公开(公告)号：US5700358A

公开(公告)日：1997-12-23

申请号：US396623

申请日：1995-03-01

Applicant: Hugo Fuchs ,  Josef Ritz ,  Gerald Neubauer

Inventor： Hugo Fuchs ,  Josef Ritz ,  Gerald Neubauer

IPC: C07D201/12 ,  C07D201/16 ,  C08G69/14 ,  C08G69/46 ,  B01D3/34

CPC classification number: C07D201/12 ,  C07D201/16

Abstract: Caprolactam is recovered from oligomers and/or polymers of caprolactam by cleavage of oligomers and/or polymers of caprolactam and subsequent working up by distillation of the caprolactam obtained in the cleavage, by a process including (a) cleaving oligomers and/or polymers of caprolactam to obtain an aqueous reaction mixture which contains caprolactam, (b) removing water from the reaction mixture obtained under (a) to obtain a residue, (c) distilling the residue obtained under (b) in an acidic medium and (d) then distilling the distillate in an alkaline medium to obtain caprolactam, or (c') distilling the residue obtained under (b) in an alkaline medium and (d') then distilling the distillate in an acidic medium to obtain caprolactam.

Abstract translation: 通过裂解己内酰胺的低聚物和/或聚己内酯并随后通过蒸馏在切割中获得的己内酰胺来处理己内酰胺从己内酰胺的低聚物和/或聚合物中回收己内酰胺，方法包括（a）裂解己内酰胺的低聚物和/或聚合物 得到含有己内酰胺的水性反应混合物，（b）从（a）得到的反应混合物中除去水，得到残渣，（c）将酸性介质中的（b）得到的残渣蒸馏，然后蒸馏 在碱性介质中的馏出物得到己内酰胺，或（c'）将在（b）获得的残余物在碱性介质中蒸馏，然后（d'），然后在酸性介质中蒸馏出馏出物，得到己内酰胺。

公开(公告)号：US5459261A

公开(公告)日：1995-10-17

申请号：US289577

申请日：1994-08-15

Applicant: Yasuhiko Higashio ,  Hiroshi Kajikuri ,  Keisuke Sugita ,  Hideki Doi ,  Masanobu Matsubara

Inventor： Yasuhiko Higashio ,  Hiroshi Kajikuri ,  Keisuke Sugita ,  Hideki Doi ,  Masanobu Matsubara

IPC: C07D201/16 ,  C07D201/14

CPC classification number: C07D201/16

Abstract: 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.

Abstract translation: 公开了一种制备高纯度己内酰胺的方法，其中通过环己酮肟的催化重排获得的粗己内酰胺在搅拌下与至少一种选自脂族烃和脂环族烃的烃进行混合 形成液 - 液两层液体混合物，然后从该液体混合物中结晶己内酰胺; （2）与选自脂族烃和脂环烃的至少一种烃和水混合以形成液体混合物，将液体混合物分离成烃层和水层，然后从其中回收己内酰胺 水层; 或（3）在至少一种10至18个碳原子的脂族饱和烃的共存下进行蒸馏。

公开(公告)号：US5362870A

公开(公告)日：1994-11-08

申请号：US46146

申请日：1993-04-15

Applicant: Yasuhiko Higashio ,  Hiroshi Kajikuri ,  Keisuke Sugita ,  Hideki Doi ,  Masanobu Matsubara

Inventor： Yasuhiko Higashio ,  Hiroshi Kajikuri ,  Keisuke Sugita ,  Hideki Doi ,  Masanobu Matsubara

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: 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.

Abstract translation: 公开了一种制备高纯度己内酰胺的方法，其中通过环己酮肟的催化重排获得的粗己内酰胺在搅拌下与至少一种选自脂族烃和脂环族烃的烃进行混合 形成液 - 液两层液体混合物，然后从该液体混合物中结晶己内酰胺; （2）与选自脂族烃和脂环烃的至少一种烃和水混合以形成液体混合物，将液体混合物分离成烃层和水层，然后从其中回收己内酰胺 水层; 或（3）在至少一种10至18个碳原子的脂族饱和烃的共存下进行蒸馏。

公开(公告)号：US4855053A

公开(公告)日：1989-08-08

申请号：US944271

申请日：1986-12-18

Applicant: Charles Benedetti ,  Claude Gluntz ,  Robert Pascal ,  Michel Stefanini

Inventor： Charles Benedetti ,  Claude Gluntz ,  Robert Pascal ,  Michel Stefanini

IPC: C07B63/00 ,  B01D11/04 ,  C02F1/26 ,  C07B31/00 ,  C07C27/00 ,  C07C37/72 ,  C07C39/04 ,  C07C39/27 ,  C07C67/00 ,  C07C209/00 ,  C07C209/86 ,  C07C211/03 ,  C07C211/27 ,  C07C227/40 ,  C07C229/08 ,  C07D201/16 ,  C07D225/02

CPC classification number: C07C37/72 ,  C02F1/26 ,  Y10S210/908 ,  Y10S210/909

Abstract: Process for extracting organic compounds which are present in water in the form of solutions or suspensions by a liquid carboxylic acid which is immiscible with water. Branched or unbranched linear acids such as n-heptanoic, n-octanoic, or 2-ethylhexanoic acids make it possible to quantitatively extract compounds such as phenols, amines or amino acids from such aqueous solutions, thereby rendering the process useful for the purification of industrial wastewaters.

Abstract translation: 通过与水不混溶的液体羧酸萃取溶液或悬浮液形式存在于水中的有机化合物的方法。 支链或非支链的直链酸如正庚酸，正辛酸或2-乙基己酸可以定量地从这些水溶液中提取化合物如酚，胺或氨基酸，从而使该方法可用于纯化工业 废水

公开(公告)号：US4795571A

公开(公告)日：1989-01-03

申请号：US154227

申请日：1988-02-10

Applicant: Bernhard Holzknecht ,  Hugo Fuchs ,  Eckhard Hetzel ,  Klaus Wintermantel ,  Peter Thoma

Inventor： Bernhard Holzknecht ,  Hugo Fuchs ,  Eckhard Hetzel ,  Klaus Wintermantel ,  Peter Thoma

IPC: B01D9/00 ,  B01D9/02 ,  B01D9/04 ,  C07B63/00 ,  C07C67/00 ,  C07C241/00 ,  C07C265/14 ,  C07D201/16

CPC classification number: C07D201/16 ,  B01D9/0013

Abstract: Frozen crystal layers are purified by a process in which these crystal layers, after they have been frozen out from a melt or solution on a cooling surface, are brought into contact with a purifying liquid and thus purified over their entire thickness, after which the said layers are separated from the purifying liquid and then melted, wherein the temperature of the crystal layers and of the purifying liquid is close to the melting point or solubility temperature, mass transfer at the phase boundary is intensified by forced convection, and this purification is carried out in the course of from 1 to 60 minutes on layers having a thickness of from 0.2 to 10 mm.

Abstract translation: 冷冻的晶体层通过这些方法纯化，其中这些晶体层在从冷却表面上的熔体或溶液中冷冻出来之后，与净化液体接触并由此在其整个厚度上净化，之后所述 将层与净化液分离，然后熔融，其中晶体层和净化液的温度接近熔点或溶解温度，通过强制对流加强相边界处的质量传递，并进行该纯化 在厚度为0.2至10mm的层上为1至60分钟的过程。

公开(公告)号：US4610768A

公开(公告)日：1986-09-09

申请号：US803752

申请日：1985-12-02

Applicant: Seid H. Moosavian

Inventor： Seid H. Moosavian

IPC: B01D3/36 ,  C07D201/16

CPC classification number: C07D201/16 ,  B01D3/36

Abstract: A process for drying lactams to extremely low water contents is provided which comprises mixing the lactam with hydrocarbon distilling from the mixture a water/hydrocarbon vapor and or condensate, contacting said vapor or condensate with a drying agent to remove water and returning the dried distillate to the mixture to permit recycling process is capable of providing anionic polymerization grade lactam with a water content of less than about 50 ppm.

Abstract translation: 提供了将内酰胺干燥至极低含水量的方法，其包括将内酰胺与从混合物中蒸馏出的水/烃蒸气和/或冷凝物混合，将所述蒸气或冷凝物与干燥剂接触以除去水并将干燥的馏出物返回到 允许再循环过程的混合物能够提供含水量小于约50ppm的阴离子聚合级内酰胺。

公开(公告)号：US4582642A

公开(公告)日：1986-04-15

申请号：US625143

申请日：1984-06-27

Applicant: Lamberto Crescentini ,  William B. Fisher ,  Richard E. Mayer ,  Joseph D. DeCaprio ,  Ronald K. Nilsen

Inventor： Lamberto Crescentini ,  William B. Fisher ,  Richard E. Mayer ,  Joseph D. DeCaprio ,  Ronald K. Nilsen

IPC: C07D201/16 ,  C07D201/12

CPC classification number: C07D201/16

Abstract: This invention is a method to recover caprolactam from a combined stream of mother liquor from a caprolactam crystallizer and other lactam containing aqueous streams, the improvement comprising steam distilling the combined stream at a temperature of from between about 180.degree. C. to 235.degree. C. in the absence of any depolymerization agent such as phosphoric acid; so that the residue from the steam distilling remains fluid; relatively low levels of caprolactam remain in the residue; less residue is generated; the recovered caprolactam has improved high quality; and losses of caprolactam due to side reactions are reduced.

Abstract translation: 本发明是从己内酰胺结晶器和其它含内含物含水流的母液的合并流中回收己内酰胺的方法，其改进包括在约180℃至235℃的温度下蒸馏合并的流。 在没有任何解聚剂如磷酸的情况下; 使蒸汽蒸馏残渣保持流体; 残余物中残留的己内酰胺水平相对较低; 产生较少的残留物; 回收的己内酰胺具有改善的高品质; 并且由于副反应而导致己内酰胺的损失降低。

公开(公告)号：US4293494A

公开(公告)日：1981-10-06

申请号：US143418

申请日：1980-04-24

Applicant: Paolo Senni ,  Domenico Astarita

Inventor： Paolo Senni ,  Domenico Astarita

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A method for purifying raw caprolactam containing, as impurities, primary amides of the formula ##STR1## R being a hydrocarbon radical having 1-14 carbon atoms, and other by-products is described. The operations, carried out in the following order, consist in (a) treating a solution of raw caprolactam in a water insoluble organic solvent with water to extract most of the caprolactam in purified form, (b) separating the aqueous caprolactam solution and isolating the caprolactam, (c) treating the remaining organic solution with mineral acid to cause the formation of two phases, (d) separating these phases into a heavy phase containing the mineral acid, dilution water and most of the amides and by-products and a light phase containing the organic solvent and any residual amides and by-products, and (e) preferably recycling the light phase to (a). Further object of the invention is the purified caprolactam thus obtained.

Abstract translation: 描述了含有作为杂质的具有1-14个碳原子的烃基的式（I）的初级酰胺和其它副产物的原己内酰胺的纯化方法。 按以下顺序进行的操作包括：（a）用水处理含水的不溶于水的有机溶剂中的己内酰胺溶液以提取大部分纯化形式的己内酰胺，（b）分离己内酰胺水溶液并分离 己内酰胺，（c）用无机酸处理剩余的有机溶液以形成两相，（d）将这些相分离成含有无机酸，稀释水和大部分酰胺和副产物的重相和轻质 相包含有机溶剂和任何残留的酰胺和副产物，和（e）优选将轻相循环至（a）。 本发明的另一个目的是由此获得的纯化的己内酰胺。

公开(公告)号：US4276215A

公开(公告)日：1981-06-30

申请号：US818564

申请日：1977-07-25

Applicant: Eugene V. Hort ,  Waldo R. De Thomas

Inventor： Eugene V. Hort ,  Waldo R. De Thomas

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: 2-Pyrrolidone is purified by contact with particulate calcium oxide for a sufficient time at elevated temperatures followed by distilling and condensing the purified 2-pyrrolidone.

Abstract translation: 通过在高温下与颗粒状氧化钙接触足够的时间，然后蒸馏并冷凝纯化的2-吡咯烷酮，纯化2-吡咯烷酮。

公开(公告)号：US4170592A

公开(公告)日：1979-10-09

申请号：US832007

申请日：1977-09-09

Applicant: Harry Danziger ,  Bernd-Ulrich Kaiser ,  Guido Rampart ,  Jurgen Schroter

Inventor： Harry Danziger ,  Bernd-Ulrich Kaiser ,  Guido Rampart ,  Jurgen Schroter

IPC: C01C1/24 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A process for the purification of a solution of .epsilon.-caprolactam in benzene, toluene or xylene by washing with a liquid, wherein the washing liquid is a solution of .epsilon.-caprolactam in water in a weight ratio of from 15 : 1 to 1 : 3, which is used in a quantity of from 5 to 20% by weight, based on the solution of caprolactam in benzene, toluene or xylene, and wherein there are several washing stages so that the equilibrium between the two solutions can be readjusted.

Abstract translation: 一种通过用液体洗涤来纯化ε-己内酰胺在苯，甲苯或二甲苯中的溶液的方法，其中洗涤液是ε-己内酰胺在水中的重量比为15:1至1:3的溶液 ，其用量为5至20重量％，基于己内酰胺在苯，甲苯或二甲苯中的溶液，并且其中有几个洗涤阶段，使得可以重新调节两种溶液之间的平衡。