公开(公告)号：US4028347A

公开(公告)日：1977-06-07

申请号：US584219

申请日：1975-06-05

Applicant: Hans-Helmut Schwarz ,  Otto Immel

Inventor： Hans-Helmut Schwarz ,  Otto Immel

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: Object of the invention is a process for the treatment of a lactam distillation residue which contains boric acid in which a polyhydric alcohol is added to the crude lactam. By these means the formation of deposits and incrustations on the heating surfaces of the distillation apparatus can be prevented.

Abstract translation: 本发明的目的是一种处理含有硼酸的内酰胺蒸馏残余物的方法，其中将多元醇加入到粗内酰胺中。 通过这些方法，可以防止在蒸馏装置的加热面上形成沉积物和结垢。

公开(公告)号：US4014900A

公开(公告)日：1977-03-29

申请号：US482166

申请日：1974-06-24

Applicant: Stephen F. Pusztaszeri

Inventor： Stephen F. Pusztaszeri

IPC: C07D201/16 ,  C07D207/26

CPC classification number: C07D201/16

Abstract: Commercially efficient process for purifying commercial 2-pyrrolidone into substantially pure anhydrous 2-pyrrolidone comprises treating liquid impure 2-pyrrolidone with a minor amount of a solid substantially anhydrous metal hydroxide and flash vaporizing from a heated surface under closely controlled temperature and pressure conditions in a molecular distillation apparatus, without establishing a vapor pressure equilibrium. Very dark colored commercial 2-pyrrolidone may be given a preliminary purification treatment by cooling until the 2-pyrrolidone solidifies and draining off the dark-colored liquid containing impurities.

Abstract translation: 将市售2-吡咯烷酮纯化成基本上纯的无水2-吡咯烷酮的商业上有效的方法包括用少量固体基本上无水的金属氢氧化物处理液体不纯的2-吡咯烷酮，并在密封控制的温度和压力条件下从加热表面闪蒸 分子蒸馏装置，而不产生蒸气压平衡。 可以通过冷却进行非常深色的商业2-吡咯烷酮的初步纯化处理，直到2-吡咯烷酮固化并排出含有杂质的深色液体。

公开(公告)号：US3912721A

公开(公告)日：1975-10-14

申请号：US37379973

申请日：1973-06-26

Applicant: SNIA VISCOSA

Inventor： MATTONE ROBERTO ,  SIOLI GIANCARLO ,  GIUFFRE LUIGI

IPC: B01D11/04 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A method is disclosed for recovering lactams from acidic reaction mixtures, the improvement consisting in the fact that the extractant is an alkylsubstituted phenol the alkyl chain of which contains at least three carbon atoms, the alkyl substituent being capable of imparting to the phenol a lipophilic character. Monosubstituted and disubstituted phenols, such as isopropyl phenols, sec. and tert. butyl phenols, sec. and tert. amylphenols, di-sec. amylphenols and di-tert. amylphenols are preferred.

Abstract translation: 公开了一种用于从酸性反应混合物中回收内酰胺的方法，其改进在于提取剂是其烷基链含有至少三个碳原子的烷基取代酚，烷基取代基能够赋予苯酚亲油性 。 单取代和二取代的酚，如异丙基苯酚， 和叔丁基。 丁基酚，秒 和叔丁基。 戊基酚，二 - 戊基酚和二叔丁基。 戊基酚是优选的。

公开(公告)号：US3907781A

公开(公告)日：1975-09-23

申请号：US48260174

申请日：1974-06-24

Applicant: STAMICARBON

Inventor： DE ROOIJ ABRAHAM H ,  ELMENDORP JAN

IPC: C01C1/24 ,  C01C1/242 ,  C05C3/00 ,  C07D201/16 ,  C07D201/18

CPC classification number: C07D201/16 ,  E05Y2900/104

Abstract: Epsilon -CAPROLACTAM IS RECOVERED FROM A Beckmann rearrangement mixture of the lactam and aqueous sulfuric acid by simultaneously neutralizing the rearrangement mixture with ammonia at a pressure of 1-5 atmospheres and crystallizing out ammonium sulfate, the heat liberated by the neutralization reaction is removed from the system by evaporating a portion of the water from the solution. At the conditions employed hydrolysis of the lactam is substantially reduced if not entirely avoided.

Abstract translation: 通过在1-5个大气压的压力下同时用氨中和重排混合物并结晶出硫酸铵，将ε-CAPROLACTAM从内酰胺和硫酸水溶液的贝克曼重排混合物中回收，中和反应释放的热量从 系统通过从溶液中蒸发一部分水。 在使用条件下，如果不完全避免，内酰胺的水解将显着降低。

公开(公告)号：US3904609A

公开(公告)日：1975-09-09

申请号：US38033273

申请日：1973-07-18

Applicant: SNIA VISCOSA

Inventor： MATTONE ROBERTO ,  SIOLI GIANCARLO ,  GIUFFRE LUIGI

IPC: B01D3/00 ,  B01D9/02 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A method for the preparation of pure lactam is disclosed wherein a primary solution of the lactam in an organic phenolic solvent is supplemented by a compound miscible with the solution which is compatible with the primary solvent and is a solvent for the primary solvent but not for the lactam and susceptible of giving rise to precipitation of the lactam, the lactam being then separated from the mixture of the primary solvent and the compound which is a solvent for said primary solvent.

公开(公告)号：US3899485A

公开(公告)日：1975-08-12

申请号：US32612573

申请日：1973-01-23

Applicant: BAYER AG

Inventor： IMMEL OTTO ,  SCHWARZ HANS HELMUT

IPC: B01D11/04 ,  C07D201/16 ,  C07D1/06

CPC classification number: C07D201/16

Abstract: Object of the invention is a process for the purification of Epsilon -caprolactam prepared either by Beckmann rearrangement or by rearrangement of cyclohexanoxime in the gaseous phase or by depolymerisation of polyamide waste comprising treating the solid, finely-divided crude lactam with an organic solvent for a period of up to 60 hours at a temperature from 0* to 50*C. According to the purification process many impurities could be removed without a substantial decrease in the yield of the purified caprolactam.

Abstract translation: 本发明的目的是通过贝克曼重排或通过在气相中重新排列环己酮肟或通过聚酰胺废物的解聚来纯化ε-己内酰胺的方法，包括用有机溶剂处理固体细碎的内酰胺， 在0℃至50℃的温度下达60小时。根据纯化方法，可以除去许多杂质，而不会显着降低纯化的己内酰胺的产率。

公开(公告)号：US3859278A

公开(公告)日：1975-01-07

申请号：US38474773

申请日：1973-08-01

Applicant: STAMICARBON

Inventor： DE ROOY ABRAHAM H ,  GOETTSCH REIJER

IPC: C07D201/16 ,  C07D41/06

CPC classification number: C07D201/16

Abstract: Lactams are recovered from a solution of one or more lactams and sulfuric acid in an organic solvent after neutralization with ammonia or an ammonium salt and water without the simultaneous coproduction of solid ammonium sulfate according to the disclosed process. Ammonium hydrogen sulfate produced in the neutralization step is removed in the solution form, preferably concentrated to about 80 per cent by weight and the lactam is recovered from the organic solvent. Removing the ammonium hydrogen sulfate in the solution form rather than a solid avoids crystallization and deposition of the salt onto the surfaces of processing equipment.

公开(公告)号：US3852272A

公开(公告)日：1974-12-03

申请号：US24964272

申请日：1972-05-02

Applicant: STAMICARBON

Inventor： DE ROOIJ A H

IPC: C07D223/02 ,  C07D201/16 ,  C07D41/06

CPC classification number: C07D201/16

Abstract: A process for recovering lactam from a mixture of lactam and sulphuric acid is disclosed, wherein the mixture of lactam and sulphuric acid, such as that produced in a Beckmann rearrangement is partially neutralized and diluted by the addition of ammonia water. The amount of ammonia added is such that the molar ratio

Abstract translation: 公开了从内酰胺和硫酸的混合物中回收内酰胺的方法，其中内酯和硫酸的混合物，例如以贝克曼重排产生的那些，被部分中和并通过加入氨水稀释。 加入的氨的数量使得（NH 4）2 SO 4 /（NH 4）2 SO 4 + H 2 SO 4的摩尔比为约0.30:1至0.65:1。 加入的水的量为每摩尔最初存在的三氧化硫约3至约10摩尔水。 通过与水不混溶的有机内酰胺溶剂逆流萃取将内酰胺与部分中和的硫酸分离。

公开(公告)号：US3794647A

公开(公告)日：1974-02-26

申请号：US3794647D

申请日：1971-09-22

Applicant: INVENTA AG

Inventor： HENN R ,  SCHULTZE H ,  BERTHER C

IPC: C07D201/16 ,  C07D41/06

CPC classification number: C07D201/16

Abstract: A PROCESS FOR THE PURIFICATION OF LACTAMS OF EXTRACTION WHEREIN THE LACTAM IS TREATED IN THE CRYSTALLINE STATE WITH A SOLVENT CAPABLE OF DISSOLVING THE IMPURITIES SELECTIVELY.

公开(公告)号：US3761467A

公开(公告)日：1973-09-25

申请号：US3761467D

申请日：1971-02-11

Applicant: ALLIED CHEM

Inventor： WILLIAMS B ,  BOHN F

IPC: C07D201/16 ,  C07D41/06

CPC classification number: C07D201/16

Abstract: A PROCESS FOR SEPARATING E-CAPROLACTAM FROM AN AQUEOUS SOLUTION HIGHLY CONCENTRATED IN BOTH COLOR-FORMING AND OXIDIZABLE IMPURITIES WHEREBY THE SOLUTION IS FIRST EXTRACTED WITH AN ORGANIC, WATER-IMMISCIBLE SOLVENT FOR E-CAPROLACTAM, THEREBY SEPARATING THE E-CAPROLACTAM FROM THE COLOR-FORMING IMPURITIES AND THE RESULTANT ORGANIC E-CAPROLACTAM SOLUTION IS EXTRACTED WITH AN AQUEOUS SOLUTION, THEREBY SEPARATING THE E-CAPROLACTAM FROM THE OXIDIZABLE IMPURITIES.