Recovery of caprolactam from caprolactam-containing distillation residue
    141.
    发明授权
    Recovery of caprolactam from caprolactam-containing distillation residue 失效
    从含己内酰胺的蒸馏残余物中回收己内酰胺

    公开(公告)号:US4563308A

    公开(公告)日:1986-01-07

    申请号:US643026

    申请日:1984-08-21

    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。

    Process for the rapid cooling of gases which contain caprolactam vapor
    142.
    发明授权
    Process for the rapid cooling of gases which contain caprolactam vapor 失效
    快速冷却含有己内酰胺蒸气的气体的方法

    公开(公告)号:US4267105A

    公开(公告)日:1981-05-12

    申请号:US138545

    申请日:1980-04-09

    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。

    Process for the manufacture of lactams
    144.
    发明授权
    Process for the manufacture of lactams 失效
    内酰胺的制造工艺

    公开(公告)号:US4054562A

    公开(公告)日:1977-10-18

    申请号:US261219

    申请日:1972-06-09

    Inventor: Herbert Furkert

    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:

    Process for preparing lactams
    145.
    发明授权
    Process for preparing lactams 失效
    制备内酰胺的方法

    公开(公告)号:US3991047A

    公开(公告)日:1976-11-09

    申请号:US608249

    申请日:1975-08-27

    CPC classification number: C07D201/04

    Abstract: In a process for the preparation of lactam from cycloalkanone comprising reacting said alkanone with hydroxylamine sulfate to form the corresponding cycloalkanone oxime followed by Beckman rearrangement to yield said lactam and neutralization of the sulfuric acid formed by ammonia whereby ammonium sulfate is formed as a byproduct, the improvement which comprises reacting said ammonium sulfate with an alkaline-earth metal oxide or hydroxide to form an alkaline earth metal sulfate and ammonia, heating said alkaline-earth metal sulfate to decompose it into said alkaline-earth metal oxide and sulfur dioxide and/or sulfur trioxide, converting said sulfur dioxide and/or sulfur trioxide into sulfuric acid, whereby said sulfuric acid and said ammonia are capable of reuse in said process.

    Abstract translation: 在由环烷酮制备内酰胺的方法中,包括使所述烷酮与硫酸羟胺反应形成相应的环烷酮肟,然后进行贝克曼重排,得到所述内酰胺并中和由氨形成的硫酸,由此形成副产物硫酸铵。 改进包括使所述硫酸铵与碱土金属氧化物或氢氧化物反应以形成碱土金属硫酸盐和氨,加热所述碱土金属硫酸盐以将其分解成所述碱土金属氧化物和二氧化硫和/或硫 三氧化硫,将所述二氧化硫和/或三氧化硫转化为硫酸,由此所述硫酸和所述氨能够在所述方法中再利用。

    Process for the preparation of omega laurinolactame
    146.
    发明授权
    Process for the preparation of omega laurinolactame 失效
    制备OMEGA LAURINOLACTAME的方法

    公开(公告)号:US3825532A

    公开(公告)日:1974-07-23

    申请号:US19232771

    申请日:1971-10-26

    Inventor: KERN R POULAIN C TOCK F

    CPC classification number: C07D201/04

    Abstract: A PROCESS FOR REARRANGING CYCLODODECANONEOXIME INTO PURE CYCLODODECALACTAME, CHARACTERIZED BY THE FACT THAT THE OXIME, CONVERTED INTO OXIME CHLORHYDRATE, IS MADE INTO A SOLUTION WITH A SELECTIVE SOLVENT, IN THE PRESENCE OF A SMALL QUANTITY OF CATALYST, CHOSEN FROM THE GROUP OF ACID HALIDES AND OXYHALIDES, AND THEN HEATED TO A TEMPERATURE OF BETWEEN 65 AND 110* C. FOR ONE TO TWO HOURS, THE RESULTING HYDROCHLORIC ACID IS DRAWN OFF BY MEANS OF A FLOW OF GAS WHILE MAINTAINING THE REFLUX TEMPERATURE OF THE SOLVENT, THE REACTION MIXTURE IS WASHED WHILE HOT WITH AN ALKALINE AQUEOUS SOLUTION, THE ORGANIC PHASE CONTAINING THE LACTAME IS WASHED IN HOT WATER UNTIL BECOMES NEUTRAL, AND THE LACTAME IS RECOVERED BY CRYSTALLIZATION OR DISTILLATION OF THE SOLVENT. THE QUANTITY OF CATALYST USED RANGES FROM 0.5 TO 5%, AND PREFERABLY 1 TO 2%, OF THE WEIGHT OF OXIME. THE SOLVENT IS PREFERABLY SELECTED FROM ALKANES, CYCLOALKANES, SUBSTITUTED ALKANE AND CYCLOALKANE DERIVATIVES, AND HALOGENATED ALKANE AND CYCLOALKANE DERIVATIVES.

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