公开(公告)号：US4138472A

公开(公告)日：1979-02-06

申请号：US844647

申请日：1977-10-25

申请人： Gerald Neubauer ,  Gerard Van Wauwe ,  Josef Beullens ,  Uwe Brand ,  Hugo Fuchs ,  Klaus Kartte

发明人： Gerald Neubauer ,  Gerard Van Wauwe ,  Josef Beullens ,  Uwe Brand ,  Hugo Fuchs ,  Klaus Kartte

IPC分类号： C01C1/242 ,  C01C1/248

CPC分类号： C01C1/242 ,  C01C1/248

摘要： A process for obtaining coarsely crystalline pure ammonium sulfate from reaction mixtures which have been obtained by Beckmann rearrangement of cyclohexanone-oxime with sulfuric acid or oleum, by neutralizing the mixtures with ammonia at an elevated temperature, with the addition of recycled ammonium sulfate mother liquor, the concentration being so chosen that during the neutralization no solid ammonium sulfate precipitates, separating the crude caprolactam from the ammonium sulfate solution, crystallizing ammonium sulfate by evaporating the ammonium sulfate solution under reduced pressure, separating off the crystallized ammonium sulfate and recycling the mother liquor to the neutralization stage. The neutralization is carried out at from 80.degree. to 115.degree. C. under autogenous pressure and the ammonium sulfate solution obtained after separating off the crude lactam is evaporated under a pressure of from 200 to 600 mm Hg while cooling to from 72.degree. to 101.degree. C.

摘要翻译： 从反应混合物中获得粗结晶纯硫酸铵的方法，其通过用硫酸或发烟硫酸重整环己酮 - 肟，通过在升高的温度下用氨中和混合物，再加入回收的硫酸铵母液， 浓度如此选择，使得在中和期间没有固体硫酸铵沉淀，将粗己内酰胺与硫酸铵溶液分离，通过在减压下蒸发硫酸铵溶液使硫酸铵结晶，分离结晶的硫酸铵并将母液再循环至 中和阶段。 中和在自生压力下在80〜115℃进行，分离出内酰胺后得到的硫酸铵溶液在200〜600mmHg的压力下蒸发，同时冷却至72〜101℃。 C。

公开(公告)号：US4804754A

公开(公告)日：1989-02-14

申请号：US130949

申请日：1987-12-10

申请人： Emile De Decker ,  Jozef Oostvogels ,  Gerard van Wauwe ,  Gerald Neubauer

发明人： Emile De Decker ,  Jozef Oostvogels ,  Gerard van Wauwe ,  Gerald Neubauer

IPC分类号： C07D201/04 ,  C07D201/16

CPC分类号： C07D201/04

摘要： Caprolactam is prepared in a process comprising(a) a Beckmann rearrangement of cyclohexanone oxime with oleum at from 70.degree. to 130.degree. C. in one or more rearrangement stages, and(b) aftertreatment of the reaction mixture obtained from the rearrangement stage in a delay zone at from 70.degree. to 110.degree. C. for from 10 to 600 minutes.

摘要翻译： 在一个方法中制备己内酰胺，该方法包括（a）在一个或多个重排阶段中，环己酮肟与发烟硫酸在发酵油中的贝克曼重排在70〜130℃，（b）后处理从重排阶段获得的反应混合物 延迟区为70〜110℃，时间为10〜600分钟。