公开(公告)号：US4647661A

公开(公告)日：1987-03-03

申请号：US845122

申请日：1986-03-27

Applicant: Paolo Senni ,  Leandro Zuliani ,  Sergio Ferruzzi

Inventor： Paolo Senni ,  Leandro Zuliani ,  Sergio Ferruzzi

IPC: C07D201/16 ,  C07D201/08 ,  C07D201/10

CPC classification number: C07D201/08

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US4606858A

公开(公告)日：1986-08-19

申请号：US699520

申请日：1985-02-07

Applicant: Enrico Bondi ,  Paolo Senni

Inventor： Enrico Bondi ,  Paolo Senni

IPC: C07D223/10 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: The invention is concerned with a method of purifying caprolactam as obtained by Beckmann transposition or by nitrosation of cyclohexyl compounds, characterized in that it comprises the following steps:(a) the caprolactam oil is treated with ammonia to obtain a pH in the 8 to 10 range;(b) the caprolactam in water-ammonia solution yielded by (a) is extracted with toluene;(c.sub.1) any caprolactam still in the toluene solution yielded by (b) is treated with NaOH;(C.sub.2) the aqueous phase left over from the extraction with toluene (b) is removed.

Abstract translation: 本发明涉及通过Beckmann转位或通过环己基化合物的亚硝化得到的己内酰胺的纯化方法，其特征在于其包括以下步骤：（a）己内酰胺油用氨处理以获得8至10的pH 范围; （b）由（a）产生的水 - 氨溶液中的己内酰胺用甲苯萃取; （c1）由（b）产生的仍然在甲苯溶液中的任何己内酰胺用NaOH处理; （C2）除去用甲苯（b）从萃取液中留下的水相。

公开(公告)号：US4563308A

公开(公告)日：1986-01-07

申请号：US643026

申请日：1984-08-21

Applicant: Otto G. Plantema ,  Arnold G. M. Jetten ,  Nicolaas F. Haasen

Inventor： Otto G. Plantema ,  Arnold G. M. Jetten ,  Nicolaas F. Haasen

IPC: C07D201/16 ,  C07D201/04

CPC classification number: C07D201/16

Abstract: Process the recovering caprolactam from the residue remaining following the distillation, under reduced pressure, of impure caprolactam obtained by rearrangement of cyclohexanone oxime with sulphuric acid or oleum, by distilling the residue under reduced pressure whereby a caprolactam-containing distillate is obtained; hydrogenating the caprolactam containing distillate in an aqueous medium to obtain a hydrogenation product; and recovering caprolactam from the resulting hydrogenation product.

Abstract translation: 在减压下，通过将环己酮肟与硫酸或发烟硫酸重排而得到的不纯的己内酰胺在减压蒸馏后残留的残余物中处理回收的己内酰胺，通过在减压下蒸馏残余物，得到含己内酰胺的馏出物; 在含水介质中氢化含己内酰胺的馏出物得到氢化产物; 并从所得氢化产物中回收己内酰胺。

公开(公告)号：US4384125A

公开(公告)日：1983-05-17

申请号：US271933

申请日：1981-06-09

Applicant: Reijer Goettsch ,  Arnold G. M. Jetten

Inventor： Reijer Goettsch ,  Arnold G. M. Jetten

IPC: C07D207/26 ,  C07D201/16 ,  C07D207/267

CPC classification number: C07D201/16

Abstract: In a distillation process 2-pyrrolidones obtained from succinonitrile are purified by treating the impure liquid pyrrolidone with a strong base, fractionally distilling this product to yield, as distillate, polymerization grade purified 2-pyrrolidone, mixing the 2-pyrrolidone-containing residue from the fractional distillation with water and an acid, and extracting purified 2-pyrrolidone from the water/acid mixture. The latter purified 2-pyrrolidone products are suitable for recycling to the pyrrolidone synthesis or to make other products.

Abstract translation: 在蒸馏过程中，由琥珀腈获得的2-吡咯烷酮通过用强碱处理不纯的液体吡咯烷酮来纯化，分馏出该产物，得到作为馏出物的聚合级纯化的2-吡咯烷酮，将含2-吡咯烷酮的残留物从 用水和酸分馏，从水/酸混合物中提取纯化的2-吡咯烷酮。 后者纯化的2-吡咯烷酮产物适用于回收到吡咯烷酮合成或制备其它产物。

公开(公告)号：US4301073A

公开(公告)日：1981-11-17

申请号：US160308

申请日：1980-06-17

Applicant: Hugo Fuchs ,  Otto-Alfred Grosskinsky ,  Elmar Frommer ,  Klaus Kartte

Inventor： Hugo Fuchs ,  Otto-Alfred Grosskinsky ,  Elmar Frommer ,  Klaus Kartte

IPC: C07D201/02 ,  C07D201/16 ,  C07D223/10

CPC classification number: C07D201/16

Abstract: A process for purifying caprolactam, which has been obtained by a Beckmann rearrangement, by extracting crude caprolactam with solvents, distilling the extract in the presence of alkali, and isolating pure caprolactam, wherein, in a first stage, caprolactam is distilled from the alkaline distillation residue at a bottom temperature of 130.degree.-160.degree. C., and is recycled to the distillation stage, the residue thus obtained is distilled, in a second stage, at a bottom temperature of 140.degree.-180.degree. C., and the distillate is treated with strongly acidic agents in a third stage and is then recycled to the extraction stage.

Abstract translation: 一种通过贝克曼重排获得的己内酰胺的纯化方法，用溶剂萃取粗己内酰胺，在碱存在下蒸馏提取物，并分离纯己内酰胺，其中在第一阶段中，从碱性蒸馏中蒸馏己内酰胺 残余物在130℃-160℃的底部温度下再循环至蒸馏阶段，所得残余物在第二阶段在140-180℃的底部温度下蒸馏，馏出物 在第三阶段用强酸性剂处理，然后再循环至萃取阶段。

公开(公告)号：US4267105A

公开(公告)日：1981-05-12

申请号：US138545

申请日：1980-04-09

Applicant: Uwe Brand ,  Hugo Fuchs ,  Ruediger Schmitz

Inventor： Uwe Brand ,  Hugo Fuchs ,  Ruediger Schmitz

IPC: C07D201/04 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A process for rapidly cooling gases which contain caprolactam vapor and which have been obtained by catalytic rearrangement of cyclohexanone-oxime in the gas phase in the presence of a supported catalyst containing boric acid, wherein a finely divided coolant at from 90.degree. to 200.degree. C. is fed into a cooling zone from above, gases which are at 330.degree.-400.degree. C. and contain caprolactam vapor are introduced radially at high speed through nozzle orifices over the downstream portion of the cooling zone, and are cooled to 100.degree.-200.degree. C. by thorough mixing with the finely divided coolant, and the cooled mixture is discharged.

Abstract translation: 一种快速冷却含有己内酰胺蒸气的气体的方法，其通过在含有硼酸的负载型催化剂存在下在气相中催化重排环己酮 - 肟而得到，其中在90℃至200℃的细分散的冷却剂 从上方进入冷却区，在330〜-400℃的含有己内酰胺蒸汽的气体通过喷嘴孔径向径向高速地通过冷却区的下游部分被冷却至100℃， 通过与细分散的冷却剂充分混合，并且冷却的混合物被排出。

公开(公告)号：US4239682A

公开(公告)日：1980-12-16

申请号：US740416

申请日：1976-11-10

Applicant: Harry Danziger ,  Bernd-Ulrich Kaiser

Inventor： Harry Danziger ,  Bernd-Ulrich Kaiser

IPC: C01C1/14 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: A process for the purification of acid-containing crude caprolactam obtained by the rearrangement of cyclohexanone oxime, wherein the crude caprolactam is mixed with from 0.8 to 2.0 equivalents of a base, from 3 to 6 parts by weight of toluene, based on caprolactam and from 2 to 10 parts by weight of water, based on inorganic constituents, separating the mixture into a toluene phase and two aqueous phases the upper of which containing all contaminants and discarding this phase.

Abstract translation: 通过环己酮肟重排获得的含酸粗己内酰胺的纯化方法，其中将粗己内酰胺与0.8-2.0当量的碱混合，3至6重量份的基于己内酰胺的甲苯和 2至10重量份水，基于无机成分，将混合物分离成甲苯相和两个水相，其上部含有所有污染物并丢弃该相。

公开(公告)号：US4140685A

公开(公告)日：1979-02-20

申请号：US810568

申请日：1977-06-27

Applicant: Reijer Goettsch ,  Rudolf L. Zwart

Inventor： Reijer Goettsch ,  Rudolf L. Zwart

IPC: C01C1/24 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: The process is directed to recovering .epsilon.-caprolactam from a reaction mixture containing .epsilon.-caprolactum and sulfuric acid by separating the caprolactam from the sulfuric acid by an extraction. Extraction includes the steps of neutralizing a part of said sulfuric acid with ammonia, ammonium sulfate, ammonium hydrogen sulfate or mixture thereof, to form an ammonium salt of at least part of said sulfuric acid as a neutralization product, thermally decomposing a part of the ammonium salt formed to produce a gaseous mixture of ammonia and sulfur dioxide and contacting another portion of the neutralization product with said gaseous mixture to produce ammonium hydrogen sulfate, ammonium sulfate or both, and neutralizing at least a part of the sulfuric acid in the reaction mixture with said ammonium hydrogen sulfate, ammonium sulfate or both.

Abstract translation: 该方法涉及通过萃取从己酸内酯和己酸的反应混合物中回收ε-己内酰胺。 提取包括用氨，硫酸铵，硫酸氢铵或其混合物中和一部分硫酸的步骤，以形成至少部分所述硫酸的铵盐作为中和产物，热分解一部分铵 形成的盐以产生氨和二氧化硫的气体混合物，并使另一部分中和产物与所述气体混合物接触以产生硫酸氢铵，硫酸铵或两者，并将反应混合物中的至少一部分硫酸中和 所述硫酸氢铵，硫酸铵或两者。

公开(公告)号：US4072678A

公开(公告)日：1978-02-07

申请号：US698122

申请日：1976-06-21

Applicant: Fusao Oyama ,  Sadatomi Murao ,  Shizuo Okada

Inventor： Fusao Oyama ,  Sadatomi Murao ,  Shizuo Okada

IPC: C07D201/16 ,  B01D53/50 ,  B01D53/77 ,  C02F1/04 ,  C02F1/26 ,  C02F1/72 ,  C02F9/00 ,  C07D201/04 ,  D04H1/74 ,  F16B7/04 ,  F23G7/04

CPC classification number: D04H1/74 ,  C07D201/04 ,  D04H1/70 ,  F16B7/04 ,  B23Q2701/01 ,  B23Q2703/00 ,  Y02W10/37

Abstract: Treatment of process waste waters to be discharged from a lactam manufacturing plant by stepwise concentration in two steps under suitable conditions, extraction of lactam from the concentrate with an organic solvent, oxidative combustion of the extract residue and conversion of sulfur dioxide formed into sulfuric acid can save losses of lactams, organic solvents and sulfur containing compounds to a considerable extent and render the waste waters no longer harmful.

Abstract translation: 在合适的条件下，通过两步逐步浓缩从内酰胺制造厂排出的工艺废水的处理，用有机溶剂从浓缩物中萃取内酰胺，提取残渣的氧化燃烧和硫酸形成的二氧化硫的转化 在相当程度上节省内酰胺，有机溶剂和含硫化合物的损失，使废水不再有害。

公开(公告)号：US4054562A

公开(公告)日：1977-10-18

申请号：US261219

申请日：1972-06-09

Applicant: Herbert Furkert

Inventor： Herbert Furkert

IPC: C01B17/50 ,  C01C1/24 ,  C07D201/16 ,  C07D201/04

CPC classification number: C07D201/16 ,  C01B17/504 ,  C01C1/24 ,  Y02P20/129

Abstract: In a process for manufacturing a lactam which includes rearranging a cycloalkanone-oxime with sulfuric acid to form the lactam, neutralizing the rearrangement mixture with ammonia to form ammonium sulfate, and separating the lactam and the ammonium sulfate, the improvement which comprises:A. heating at least a portion of the ammonium sulfate to a temperature of 240.degree. - 460.degree. C to form ammonia and ammonium bisulfate;B. separating the ammonia from the ammonium bisulfate;C. recycling the ammonia to neutralize the rearrangement mixture;D. burning the ammonium bisulfate at a temperature of 850.degree. - 1250.degree. C to form an SO.sub.2 -containing gas;E. oxidizing the SO.sub.2 -containing gas to form sulfuric acid; andF. recycling the sulfuric acid to the rearrangement stage.

Abstract translation: 在制备内酰胺的方法中，其中包括用硫酸重排环烷酮肟以形成内酰胺，用氨中和重排混合物形成硫酸铵，并分离内酰胺和硫酸铵，其改进包括：