公开(公告)号：US4216151A

公开(公告)日：1980-08-05

申请号：US964790

申请日：1978-11-28

Applicant: Reijer Goettsch ,  Arnold G. M. Jetten

Inventor： Reijer Goettsch ,  Arnold G. M. Jetten

IPC: C07D207/263 ,  C07D201/16 ,  C07D207/26

CPC classification number: C07D201/16

Abstract: A process for the recovery of 2-pyrrolidone from the aqueous reaction product obtained in the preparation of 2-pyrrolidone from the hydrogenation of succinonitrile and subsequent reaction with water of the hydrogenation product thus obtained. The aqueous reaction mixture is adjusted to a pH value of 7 or lower and extracted with chloroform or methylene chloride to form an organic phase containing substantially all of the 2-pyrrolidone. The 2-pyrrolidone can be recovered from the organic phase by distillation, or by further extraction with water followed by crystallization from the aqueous phase thus formed or by evaporation of water.

Abstract translation: 从由琥珀腈的氢化制备2-吡咯烷酮得到的水性反应产物和随后与如此得到的氢化产物与水的反应中回收2-吡咯烷酮的方法。 将水性反应混合物调节至pH值为7以下，用氯仿或二氯甲烷萃取，形成基本上含有所有2-吡咯烷酮的有机相。 可以通过蒸馏从有机相中回收2-吡咯烷酮，或者通过进一步用水萃取，然后从由此形成的水相或通过蒸发水结晶。

公开(公告)号：US4178287A

公开(公告)日：1979-12-11

申请号：US968807

申请日：1978-12-12

Applicant: Roberto Mattone ,  Mario Catoni

Inventor： Roberto Mattone ,  Mario Catoni

IPC: C07D201/16 ,  C07D223/10

CPC classification number: C07D223/10 ,  C07D201/16

Abstract: There is described a process for the purification of caprolactam from the idable impurities present therein, by means of a treatment with an oxidizing agent consisting of ozone, the process comprising the steps of dissolving the polluted caprolactam into a solvent inert to ozone, such as water, and of causing the ozone to bubble through the resulting solution, the concentration of the caprolactam in the solution being preferably comprised between about 40% and 78% by weight of caprolactam, and the treatment being preferably effected at a temperature between the freezing temperature of the solution and 70.degree. C.

Abstract translation: 描述了通过用由臭氧组成的氧化剂的处理从其中存在的可氧化杂质中纯化己内酰胺的方法，该方法包括以下步骤：将被污染的己内酰胺溶解在对臭氧惰性的溶剂中，例如水 ，并且通过所得溶液使臭氧气泡，所述溶液中己内酰胺的浓度优选为己内酰胺的约40％至78％（重量），并且处理优选在冷冻温度 溶液和70℃

公开(公告)号：US4165328A

公开(公告)日：1979-08-21

申请号：US901089

申请日：1978-04-28

Applicant: Kenji Nishimura ,  Haruhiko Miyazaki ,  Kenji Kuniyasu ,  Satoru Ono

Inventor： Kenji Nishimura ,  Haruhiko Miyazaki ,  Kenji Kuniyasu ,  Satoru Ono

IPC: C07C45/00 ,  C07C45/78 ,  C07C45/80 ,  C07C45/82 ,  C07C49/403 ,  C07D201/02 ,  C07D201/04 ,  C07D201/16 ,  C07C121/407

CPC classification number: C07C255/00 ,  C07C45/783 ,  C07C45/80 ,  C07C45/82 ,  C07D201/16

Abstract: Disclosed is a process for separating 11-cyanoundecanoic acid, cyclohexanone and .epsilon.-caprolactam from a pyrolysis product obtained by pyrolyzing 1,1'-peroxydicyclohexylamine in the presence of steam at a temperature of 300.degree. to 1,000.degree. C. The pyrolysis product is first contacted with a mixture comprised of aqueous ammonia and at least one organic solvent selected from benzene, toluene and xylene, and the so prepared liquid is separated into the oily layer and the aqueous layer. On one hand, the oily layer is distilled to separate cyclohexanone therefrom. On the other hand, the aqueous layer is acidified to a pH of below 4.0 by adding thereto a mineral acid and maintained at a temperature of 40.degree. to 100.degree. C. to separate crude 11-cyanoundecanoic acid in molten form from the aqueous layer, and then, the separated crude molten 11-cyanoundecanoic acid is washed with hot water to extract .epsilon.-caprolactam therefrom.

Abstract translation: 公开了一种通过在300℃至1000℃的温度下在1,1'-二氧化二环己基胺蒸气存在下热解得到的热解产物中分离出11-氰基十一烷酸，环己酮和ε-己内酰胺的方法。热解产物是先 与由氨水和选自苯，甲苯和二甲苯中的至少一种有机溶剂组成的混合物接触，将如此制备的液体分离成油层和水层。 一方面，将油层蒸馏以分离出环己酮。 另一方面，通过向其中加入无机酸将水层酸化至pH值低于4.0，并保持在40℃至100℃的温度下，将熔融形式的粗的11-氰基十一烷酸与水层分离， 然后，将分离的粗熔融的11-氰基十一烷酸用热水洗涤以从其中提取ε-己内酰胺。

公开(公告)号：US4154729A

公开(公告)日：1979-05-15

申请号：US848210

申请日：1977-11-03

Applicant: Hugo Fuchs ,  Uwe Brand ,  Klaus Kartte

Inventor： Hugo Fuchs ,  Uwe Brand ,  Klaus Kartte

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: In a process for the continuous extraction of caprolactam from crude lactam by means of benzene in counter-current, in which crude lactam is fed into the upper part of an extraction zone and benzene into the lower part, a solution of caprolactam in benzene is taken off at the top and an aqueous solution containing impurities is taken off at the bottom, the improvement that water is additionally fed into the upper part of the extraction zone and a part of the aqueous solution, containing impurities, obtained at the bottom of the extraction zone is recycled into the extraction zone. Caprolactam is used for the manufacture of nylon.

Abstract translation: 在将粗制内酰胺进料到提取区上部并进入下部的苯中，通过逆流中的苯从粗制内酰胺连续提取己内酰胺的方法，将己内酰胺在苯中的溶液 在底部取出含有杂质的水溶液，改善了将水另外进料到提取区的上部，并将部分含有杂质的水溶液在提取物的底部获得 区域被回收到提取区域。 己内酰胺用于制造尼龙。

公开(公告)号：US4148793A

公开(公告)日：1979-04-10

申请号：US832002

申请日：1977-09-09

Applicant: Harry Danziger ,  Ludwig Deibele ,  Bernd-Ulrich Kaiser

Inventor： Harry Danziger ,  Ludwig Deibele ,  Bernd-Ulrich Kaiser

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: Process for the removal of residues of solvent from crystallized .epsilon.-caprolactam, wherein the major quantity of solvent is removed in a first stage by distillation in the presence of water in an amount so that the water content of the residue of the first stage is from 0.5 to 6% by weight, and in a second stage by distilling water and any residues of solvent still present.

Abstract translation: 从结晶的ε-己内酰胺中除去溶剂残留物的方法，其中在第一阶段通过在水存在下蒸馏除去主要量的溶剂，其量使得第一阶段的残留物的水含量来自 0.5至6重量％，并且在第二阶段通过蒸馏水和仍然存在的溶剂的任何残留物。

公开(公告)号：US4139696A

公开(公告)日：1979-02-13

申请号：US792421

申请日：1977-04-29

Applicant: Byron E. Anshus ,  Kiyoshi Katsumoto ,  Ira M. Serkes

Inventor： Byron E. Anshus ,  Kiyoshi Katsumoto ,  Ira M. Serkes

IPC: B01D3/34 ,  C07D201/16 ,  C07D207/26 ,  C07D207/267 ,  C08G69/24

CPC classification number: C07D207/267 ,  B01D3/34 ,  C07D201/16 ,  C08G69/24

Abstract: 2-Pyrrolidone is continuously polymerized to a high-molecular-weight particulate product by the stirred polymerization of the carbonated alkaline polymerizate. The polymerizate is prepared by contacting an aqueous hydroxide with excess 2-pyrrolidone, maintaining the resultant alkaline mixture at an elevated temperature for sufficient time to reduce the 2-pyrrolidone dimer content of the mixture to within the desired limits, dehydrating the alkaline mixture to reduce the water content to within the desired limits, and contacting the alkaline mixture with carbon dioxide to form the carbonated alkaline polymerizate. The paste of particular polypyrrolidone and liquid polymerizate is continuously withdrawn from the reactor, neutralized with aqueous acid and washed with warm water.

Abstract translation: 通过碳酸化碱性聚合物的搅拌聚合将2-吡咯烷酮连续聚合成高分子量颗粒产物。 通过使氢氧化钠与过量的2-吡咯烷酮接触来制备聚合物，将得到的碱性混合物保持在升高的温度下足够的时间以将混合物的2-吡咯烷酮二聚体含量降低至所需限度内，使碱性混合物脱水以减少 水含量达到所需限度内，并使碱性混合物与二氧化碳接触以形成碳酸化的碱性聚合物。 将特定聚吡咯烷酮和液体聚合物的糊料从反应器中连续取出，用酸水溶液中和，并用温水洗涤。

公开(公告)号：US4107160A

公开(公告)日：1978-08-15

申请号：US827370

申请日：1977-08-24

Applicant: Ovidiu Dicoi ,  Erwin Doerr

Inventor： Ovidiu Dicoi ,  Erwin Doerr

IPC: C07D201/12 ,  C07D201/16

CPC classification number: C07D201/16 ,  C07D201/12

Abstract: A process for the continuous recovery of caprolactam from either solid polycaprolactam waste by depolymerization or from liquid polycaprolactam extraction water from an extraction zone where, in either instance, a caprolactam water vapor mixture is produced and subsequently upgraded in a distillation zone to provide a dilute mixture of caprolactam and water vapor. A minor portion of this dilute caprolactam water vapor is condensed and recycled to the distillation zone. The remaining, major portion of this mixture is compressed and admixed with fresh steam, superheated and passed to either the extraction zone or depolymerization reaction.

Abstract translation: 从固体聚己内酰胺废物通过解聚连续回收己内酰胺或从液体聚己内酰胺萃取水中从萃取区连续回收己内酰胺的方法，其中在任何一种情况下产生己内酰胺水蒸气混合物，随后在蒸馏区中升级以提供稀释混合物 的己内酰胺和水蒸汽。 该稀少己内酰胺水蒸气的一小部分被冷凝并再循环到蒸馏区。 将该混合物的剩余部分压缩并与新鲜蒸汽混合，过热并通过萃取区或解聚反应。

公开(公告)号：US4050994A

公开(公告)日：1977-09-27

申请号：US745501

申请日：1976-11-26

Applicant: Byron E. Anshus

Inventor： Byron E. Anshus

IPC: C08G69/00 ,  B01D3/34 ,  C07D201/16 ,  C07D207/26 ,  C07D207/267 ,  C08G69/24 ,  C07D207/12

CPC classification number: C07D207/267 ,  B01D3/34 ,  C07D201/16

Abstract: A two-stage evaporative method for recovering polymerizable 2-pyrrolidone from alkaline aqueous solutions such as those obtained by washing the catalyst from an incompletely reacted polypyrrolidone polymerizate, includes the steps of neutralizing the base with mineral acid, removing most of the water in an initial reduced pressure evaporation and recovering the pyrrolidone from a salt/pyrrolidone slurry by vaporization under reduced pressure.

Abstract translation: 从由不完全反应的聚吡咯烷酮聚合物洗涤催化剂得到的碱性水溶液中回收可聚合的2-吡咯烷酮的两阶段蒸发方法包括以无机酸中和碱的步骤，初始地除去大部分水 减压蒸发并通过在减压下汽化从盐/吡咯烷酮浆液中回收吡咯烷酮。

公开(公告)号：US4036830A

公开(公告)日：1977-07-19

申请号：US681745

申请日：1976-04-29

Applicant: Abraham H. de Rooij ,  Reijer Goettsch

Inventor： Abraham H. de Rooij ,  Reijer Goettsch

IPC: C01C1/24 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A process for recovering substantially pure .epsilon.-caprolactam from a contaminated solution thereof is disclosed by concentrating, if needed, the caprolactam content of the solution to about 60-75 weight percent then extracting the concentrated solution with an organic solvent such as benzene or the like, then recovering the resulting caprolactam-laden organic solution.

Abstract translation: 通过将需要的己内酰胺含量浓缩至约60-75％（重量），然后用有机溶剂如苯等萃取浓缩溶液来公开从其污染溶液中回收基本上纯的ε-己内酰胺的方法 ，然后回收所得的己内酰胺负载有机溶液。

公开(公告)号：US4001274A

公开(公告)日：1977-01-04

申请号：US635996

申请日：1975-11-28

Applicant: Kiyoshi Katsumoto

Inventor： Kiyoshi Katsumoto

IPC: C07D201/16 ,  C07D207/12

CPC classification number: C07D201/16

Abstract: 2-PYRROLIDONE IS SEPARATED FROM AQUEOUS SOLUTION BY PHASE SEPARATION IN THE PRESENCE OF POTASSIUM HYDROGEN PHOSPHATE.