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91. 发明授权

US06849731B2 Process for recovering and purifying caprolactam from an organic solvent 失效
标题翻译：从有机溶剂中回收和纯化己内酰胺的方法
公开(公告)号：US06849731B2
公开(公告)日：2005-02-01
申请号：US10468263
申请日：2002-02-27
申请人： Maria Louisa Christina Dsinter-De Hondt , Joannes Albertus Wilhelmus Lemmens
发明人： Maria Louisa Christina Dsinter-De Hondt , Joannes Albertus Wilhelmus Lemmens
IPC分类号： C07D201/16
CPC分类号： C07D201/16
摘要： Process for recovering caprolactam from a solution comprising caprolactam dissolved in an organic solvent, said process comprising: a) washing the solution with water or an aqueous alkaline solution, resulting in a washed solution comprising caprolactam and organic solvent and in a washing residue, b) evaporating organic solvent from the washed solution, resulting in caprolactam product, c) optionally, hydrogenating the caprolactam product, d) optionally, evaporating water from the caprolactam product, e) distilling the caprolactam product to recover caprolactam and a distillation residue, f) extracting the distillation residue with an organic solvent in the presence of water to obtain (i) an extract comprising caprolactam dissolved in organic solvent and (ii) an aqueous effluent, and g) recycling the extract to step a) or b).
摘要翻译：从包含溶解在有机溶剂中的己内酰胺的溶液中回收己内酰胺的方法，所述方法包括：a）用水或碱性水溶液洗涤溶液，得到包含己内酰胺和有机溶剂的洗涤溶液，并在洗涤残渣中，b）从洗涤的溶液中蒸发有机溶剂，得到己内酰胺产物，c）任选地使己内酰胺产物氢化，d）任选地从己内酰胺产物蒸发水，e）蒸馏己内酰胺产物以回收己内酰胺和蒸馏残渣，f）在水的存在下用有机溶剂蒸馏残余物，得到（i）包含溶解在有机溶剂中的己内酰胺的提取物和（ii）含水流出物，和g）将提取物再循环到步骤a）或b）。

92. 发明申请

US20030023083A1 Method for separating an azepine derivative out of a mixture containing an amine an azepine derivative 失效
标题翻译：从含有吖庚因衍生物的胺的混合物中分离出吖庚因衍生物的方法
公开(公告)号：US20030023083A1
公开(公告)日：2003-01-30
申请号：US10204966
申请日：2002-08-27
发明人： Hermann Luyken , Frank Ohlbach
IPC分类号： B01D001/00 , C07D201/16
CPC分类号： C07C209/86 , C07C253/34 , C07D223/04 , C07D223/12 , Y10S203/90
摘要： The invention relates to a method for separating by distillation a portion or the entirety of an azeptine derivative (III), which is selected from the group consisting of aminohexylidene imine, tetrahydroazepine, hexylhexahydroazepine and of aminohexylhexahydroazepine, out of a mixture (II) containing an azepine derivative (III) and an amine (I). The inventive method is characterized in that the distillation is carried out with a maximum bottom temperature of 150null C.
摘要翻译：本发明涉及一种通过蒸馏法从含有氨基亚氨基亚胺，四氢氮杂，己基六氢吖庚因和氨基己基六氢吖庚因的一种或多种氮杂基衍生物（III）的混合物（II）中分离出来的方法，吖庚因衍生物（III）和胺（I）。本发明的方法的特征在于在150℃的最高底部温度下进行蒸馏。

93. 发明授权

US5990306A Process for the purification of caprolactam obtained from the depolymerization of polyamide-containing carpet 失效
标题翻译：从含聚酰胺的地毯解聚得到的己内酰胺的纯化方法
公开(公告)号：US5990306A
公开(公告)日：1999-11-23
申请号：US922853
申请日：1997-09-03
申请人： Richard Eugene Mayer , Lamberto Crescentini , Theodore John Jenczewski
发明人： Richard Eugene Mayer , Lamberto Crescentini , Theodore John Jenczewski
IPC分类号： C07D201/12 , C07D201/16
CPC分类号： C07D201/12
摘要： The present invention provides a process for the preparation of purified caprolactam comprising the steps of:(a) depolymerizing polyamide-containing carpet in the presence of steam to obtain crude caprolactam and steam;(b) removing substantially all of said water from said crude caprolactam and steam(c) distilling the resulting concentrated crude caprolactam at a pressure of less than about 8 mmHg and a temperature from about 110.degree. C. to about 145.degree. C. so as to form overheads and bottoms of the caprolactam; and(d) crystallizing the caprolactam overheads to obtain caprolactam crystals and mother liquor.The resulting purified caprolactam may then be used to make polycaprolactam which may then be used in engineered materials or spun into fiber.
摘要翻译：本发明提供了制备纯己内酰胺的方法，包括以下步骤：（a）在蒸汽存在下解聚含聚酰胺的地毯以获得粗己内酰胺和蒸汽; （b）从所述粗己内酰胺和蒸汽中去除基本上所有的所述水;（c）在小于约8mmHg的压力和约110℃至约145℃的温度下蒸馏所得浓缩的粗己内酰胺，以便以形成己内酰胺的塔顶馏出物和塔底物; 和（d）结晶己内酰胺塔顶馏出物以获得己内酰胺晶体和母液。然后将所得纯化的己内酰胺用于制备聚己内酰胺，然后将其用于工程化材料或纺成纤维。

94. 发明授权

US5441607A Recovery of caprolactam from distillation residues obtained in the purification of caprolactam 失效
标题翻译：从己内酰胺纯化中获得的蒸馏残余物中回收己内酰胺
公开(公告)号：US5441607A
公开(公告)日：1995-08-15
申请号：US265740
申请日：1994-06-27
申请人： Hugo Fuchs , Josef Ritz , Hans J. Wilfinger , David Weatherford
发明人： Hugo Fuchs , Josef Ritz , Hans J. Wilfinger , David Weatherford
IPC分类号： C07D201/12 , C07D201/16 , B01D3/34
CPC分类号： C07D201/12 , C07D201/16
摘要： Recovery of caprolactam and of an alkali metal carbonate from distillation residues which are obtained in the purification of caprolactam and contain caprolactam and/or oligomers and/or polymers of caprolactam and also alkali metal hydroxides by(a) melting the distillation residues, the caprolactam and/or oligomers and/or polymers of caprolactam and alkali metal hydroxides,(b) continuously removing caprolactam from the melt,(c) after removing caprolactam, cooling the melt and obtaining a residue,(d) dissolving the residue thus obtained in water and(e) subjecting the aqueous solution thus obtained to combustion with the formation of an alkali metal carbonateis described.
摘要翻译：从纯化己内酰胺获得的己内酰胺和碱金属碳酸盐回收己内酰胺和/或己内酰胺和/或己内酰胺的聚合物和/或碱金属氢氧化物的齐聚物和/或碱金属氢氧化物，通过（a）将蒸馏残余物，己内酰胺和 /或己内酰胺和碱金属氢氧化物的低聚物和/或聚合物，（b）从熔体中连续除去己内酰胺，（c）除去己内酰胺后，冷却熔体并获得残余物，（d）将由此获得的残余物溶于水和（e）描述了所得到的水溶液在形成碱金属碳酸盐时的燃烧。

95. 发明授权

US5350847A Purification of caprolactam 失效
标题翻译：己内酰胺的纯化
公开(公告)号：US5350847A
公开(公告)日：1994-09-27
申请号：US113081
申请日：1993-08-30
申请人： Hugo Fuchs , Gerald Neubauer , Claus-Ulrich Priester
发明人： Hugo Fuchs , Gerald Neubauer , Claus-Ulrich Priester
IPC分类号： C07B63/02 , C07D201/16 , C07D201/12
CPC分类号： C07D201/16
摘要： Caprolactam is purified by oxidative treatment in which mixtures which essentially contain the caprolactam to be purified and unsaturated lactams are treated with oxygen or an oxygen-containing gas mixture in an alkaline medium.
摘要翻译：己内酰胺通过氧化处理纯化，其中基本上含有待纯化的己内酰胺和不饱和内酰胺的混合物在碱性介质中用氧或含氧气体混合物处理。

96. 发明授权

US4900821A Method for producing high-purity caprolactam 失效
标题翻译：生产高纯度己内酰胺的方法
公开(公告)号：US4900821A
公开(公告)日：1990-02-13
申请号：US330695
申请日：1989-03-30
申请人： Kazuo Tan , Takashi Hironaka , Michio Nakamura
发明人： Kazuo Tan , Takashi Hironaka , Michio Nakamura
IPC分类号： C07D201/16
CPC分类号： C07D201/16
摘要： A method for producing high-purity caprolactam from a mixture comprising a melt of crude caprolactam and water, which comprises cooling the mixture in a crystallizer under a reduced pressure of from 1 to 22 Torr while maintaining the water concentration in the mixture at a level of from 0.5 to 10% by weight, to crystallize high-purity caprolactam, and then separating the resulting crystals.

97. 发明授权

US4882430A Recovery of caprolactam from caprolactam distillation low boilers or high boilers or mixtures thereof 失效
标题翻译：从己内酰胺蒸馏低沸点锅炉或高锅炉或其混合物中回收己内酰胺
公开(公告)号：US4882430A
公开(公告)日：1989-11-21
申请号：US257274
申请日：1988-10-13
申请人： Gerald Neubauer , Emile De Decker , Hugo Fuchs , Bernhard Holzknecht , Josef Ritz
发明人： Gerald Neubauer , Emile De Decker , Hugo Fuchs , Bernhard Holzknecht , Josef Ritz
IPC分类号： C07D201/16
CPC分类号： C07D201/16
摘要： Caprolactam is recovered from caprolactam distillation low boilers or high boilers or mixtures thereof by the following steps:(a) crystallizing a low or high boiler or a mixture thereof to form purified capro-lactam crystals and a mother liquor,(b) separating off the purified caprolactam crystals to leave a mother liquor,(c) recycling from 5 to 90% by weight of the mother liquor of stage (b) into stage (a) and transferring the remainder of the mother liquor into the subsequent stage (d),(d) crystallizing the remaining mother liquor portion from stage (c) to form caprolactam crystals and a mother liquor, separating off the caprolactam crystals of stage(e) (d) and recycling the same into stage (a) to leave a mother liquor,(f) recycling from 20 to 99% by weight of mother liquor of stage (e) into stage (d) and channeling out the remainder of the impurity-containing mother liquor of stage (e).
摘要翻译：通过以下步骤从己内酰胺蒸馏低锅炉或高锅炉或其混合物回收己内酰胺：（a）使低或高锅炉或其混合物结晶以形成纯化的己内酰胺结晶和母液，（b）将纯化的己内酰胺晶体离开母液，（c）将阶段（b）的母液的5至90重量％循环到阶段（a）中，并将剩余的母液转移到后续阶段（d）中，（d）从阶段（c）中将剩余的母液部分结晶以形成己内酰胺晶体和母液，分离阶段（e）（d）的己内酰胺晶体并将其再循环到阶段（a）中以留下母液，（f）将阶段（e）的母液的20至99重量％循环到阶段（d）中，并且引出阶段（e）的含杂质母液的剩余部分。

98. 发明授权

US4767503A Removal of light impurities from caprolactam by distillation with water 失效
标题翻译：用水蒸馏从己内酰胺除去轻质杂质
公开(公告)号：US4767503A
公开(公告)日：1988-08-30
申请号：US527044
申请日：1983-08-29
申请人： Lamberto Crescentini , Joseph D. DeCaprio , William B. Fisher , Roy J. Lilley, Jr.
发明人： Lamberto Crescentini , Joseph D. DeCaprio , William B. Fisher , Roy J. Lilley, Jr.
IPC分类号： C07D201/16 , B01D3/14 , B01D3/38
CPC分类号： C07D201/16
摘要： This invention is a method of purifying crude caprolactam. The improved method comprises taking a portion of a process stream of crude caprolactam having low boiling impurities and distilling the stream in the presence of water by fractional distillation into an overhead containing water and low boiling impurities and bottoms of caprolactam having improved purity and low water content.The improvement also comprises taking a low water content stream of crude caprolactam having low boiling impurities and adding water to the stream and distilling the stream by fractional distillation as described above.
摘要翻译：本发明是纯化己内酰胺的方法。改进的方法包括取一部分具有低沸点杂质的粗己内酰胺的工艺流，并在水存在下通过分馏将该物流蒸馏到含有水和低沸点杂质的塔顶馏出物中，并且具有改善的纯度和低含水量的己内酰胺底部。改进之处还在于将低沸点杂质的低水含量的己内酰胺水含量低，并向水中加入水并通过如上所述的分馏蒸馏。

99. 发明授权

US4764607A Method for recovering caprolactam 失效
标题翻译：己内酰胺回收方法
公开(公告)号：US4764607A
公开(公告)日：1988-08-16
申请号：US945117
申请日：1986-12-22
申请人： Laszlo J. Balint , Julius Greenburg
发明人： Laszlo J. Balint , Julius Greenburg
IPC分类号： C07D201/16
CPC分类号： C07D201/16
摘要： Method and improved apparatus for recovering a volatile organic material, such as caprolactam, from a liquid mixture of organic and inorganic materials are disclosed. The method features the step of mixing the liquid mixture with superheated steam for 0.005 to 1.0 second to vaporize a large portion of the volatile organic material without degrading the organic materials. The steam and vaporized organic materials are then separated from the liquid mixture remaining, followed by separation of the vaporized organic material from the steam. The vaporized organic material subsequently is condensed. The improved apparatus features means for introducing superheated steam into a vaporizer feed pipe, as well as means for mixing the superheated steam with the liquid mixture in the pipe for 0.005 to 1.0 second so that a large portion of the volatile organic material is vaporized and feeds with the steam and remaining liquid mixture into the vaporizer for separation.
摘要翻译：公开了用于从有机和无机材料的液体混合物中回收挥发性有机材料如己内酰胺的方法和改进的装置。该方法的特征在于将液体混合物与过热蒸汽混合0.005至1.0秒以蒸发大部分挥发性有机材料而不降解有机材料。然后将蒸汽和蒸发的有机材料与剩余的液体混合物分离，然后将蒸发的有机材料与蒸汽分离。蒸发的有机材料随后被冷凝。改进的装置具有用于将过热蒸汽引入蒸发器进料管的装置，以及用于将过热蒸汽与管中的液体混合物混合0.005至1.0秒的装置，使得大部分挥发性有机材料蒸发并进料蒸汽和剩余的液体混合物进入蒸发器进行分离。

100. 发明授权

US4647661A Method of preparing .omega.-lactams, in particular caprolactam 失效
标题翻译：制备ω-内酰胺的方法，特别是己内酰胺
公开(公告)号：US4647661A
公开(公告)日：1987-03-03
申请号：US845122
申请日：1986-03-27
申请人： Paolo Senni , Leandro Zuliani , Sergio Ferruzzi
发明人： Paolo Senni , Leandro Zuliani , Sergio Ferruzzi
IPC分类号： C07D201/16 , C07D201/08 , C07D201/10
CPC分类号： C07D201/08
摘要： A method of preparing .omega.-lactams, in particular caprolactam, comprising: a step of premixing cycloaliphatic acids having the formula ##STR1## where n=3-13, with a dehydrating agent; the first step of reaction with a nitrosating agent; the second step of reaction with the addition of a very small amount of water corresponding to a molar ratio U=H.sub.2 O/SO.sub.3 within the 0.1 to 0.9 range; and the step of reclaiming the unreacted cycloaliphatic acid. The method affords improved output from the lactamization reaction and reduced byproducts.
摘要翻译：一种制备ω-内酰胺，特别是己内酰胺的方法，包括：将具有式“IMAGE”的其中n = 3-13的脂环族酸与脱水剂预混合的步骤; 与亚硝化剂反应的第一步; 反应的第二步骤是加入相当于0.1至0.9范围内的摩尔比U = H 2 O / SO 3的非常少量的水; 以及回收未反应的脂环族酸的步骤。该方法提供了来自内酰胺化反应的改进的产物和减少的副产物。

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