公开(公告)号：US5264571A

公开(公告)日：1993-11-23

申请号：US954731

申请日：1992-09-30

Applicant: Hugo Fuchs ,  Gerald Neubauer ,  Josef Ritz

Inventor： Hugo Fuchs ,  Gerald Neubauer ,  Josef Ritz

IPC: C07D201/04 ,  C07D201/06 ,  C07D223/10 ,  C07D201/16

CPC classification number: C07D201/04 ,  C07D201/06

Abstract: A process for preparing caprolactam by Beckmann rearrangement of cyclohexanone oxime with oleum at from 85.degree. to 125.degree. C. in a plurality of rearrangement stages arranged in series entails returning a portion of the reaction mixture leaving the last rearrangement stage to at least one of the preceding rearrangement stages.

Abstract translation: 通过贝克曼重整环己酮肟与发烟硫酸在85℃至125℃下重排排列的多个重排阶段制备己内酰胺的方法需要将离开最后一个重排阶段的一部分反应混合物返回至 以前的重排阶段。

公开(公告)号：US5227028A

公开(公告)日：1993-07-13

申请号：US725090

申请日：1991-07-03

Applicant: Hubertus J. M. Bosman ,  Paul C. Van Geem ,  Petrus J. H. Thomissen

Inventor： Hubertus J. M. Bosman ,  Paul C. Van Geem ,  Petrus J. H. Thomissen

IPC: C07C231/24 ,  B01D9/04 ,  C07B63/02 ,  C07C227/22 ,  C07D201/14 ,  C07D201/16 ,  C07D223/10

CPC classification number: C07C227/22 ,  C07D201/16 ,  C07D223/10

Abstract: A process of treating a ketoxime or aldoxime-containing amide mixture resulting from a Beckmann rearrangement of the corresponding ketoxime or aldoxime. The process involves hydrolysis of the mixture to remove the remaining ketoxime or aldoxime which are converted to the corresponding ketone or aldehyde and then separated off from the mixture. Any amino acid resulting from the hydrolysis can be reconverted to the corresponding amide by raising the temperature of the mixture.

公开(公告)号：US4963672A

公开(公告)日：1990-10-16

申请号：US448899

申请日：1989-12-12

Applicant: Franz Merger ,  Rolf Fischer ,  Wolfgang Harder ,  Claus-Ulrich Priester ,  Uwe Vagt

Inventor： Franz Merger ,  Rolf Fischer ,  Wolfgang Harder ,  Claus-Ulrich Priester ,  Uwe Vagt

IPC: B01J23/46 ,  C07B61/00 ,  C07D201/08 ,  C07D201/16

CPC classification number: C07D201/08 ,  Y02P20/52

Abstract: Caprolactam is prepared in a process comprising the following steps:(a) reacting the 5-formylvaleric ester with liquid ammonia as reaction medium and hydrogen in the presence of a ruthenium catalyst in liquid phase at from 80.degree. to 140.degree. C. under a hydrogen partial pressure of from 40 to 100 bar,(b) replacing the reaction medium ammonia by an aromatic hydrocarbon having a boiling point of from 80.degree. to 240.degree. C. which is liquid under the reaction conditions,(c) heating the resulting mixture in liquid phase under superatmospheric pressure at 230.degree.-350.degree. C. to form caprolactam, and(d) isolating caprolactam from the resulting reaction mixture.

Abstract translation: 己内酰胺以包括以下步骤的方法制备：（a）使5-甲酰基戊酸酯与液氨作为反应介质和氢在钌催化剂存在下在液相中在80-140℃下在氢气 分压为40〜100巴，（b）在反应条件下用沸点为80〜240℃的芳烃替代反应介质氨，（c）将所得混合物加热 液相在超大气压下在230-350℃下反应形成己内酰胺，和（d）从所得反应混合物中分离己内酰胺。

公开(公告)号：US4720328A

公开(公告)日：1988-01-19

申请号：US529063

申请日：1983-09-02

Applicant: Tom F. Corbin ,  Jack A. Dellinger ,  Kenneth B. Wagener

Inventor： Tom F. Corbin ,  Jack A. Dellinger ,  Kenneth B. Wagener

IPC: C07D201/16 ,  B01D3/10 ,  B01D3/34

CPC classification number: C07D201/16

Abstract: A method for removing impurities from caprolactam is disclosed. The method comprises the sequential steps of treating the impure caprolactam with phosphorus pentoxide so that the impurities react therewith to form high boiling species and then distilling the so treated impure lactam to recover substantially pure caprolactam as overhead, with the impurities remaining as bottoms.

Abstract translation: 公开了从己内酰胺除去杂质的方法。 该方法包括用五氧化二磷处理不纯的己内酰胺的顺序步骤，使得杂质与其反应形成高沸点物质，然后蒸馏如此处理的不纯内酰胺以回收基本上纯的己内酰胺作为塔顶馏出物，其中杂质作为底部残留。

公开(公告)号：US4311642A

公开(公告)日：1982-01-19

申请号：US187864

申请日：1980-09-17

Applicant: Lamberto Crescentini ,  Webb B. Blackman, Jr. ,  Joseph D. DeCaprio ,  William B. Fisher ,  Roy J. Lilley, Jr. ,  John W. Wagner

Inventor： Lamberto Crescentini ,  Webb B. Blackman, Jr. ,  Joseph D. DeCaprio ,  William B. Fisher ,  Roy J. Lilley, Jr. ,  John W. Wagner

IPC: C07D201/12 ,  C07D201/16

CPC classification number: C07D201/12 ,  C07D201/16

Abstract: This invention is the method to recover caprolactam from a concentrated nylon 6 chip wash water containing water, cyclic oligomer, and caprolactam. The method comprises feeding the concentrated wash water to a wiped-film evaporator operated at a temperature of from about 200.degree. C. to 300.degree. C. and a pressure from about 10 to about 250 Torr, thereby separating the wash water into (a) an overhead stream of water and caprolactam and (b) a bottom stream of caprolactam and cyclic oligomers, then recovering the caprolactam from the overhead stream. The caprolactam in the bottom stream can also be recovered, and the cyclic oligomers depolymerized to caprolactam for recovery.

Abstract translation: 本发明是从含有水，环状低聚物和己内酰胺的浓缩尼龙6片洗涤水中回收己内酰胺的方法。 该方法包括将浓缩的洗涤水加入到在约200℃至300℃的温度和约10至约250托的压力下操作的擦膜蒸发器，从而将洗涤水分离成（a） 水和己内酰胺的顶部物流和（b）己内酰胺和环状低聚物的底部流，然后从顶部物流中回收己内酰胺。 也可以回收底部流中的己内酰胺，环状低聚物解聚为己内酰胺以进行回收。

公开(公告)号：US4187370A

公开(公告)日：1980-02-05

申请号：US842758

申请日：1977-10-17

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: An alkaline-catalyzed process for preparing poly-2-pyrrolidone characterized by the step of treating the polypyrrolidone reaction product mixture with an acid to prevent polymer agglomeration and prevent base-catalyzed polymer degradation. In another embodiment, unreacted poly-2-pyrrolidone is recovered by washing the acid-treated polymer reaction product mixture with water and the resulting wash water recovered, treated with further acid, and then subjected to a two-stage evaporation process. Poly-2-pyrrolidone is known as nylon 4, and can be shaped into filaments and various molded articles.

Abstract translation: 一种碱催化的制备聚-2-吡咯烷酮的方法，其特征在于用酸处理聚吡咯烷酮反应产物混合物以防止聚合物凝聚并防止碱催化聚合物降解的步骤。 在另一个实施方案中，通过用水洗涤酸处理的聚合物反应产物混合物来回收未反应的聚-2-吡咯烷酮，并将所得洗涤水回收，再用酸处理，然后进行两阶段蒸发处理。 聚-2-吡咯烷酮被称为尼龙4，并且可以成形为长丝和各种模制品。

公开(公告)号：US4153600A

公开(公告)日：1979-05-08

申请号：US865338

申请日：1977-12-28

Applicant: Gerardus A. Geurts ,  Reijer Goettsch

Inventor： Gerardus A. Geurts ,  Reijer Goettsch

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A method of recovering .epsilon.-caprolactam from the residue remaining from the distillation of impure .epsilon.-caprolactam wherein the residue is treated with sulphuric acid or oleum at a temperature between about 80.degree. C. and about 140.degree. C. and the resultant mixture neutralized. The lactam is then extracted with an organic solvent with the lactam then recovered from the resultant solution.

Abstract translation: 从残余的不纯的ε-己内酰胺的蒸馏残余物中回收ε-己内酰胺的方法，其中残余物在约80℃至约140℃的温度下用硫酸或发烟硫酸处理，并将所得混合物中和。 然后用有机溶剂萃取内酰胺，然后从所得溶液中回收内酰胺。

公开(公告)号：US4081442A

公开(公告)日：1978-03-28

申请号：US765102

申请日：1977-02-02

Applicant: Willem J. Wassen ,  Reijer Goettsch

Inventor： Willem J. Wassen ,  Reijer Goettsch

IPC: C01C1/24 ,  C07D201/16 ,  C07D201/04

CPC classification number: C07D201/16

Abstract: A process for removing sulfuric acid from reaction mixtures containing sulfuric acid and .epsilon.-caprolactam by treating the sulfuric acid with ammonia and sulfur dioxide to produce ammonium sulfate salts and reducing the ammonium sulfate salts to ammonia and sulfur dioxide.

Abstract translation: 通过用氨和二氧化硫处理硫酸以产生硫酸铵盐并将硫酸铵盐还原成氨和二氧化硫，从含有硫酸和ε-己内酰胺的反应混合物中除去硫酸的方法。

公开(公告)号：US4017482A

公开(公告)日：1977-04-12

申请号：US603444

申请日：1975-08-11

Applicant: Rudolph Hans Gath ,  Hugo Fuchs

Inventor： Rudolph Hans Gath ,  Hugo Fuchs

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A method of simultaneously purifying crude caprolactams obtained from the Beckmann rearrangement of cyclohexanone oxime in oleum and the gas-phase rearrangement of cyclohexanone oxime in the presence of catalysts. The improvement consists in that the crude caprolactam obtained from the catalytic gas-phase rearrangement is added to the acid rearrangement mixture derived from the Beckmann rearrangement in oleum and the mixture is maintained at temperatures of from 100.degree. to 200.degree. C with thorough mixing, whereupon it is neutralized and worked up. Advantageously, the content of lactam in the catalytic gas-phase rearrangement is from 5 to 30% of the content of lactam in the acid rearrangement mixture obtained from the Beckmann rearrangement.

Abstract translation: 在催化剂存在下，同时纯化得自发酵天然气的环己酮肟贝克曼重排和环己酮肟气相重排得到的粗己内酰胺的方法。 改进之处在于将从催化气相重排获得的粗己内酰胺加入到发泡油中由Beckmann重排产生的酸重排混合物中，并将混合物通过充分混合保持在100至200℃的温度， 它被中和和处理。 有利地，催化气相重排中的内酰胺的含量为从Beckmann重排得到的酸重排混合物中的内酰胺含量的5〜30％。

公开(公告)号：US4013640A

公开(公告)日：1977-03-22

申请号：US459968

申请日：1974-04-11

Applicant: George S. Somekh

Inventor： George S. Somekh

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A solvent extraction-distillation process for the recovery of a water-soluble aliphatic amide having 1 to 8 carbon atoms or mixtures thereof from an aqueous solution wherein the concentration of the amide is in the range of about 0.25 percent by weight to about 25 percent by weight, based on the weight of the solution, and the solvent is a compound having the following structural formula: ##STR1## wherein M is OH or CH.sub.2 OH, R is hydrogen or an alkyl radical, there being at least one alkyl radical, and the total number of carbon atoms in all of said alkyl radicals taken together is 3 to 12, or a mixture of isomers thereof,Said compound or mixture of isomers having a boiling point higher than the amide and less than about 350.degree. C. and being non-azeotropic with the amide,Comprising the following steps:(a) contacting the solution in an extraction zone with the solvent to provide an extract comprising solvent, amide, and no more than about 5 percent by weight of water based on the weight of the solution and a raffinate comprising at least about 95 percent by weight of water based on the weight of the solution and less than about 5 percent by weight of solvent based on the weight of the solvent;(b) introducing the extract from step (a) into a distillation zone wherein the pressure is less than about 500 millimeters of mercury and the temperature is less than the decomposition temperatures of the amide and the solvent at said pressure, to separate the solvent from a mixture of amide and water; and(c) recovering the mixture of amide and water.