07D201/08 , C07D201/16
摘要： Process to separate &egr;-caprolactam from an aqueous mixture containing &egr;-caprolactam and at least 0.5 wt % oligomers, wherein the separation is performed by extraction using an organic extraction agent. The aqueous mixture may be obtained in a process to prepare &egr;-caprolactam starting from 6-aminocapronitrile or in a process to prepare &egr;-caprolactam starting from 6-aminocaproic acid.
摘要翻译： 从含有ε-己内酰胺和至少0.5wt％低聚物的含水混合物中分离ε-己内酰胺的方法，其中通过使用有机萃取剂萃取进行分离。 含水混合物可以在从6-氨基己腈开始制备ε-己内酰胺或从6-氨基己酸开始制备ε-己内酰胺的方法中获得。
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公开(公告)号：US06333412B1
公开(公告)日：2001-12-25
申请号：US09635717
申请日：2000-08-09
申请人： Rudolf P. M. Guit , Samuel L. Lane
发明人： Rudolf P. M. Guit , Samuel L. Lane
IPC分类号： C07D20108
CPC分类号： C07D201/08
摘要： Process to prepare &egr;-caprolactam starting from a starting mixture containing a 6-aminocaproate ester, in which in a first step (1) the 6-aminocaproate ester is converted into 6-aminocaproic acid and 6-aminocaproamide by reaction with water in the presence of ammonia at a temperature of between 50 and 250° C., with a separate or simultaneous removal of alcohol(s), and in a subsequent step (2) the 6-aminocaproic acid and 6-aminocaproamide are cyclizised at an elevated temperature, wherein in step (1) the 6-aminocaproate ester is converted into 6-aminocaproic acid and 6-aminocaproamide in the presence of an amount higher than 2 wt. % and less than or equal to 25 wt. % NH3 (relative to the total amount of organic compounds, water and ammonia present in step (1)).
摘要翻译： 从含有6-氨基己酸酯的起始混合物制备ε-己内酰胺的方法，其中在第一步（1）中，6-氨基己酸酯在存在下与水反应转化为6-氨基己酸和6-氨基己酰胺 在50至250℃的温度下，分离或同时除去醇，并且在随后的步骤（2）中，6-氨基己酸和6-氨基己酰胺在升高的温度下环化， 其中在步骤（1）中，将6-氨基己酸酯在高于2重量％的量存在下转化成6-氨基己酸和6-氨基己酰胺。 ％且小于或等于25wt。 ％NH 3（相对于步骤（1）中存在的有机化合物，水和氨的总量）。
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公开(公告)号：US06268530B1
公开(公告)日：2001-07-31
申请号：US09030281
申请日：1998-01-05
IPC分类号： C07C59147
CPC分类号： C07D221/08 , C07C51/48 , C07C59/147
摘要： Process to separate linear 5-formylvaleric acid from a mixture of 5- and 3- and 4-formylvaleric acids, wherein the separation is performed by fractional extraction with two immiscible solvents of which one solvent is an aqueous solvent and the other solvent is an organic solvent, in which the organic solvent has a higher or lower affinity for 5-formylvaleric acid than its affinity for the 3-formylvaleric acids and for the 4-formylvaleric acid. Furthermore the invention relates to an improved process to prepare ∈-caprolactam starting from a mixture of branched and linear formylvaleric acids or starting from pentenoic acid.
摘要翻译： 从5-和3-甲酰基戊酸的混合物中分离线性5-甲酰戊酸的方法，其中分离通过两种不混溶的溶剂进行分离，其中一种溶剂是一种溶剂，另一种溶剂是有机溶剂 溶剂，其中有机溶剂对5-甲酰基戊酸的亲和力高于或低于其对3-甲酰基戊酸和4-甲酰基戊酸的亲和力。 此外，本发明涉及从支链和直链甲酰基戊酸的混合物开始或从戊烯酸开始制备ε-己内酰胺的改进方法。
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公开(公告)号：US06353100B1
公开(公告)日：2002-03-05
申请号：US09260143
申请日：1999-03-01
申请人： Rudolf P. M. Guit , Wim Buijs
发明人： Rudolf P. M. Guit , Wim Buijs
IPC分类号： C07D20100
CPC分类号： C07D201/08
摘要： Process for the preparation of &egr;-caprolactam, in which in a step (a) a compound with the general formula: O=CH—(CH2)4—C(O)—R (1) in which R is —OH, —NH2 or O—R′, in which R′ is an organic group with 1 to 10 carbon atoms, is contacted with ammonia and hydrogen in a suitable solvent at elevated pressure in the presence of a hydrogenation catalyst to a mixture of primary amino compounds and &egr;-caprolactam, followed by a separate second step (b) in which the primary amino compounds are reacted to &egr;-caprolactam, wherein the solvent in step (a) is an aqueous medium, including water, the yield to &egr;-caprolactam in step (a) is more than 10%, calculated on the initial molar amount of the compound according to formula (1), that &egr;-caprolactam is separated from the aqueous mixture obtained in step (a) by extraction and that the aqueous mixture resulting from the extraction, containing the primary amino compounds, is used in step (b).
摘要翻译： 制备ε-己内酰胺的方法，其中在步骤（a）具有以下通式的化合物：其中R是-OH，-NH 2或O-R'，其中R'是有机基团，其中1至 10的碳原子在合适的溶剂中，在氢化催化剂的存在下，在氨基酸和ε-己内酰胺的混合物中，在合适的溶剂中与氨和氢接触，随后分开第二步（b），其中伯氨基 化合物与ε-己内酰胺反应，其中步骤（a）中的溶剂是水性介质，包括水，步骤（a）中ε-己内酰胺的收率大于10％，根据化合物的初始摩尔量计算 根据式（1），通过萃取将ε-己内酰胺与步骤（a）中获得的含水混合物分离，并且在步骤（b）中使用含有伯氨基化合物的萃取产生的含水混合物。
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9.发明授权Process to separate &egr;-caprolactam from 6-aminocaproamide and 6-aminocaproamide oligomers 失效将ε-己内酰胺与6-氨基己酰胺和6-氨基己酰胺低聚物分离的方法公开(公告)号：US06207827B1
公开(公告)日：2001-03-27
申请号：US09295310
申请日：1999-04-21
申请人： Rudolf P. M. Guit
发明人： Rudolf P. M. Guit
IPC分类号： C07D20116
CPC分类号： C07D201/16 , C07D201/08
摘要： Process to separate &egr;-caprolactam from 6-aminocaproamide and 6-aminocaproamide oligomers, wherein &egr;-caprolactam, 6-aminocaproamide and 6 aminocaproamide oligomers are present in a first aqueous starting mixture, which mixture is contacted with an alcohol extraction solvent, resulting in a first aqueous raffinate phase which is poor in &egr;-caprolactam and an alcohol phase which is rich in &egr;-caprolactam and which alcohol phase contains 6-aminocaproamide and/or 6-aminocaproamide oligomers, wherein the latter alcohol phase is subsequently contacted with water (backwash water) resulting in an alcohol extract phase poor in 6-aminocaproamide and/or 6-aminocaproamide oligomers and a second aqueous raffinate phase rich in 6-aminocaproamide and/or 6-aminocaproamide oligomers.
摘要翻译： 将ε-己内酰胺与6-氨基己酰胺和6-氨基己酰胺低聚物分离的方法，其中ε-己内酰胺，6-氨基己酰胺和6-氨基己酰胺低聚物存在于第一含水起始混合物中，该混合物与醇提取溶剂接触，得到 第一水性萃余相，其ε-己内酰胺不良和富含ε-己内酰胺且醇相含有6-氨基己酰胺和/或6-氨基己酰胺低聚物的醇相，其中后一个醇相随后与水接触（反冲洗 水），导致6-氨基己酰胺和/或6-氨基己酰胺低聚物中的醇提取相差和富含6-氨基己酰胺和/或6-氨基己酰胺低聚物的第二含水萃余液相。
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公开(公告)号：US5973143A
公开(公告)日：1999-10-26
申请号：US141406
申请日：1998-08-21
申请人： Rudolf P. M. Guit , Samuel L. Lane , Wim Buijs
发明人： Rudolf P. M. Guit , Samuel L. Lane , Wim Buijs
IPC分类号： C07D201/08
CPC分类号： C07D201/08
摘要： Process to prepare .epsilon.-caprolactam starting from a liquid aqueous mixture containing an alcohol and 6-aminocaproic acid by cyclization of 6-aminocaproic acid in the aqueous mixture at an elevated temperature. The alcohol is separated from the starting aqueous mixture before performing the cyclization to such extent that the concentration of alcohol in the aqueous mixture during the cyclization is less than 1 wt. %. The advantages include reduced amounts of undesirable by-product.
摘要翻译： 通过在高温下在含水混合物中环化6-氨基己酸，从含有醇和6-氨基己酸的液体含水混合物中制备ε-己内酰胺的方法。 在进行环化之前，将醇与起始含水混合物分离，使得环化过程中含水混合物中醇的浓度小于1wt。 ％。 优点包括减少不希望的副产物的量。
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