公开(公告)号：US4806638A

公开(公告)日：1989-02-21

申请号：US109405

申请日：1987-10-19

Applicant: Uwe Brand ,  Ruediger Schmitz ,  Ernst Deuker ,  Hugo Fuchs

Inventor： Uwe Brand ,  Ruediger Schmitz ,  Ernst Deuker ,  Hugo Fuchs

IPC: C07D201/04 ,  C07D201/16

CPC classification number: C07D201/16

Abstract: Reaction mixtures obtained by Beckmann rearrangement of cyclohexanone oxime with sulfuric acid or oleum are neutralized by a process which comprises the following steps:(a) mixing the reaction mixture with recycled ammonium sulfate mother liquor whose concentration is chosen so that no solid ammonium sulfate is precipitated during the neutralization,(b) neutralization by feeding gaseous ammonia which contains water or an aqueous ammonium sulfate solution in finely divided liquid form through a plurality of nozzle orifices into the solution of the reaction mixture in the ammonium sulfate mother liquor at elevated temperatures,(c) separation of crude lactam from the aqueous ammonium sulfate solution,(d) evaporation of the ammonium sulfate solution under reduced pressure and with separation of the crystalline ammonium sulfate from the ammonium sulfate mother liquor and(e) recycling of the ammonium sulfate mother liquor to stage a).

Abstract translation: 通过包含以下步骤的方法中和通过Beckmann重排环己酮肟与硫酸或发烟硫酸得到的反应混合物：（a）将反应混合物与其浓度选择为不使固体硫酸铵沉淀的再循环硫酸铵母液混合 在中和期间，（b）通过将高分子液体形式的含有水或硫酸铵水溶液的气态氨通过多个喷嘴孔送入反应混合物在硫酸铵母液的溶液中，在升高的温度下中和（b） c）将粗内酰胺与硫酸铵水溶液分离，（d）在减压下蒸发硫酸铵溶液，并从硫酸铵母液中分离结晶硫酸铵，和（e）将硫酸铵母液 到a）。

公开(公告)号：US4804473A

公开(公告)日：1989-02-14

申请号：US136418

申请日：1987-12-22

Applicant: Uwe Brand ,  Emile DeDecker ,  Ernst Deuker ,  Hugo Fuchs ,  Klaus Kartte ,  Gerald Neubauer ,  Jozef Oostvogels

Inventor： Uwe Brand ,  Emile DeDecker ,  Ernst Deuker ,  Hugo Fuchs ,  Klaus Kartte ,  Gerald Neubauer ,  Jozef Oostvogels

IPC: B01D53/44 ,  B01D53/14 ,  B01D53/34 ,  B01D53/72 ,  B01D53/77 ,  C07D201/16 ,  B01D11/04

CPC classification number: B01D53/1487 ,  B01D53/1493 ,  C07D201/16

Abstract: Water-immiscible solvents are removed from offgases containing same by washing with water-containing caprolactam.

Abstract translation: 通过用含水己内酰胺洗涤除去与水相混溶的溶剂。

公开(公告)号：US4767856A

公开(公告)日：1988-08-30

申请号：US133274

申请日：1987-12-15

Applicant: Toni Dockner ,  Manfred Sauerwald ,  Rolf Fischer ,  Hans-Martin Hutmacher ,  Claus-Ulrich Priester ,  Uwe Vagt

Inventor： Toni Dockner ,  Manfred Sauerwald ,  Rolf Fischer ,  Hans-Martin Hutmacher ,  Claus-Ulrich Priester ,  Uwe Vagt

IPC: C07D201/08 ,  C07D201/16

CPC classification number: C07D201/08

Abstract: In an improved process for preparing caprolactam by heating 6-aminocaproic acid, an ester or amide or mixture thereof in the presence of an inert reaction medium which is liquid under the reaction conditions and has a boiling point above that of caprolactam, the improvement comprises using as the reaction medium a hydrocarbon, maintaining a temperature of from 150.degree. to 350.degree. C., charging the 6-aminocaproic acid, ester, amide or mixture thereof at a rate commensurate with their rate of conversion, and separating caprolactam from the reaction mixture at a rate commensurate with its rate of formation.

Abstract translation: 在通过在反应条件下为液体并且沸点高于己内酰胺的惰性反应介质的惰性反应介质的存在下加热6-氨基己酸，酯或酰胺或其混合物来制备己内酰胺的改进方法中，改进包括使用 作为反应介质，将烃保持在150℃至350℃的温度下，以与其转化速率相称的速率加入6-氨基己酸，酯，酰胺或其混合物，并将己内酰胺与反应混合物分离 其速度与其形成速度相称。

公开(公告)号：US4350630A

公开(公告)日：1982-09-21

申请号：US276815

申请日：1981-06-25

Applicant: Hugo Fuchs ,  Uwe Brand ,  Ernst Deuker ,  Elmar Frommer

Inventor： Hugo Fuchs ,  Uwe Brand ,  Ernst Deuker ,  Elmar Frommer

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: In a process for continuously extracting caprolactam from an aqueous solution, containing caprolactam and its oligomers, with organic solvents, by introducing the aqueous solution into the upper part of an extraction zone and organic solvents into the lower part, and taking off a solution of caprolactam in organic solvents at the upper end and an aqueous phase containing caprolactam oligomers at the lower end, the improvement that liquid aromatic hydrocarbons are used and the extraction is carried out at a pH of from 2.0 to 6.0.

Abstract translation: 在从有机溶剂中含有己内酰胺及其低聚物的水溶液中连续提取己内酰胺的方法中，通过将水溶液引入提取区的上部，将有机溶剂引入下部，并将己内酰胺 在上端的有机溶剂和下端含有己内酰胺低聚物的水相中，使用液态芳烃的改进，并且在2.0至6.0的pH下进行萃取。

公开(公告)号：US4328154A

公开(公告)日：1982-05-04

申请号：US203367

申请日：1980-11-03

Applicant: Paolo Senni ,  Mario Catoni ,  Domenico Astarita

Inventor： Paolo Senni ,  Mario Catoni ,  Domenico Astarita

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A process for the purification of raw caprolactam obtained by extraction h alkylated phenols from its sulphuric solution, re-extraction with water, oxidation preferably with KMnO.sub.4, evaporation of water and distillation, comprises, before the oxidation treatment, a "fast distillation", in the presence of an alkali. The oxidation is conducted at 0.degree.-80.degree. C. and at atmospheric pressure with 0.005-0.5% by weight of KMnO.sub.4. The amount of alkali (NaOH) used in the fast distillation is comprised between 0.05 and 0.5% by weight.

Abstract translation: 通过从其硫酸溶液中用烷基化酚萃取得到的己内酰胺的纯化方法，用水重新萃取，优选用KMnO 4进行氧化，蒸发水和蒸馏，在氧化处理之前包括“快速蒸馏” 碱的存在。 氧化在0〜80℃，大气压下进行，重量为0.005〜0.5％的KMnO4。 在快速蒸馏中使用的碱（NaOH）的量为0.05-0.5重量％。

公开(公告)号：US4326925A

公开(公告)日：1982-04-27

申请号：US122675

申请日：1980-02-19

Applicant: Paolo Senni ,  Domenico Astarita

Inventor： Paolo Senni ,  Domenico Astarita

IPC: C07D201/16 ,  B01D3/34

CPC classification number: C07D201/16

Abstract: A process for purifying caprolactame by continuous and/or discontinuous (oratch) vacuum distillation comprises a first stage fast vacuum distillation of the raw caprolactame possibly in the presence of an alkaline and/or alkaline-earth hydroxide, a second stage consisting of a vacuum rectification distillation of the caprolactame obtained in the first stage and a third stage consisting of the fast vacuum distillation of the caprolactame yielded from the second stage, in the presence of an alkaline and/or alkaline-earth hydroxide. The hydroxide amount in the third and possibly the first stage distillation as well varies from 0.05 to 5% preferably from 0.1% to 1%.

Abstract translation: 通过连续和/或不连续（或分批）真空蒸馏纯化己内酰胺的方法包括可能在碱性和/或碱土金属氢氧化物存在下的原始己内酰胺的第一阶段快速真空蒸馏，第二阶段由真空 在第一阶段获得的己内酰胺的精馏蒸馏和由碱和/或碱土金属氢氧化物存在下由第二阶段产生的己内酰胺的快速真空蒸馏组成的第三阶段。 在第三阶段和可能的第一阶段蒸馏中的氢氧化物量也为0.05至5％，优选为0.1％至1％。

公开(公告)号：US4314940A

公开(公告)日：1982-02-09

申请号：US142860

申请日：1980-04-21

Applicant: Paolo Senni ,  Nando Toderi

Inventor： Paolo Senni ,  Nando Toderi

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A method for the purification of raw caprolactam containing primary amidesf the formula ##STR1## wherein R is a hydrocarbon radical having 1-14 carbon atoms is described. The raw caprolactam is treated with at least one compound containing at least one hydroxyl group, in an amount of at least 20% by weight with respect to the raw caprolactam, at a temperature equal to or higher than that at which the ammonia, which is a part of the amide of formula I, is liberated. The caprolactam is then separated and isolated from the hydroxyl containing compound by known methods.

Abstract translation: 描述了含有其中R为具有1-14个碳原子的烃基的式（Ⅰ）的伯酰胺的原始己内酰胺的纯化方法。 在等于或高于氨的温度下，将至少一种含有至少一个羟基的化合物与至少20重量％的量相对于原己内酰胺一起处理， 一部分式I的酰胺被释放出来。 然后通过已知方法将己内酰胺分离并从含羟基化合物中分离。

公开(公告)号：US4248781A

公开(公告)日：1981-02-03

申请号：US78028

申请日：1979-09-24

Applicant: Peter Horn ,  Hugo Fuchs

Inventor： Peter Horn ,  Hugo Fuchs

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A process for purifying crude caprolactam which has been obtained by rearrangement of cyclohexanone-oxime in the gas phase over a catalyst containing boron trioxide, wherein caprolactam is crystallized out, by cooling, from a melt which contains, per 100 parts by weight of crude caprolactam, from 5 to 30 parts by weight of primary alkanols or fatty acids which have a carbon chain of 6 to 10 carbon atoms and are substituted by alkyl radicals of 1 to 5 carbon atoms, and from 0 to 5 parts by weight of water, and is separated from the mother liquor.

Abstract translation: 一种纯化己内酰胺纯化方法，该方法是通过在含有三氧化硼的催化剂上，在气相中重排环己酮 - 肟而得到的，其中己内酰胺通过冷却从含有每100份重量的己内酰胺 ，5〜30重量份具有碳原子数为6〜10个碳原子并且被1〜5个碳原子的烷基取代的伯烷醇或脂肪酸，0〜5重量份的水，以及 与母液分离。

公开(公告)号：US4148792A

公开(公告)日：1979-04-10

申请号：US915732

申请日：1978-06-15

Applicant: Harry Danziger ,  Otto Immel ,  Bernd-Ulrich Kaiser ,  Guido Rampart ,  Hans-Helmut Schwarz

Inventor： Harry Danziger ,  Otto Immel ,  Bernd-Ulrich Kaiser ,  Guido Rampart ,  Hans-Helmut Schwarz

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: A process for the purification of .epsilon.-caprolactam, wherein .epsilon.-caprolactam is treated with potassium permanganate in the presence of from 0.01 to 5% by weight of water, based on caprolactam, and subsequently crystallized from toluene, benzene, ethylbenzene or xylene.

Abstract translation: 用于纯化ε-己内酰胺的方法，其中ε-己内酰胺在高碱性高锰酸盐存在下，在0.01至5重量％的水的存在下，以己内酰胺为基础，随后在甲苯，苯，乙苯或二甲苯中结晶。

公开(公告)号：US4133810A

公开(公告)日：1979-01-09

申请号：US871005

申请日：1978-01-20

Applicant: Willem J. Wassen ,  Rudolf L. Zwart

Inventor： Willem J. Wassen ,  Rudolf L. Zwart

IPC: C07D201/16

CPC classification number: C07D201/16

Abstract: An improvement of processes for the recovery of .epsilon.-caprolactam wherein a neutralized sulfuric acid is subjected to thermal decomposition, forming a gaseous mixture of ammonia and sulfur dioxide which is thereafter converted to an aqueous solution of ammonium sulfite and/or ammonium hydrogen sulfite which is then used for neutralization of the reaction mixture of lactam and sulfuric acid.

Abstract translation: 改进ε-己内酰胺回收方法，其中中和的硫酸经受热分解，形成氨和二氧化硫的气体混合物，然后转化成亚硫酸氢铵和/或亚硫酸氢铵的水溶液，其为 然后用于中和内酰胺和硫酸的反应混合物。