公开(公告)号：US4806638A

公开(公告)日：1989-02-21

申请号：US109405

申请日：1987-10-19

申请人： Uwe Brand ,  Ruediger Schmitz ,  Ernst Deuker ,  Hugo Fuchs

发明人： Uwe Brand ,  Ruediger Schmitz ,  Ernst Deuker ,  Hugo Fuchs

IPC分类号： C07D201/04 ,  C07D201/16

CPC分类号： C07D201/16

摘要： 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).

摘要翻译： 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

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

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

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

CPC分类号： B01D53/1487 ,  B01D53/1493 ,  C07D201/16

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

摘要翻译： 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：US4350630A

公开(公告)日：1982-09-21

申请号：US276815

申请日：1981-06-25

申请人： Hugo Fuchs ,  Uwe Brand ,  Ernst Deuker ,  Elmar Frommer

发明人： Hugo Fuchs ,  Uwe Brand ,  Ernst Deuker ,  Elmar Frommer

IPC分类号： C07D201/16

CPC分类号： C07D201/16

摘要： 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.

摘要翻译： 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：US4267105A

公开(公告)日：1981-05-12

申请号：US138545

申请日：1980-04-09

申请人： Uwe Brand ,  Hugo Fuchs ,  Ruediger Schmitz

发明人： Uwe Brand ,  Hugo Fuchs ,  Ruediger Schmitz

IPC分类号： C07D201/04 ,  C07D201/16

CPC分类号： C07D201/16

摘要： 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.

摘要翻译： 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：US3992372A

公开(公告)日：1976-11-16

申请号：US560313

申请日：1975-03-20

申请人： Rudolph Hans Gath ,  Hugo Fuchs ,  Ruediger Schmitz ,  Klaus Kartte ,  Uwe Brand

发明人： Rudolph Hans Gath ,  Hugo Fuchs ,  Ruediger Schmitz ,  Klaus Kartte ,  Uwe Brand

IPC分类号： C08G69/46 ,  C07D201/16

CPC分类号： C08G69/46

摘要： A process for processing polycaprolactam extraction liquors by evaporation of water and distillation of the residue in which the evaporation of water is carried out in a plurality of stages and the evaporation energy for the removal of the bulk of the water is taken from the heat liberated in the rearrangement of cyclohexanone oxime to caprolactam in oleum or sulfuric acid by using the extraction water for cooling the rearrangement mixture and utilizing the heat absorbed by the extraction water for the concentration of this extraction water by evaporation of water.

摘要翻译： 通过蒸发水处理聚己内酰胺提取液的方法，并且蒸馏残留物，其中水的蒸发在多个阶段中进行，并且用于除去大部分水的蒸发能源取自在 通过使用提取水冷却重排混合物并利用由萃取水吸收的热量，通过蒸发水将该萃取水浓缩，将环己酮肟重排为己内酰胺在发烟硫酸或硫酸中。

公开(公告)号：US4683305A

公开(公告)日：1987-07-28

申请号：US883177

申请日：1986-07-08

申请人： Hugo Fuchs ,  Uwe Brand ,  Helmut Buchaeckert

发明人： Hugo Fuchs ,  Uwe Brand ,  Helmut Buchaeckert

IPC分类号： C07D201/12

CPC分类号： C07D201/12

摘要： Caprolactam is obtained by cleaving oligomers of caprolactam by a process in which the oligomers, in a liquid or solid state, are introduced into a fluidized alumina bed and cleaved at from 290.degree. to 400.degree. C. in the presence of steam, and, in addition to the amount of inert gas required to fluidize the alumina bed, from 0.1 to 3 times this amount of inert gas is introduced above the fluidized bed.

摘要翻译： 己内酰胺是通过以下方法裂解己内酰胺的低聚物来获得的：己内酰胺的低聚物是将液体或固体状态的低聚物引入流化的氧化铝床中，并在蒸气存在的情况下在290℃-400℃下裂解， 除了流化氧化铝床所需的惰性气体的量之外，将0.1-3倍量的惰性气体引入到流化床之上。

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：US4268440A

公开(公告)日：1981-05-19

申请号：US129827

申请日：1980-03-13

申请人： Joachim Werther ,  Hugo Fuchs ,  Uwe Brand ,  Friedrich R. Faulhaber

发明人： Joachim Werther ,  Hugo Fuchs ,  Uwe Brand ,  Friedrich R. Faulhaber

IPC分类号： C07B61/00 ,  C07D201/04

CPC分类号： C07D201/04

摘要： A process for the preparation of caprolactam wherein, in a first stage, cyclohexanone-oxime is vaporized, in the presence of inert gases, by bringing it into contact with a fluidized bed of inert solid particles at from 150.degree. to 250.degree. C., and the mixture of cyclohexanone-oxime vapor and inert gases is passed into a second stage, where the cyclohexanone-oxime is rearranged to caprolactam at from 230.degree. to 450.degree. C. over a supported catalyst, containing boron trioxide, in a fluidized bed.

摘要翻译： 一种制备己内酰胺的方法，其中在惰性气体存在下，在第一阶段将环己酮 - 肟气化，使其与150℃至250℃的惰性固体颗粒流化床接触， 并将环己酮 - 肟蒸气和惰性气体的混合物进入第二阶段，其中环己酮 - 肟在230℃至450℃下在含有三氧化硼的负载催化剂上在流化床中重排为己内酰胺。

公开(公告)号：USRE33073E

公开(公告)日：1989-09-26

申请号：US171414

申请日：1988-03-21

申请人： Hugo Fuchs ,  Uwe Brand ,  Helmut Buchaeckert

发明人： Hugo Fuchs ,  Uwe Brand ,  Helmut Buchaeckert

IPC分类号： C07D201/12

CPC分类号： C07D201/12

摘要： Caprolactam is obtained by cleaving oligomers of caprolactam by a process in which the oligomers, in a liquid or solid state, are introduced into a fluidized alumina bed and cleaved at from 290.degree. to 400.degree. C. in the presence of steam, and, in addition to the amount of inert gas required to fluidize the alumina bed, from 0.1 to 3 times this amount of inert gas is introduced above the fluidized bed.

公开(公告)号：US4248782A

公开(公告)日：1981-02-03

申请号：US78031

申请日：1979-09-24

申请人： Hugo Fuchs ,  Uwe Brand ,  Peter Horn

发明人： Hugo Fuchs ,  Uwe Brand ,  Peter Horn

IPC分类号： C07D201/04

CPC分类号： C07D201/04 ,  Y02P20/52

摘要： In a process for the preparation of .epsilon.-caprolactam by catalytic rearrangement of cyclohexanone-oxime in the gas phase at from 230.degree. to 450.degree. C. over a supported catalyst, containing boron trioxide, in a fluidized bed, wherein the catalyst is removed from the fluidized bed at the rate at which it becomes spent and is treated, in a fluidized state, with gases containing molecular oxygen at from 600.degree. to 900.degree. C., after which boron trioxide or boric acid is added to the fluidized catalyst, at from 300.degree. to 900.degree. C., before the catalyst is returned to the fluidized bed, the improvement that boron trioxide or boric acid of particle size from 0.05 to 1.5 mm is fed to the fluidized catalyst at one or more points.

摘要翻译： 在通过在230℃至450℃的气相中催化重排环己酮 - 肟在含有三氧化硼的载体催化剂的流化床中制备ε-己内酰胺的方法，其中将催化剂从 流化床以其流失的速率以流化状态处理含有分子氧的气体在600-900℃，之后将三氧化硼或硼酸加入到流化催化剂中，在 在催化剂返回到流化床之前，从300℃升至900℃，改善将粒径为0.05-1.5mm的三氧化硼或硼酸以一个或多个点进料到流化催化剂中。