Process for obtaining coarsely crystalline pure ammonium sulfate
    1.
    发明授权
    Process for obtaining coarsely crystalline pure ammonium sulfate 失效
    获得粗结晶纯硫酸铵的方法

    公开(公告)号:US4138472A

    公开(公告)日:1979-02-06

    申请号:US844647

    申请日:1977-10-25

    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。

    Continuous extraction of caprolactam from crude lactam
    3.
    发明授权
    Continuous extraction of caprolactam from crude lactam 失效
    从内酰胺连续提取己内酰胺

    公开(公告)号:US4154729A

    公开(公告)日:1979-05-15

    申请号:US848210

    申请日:1977-11-03

    IPC分类号: C07D201/16

    CPC分类号: C07D201/16

    摘要: In a process for the continuous extraction of caprolactam from crude lactam by means of benzene in counter-current, in which crude lactam is fed into the upper part of an extraction zone and benzene into the lower part, a solution of caprolactam in benzene is taken off at the top and an aqueous solution containing impurities is taken off at the bottom, the improvement that water is additionally fed into the upper part of the extraction zone and a part of the aqueous solution, containing impurities, obtained at the bottom of the extraction zone is recycled into the extraction zone. Caprolactam is used for the manufacture of nylon.

    摘要翻译: 在将粗制内酰胺进料到提取区上部并进入下部的苯中,通过逆流中的苯从粗制内酰胺连续提取己内酰胺的方法,将己内酰胺在苯中的溶液 在底部取出含有杂质的水溶液,改善了将水另外进料到提取区的上部,并将部分含有杂质的水溶液在提取物的底部获得 区域被回收到提取区域。 己内酰胺用于制造尼龙。

    Processing polycaprolactam extraction liquors
    4.
    发明授权
    Processing polycaprolactam extraction liquors 失效
    加工聚己内酰胺提取液

    公开(公告)号:US3992372A

    公开(公告)日:1976-11-16

    申请号:US560313

    申请日:1975-03-20

    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。

    Purification of caprolactam
    5.
    发明授权
    Purification of caprolactam 失效
    己内酰胺的纯化

    公开(公告)号:US4301073A

    公开(公告)日:1981-11-17

    申请号:US160308

    申请日:1980-06-17

    CPC分类号: C07D201/16

    摘要: 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.

    摘要翻译: 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。

    Partial dehydration of cyclohexanone oxime
    6.
    发明授权
    Partial dehydration of cyclohexanone oxime 失效
    环己酮肟部分脱水

    公开(公告)号:US3941838A

    公开(公告)日:1976-03-02

    申请号:US438167

    申请日:1974-01-30

    CPC分类号: C07C249/14

    摘要: A process for the partial dehydration of cyclohexanone oxime by treatment with aqueous solutions of inorganic salts, wherein the crude cyclohexanone oxime is extracted, above its melting point, with a concentrated ammonium salt solution and/or hydroxylammonium salt solution in countercurrent in an extraction column and the salt solution is then separated from the partly dehydrated cyclohexanone oxime, reconcentrated by evaporation and recycled to the oxime dehydration process. The cyclohexanone oxime melt which has been dehydrated to water contents of about 4 to 6% by weight is treated with a heated inert gas above its melting point and the off-gas is washed to remove entrained cyclohexanone oxime.

    摘要翻译: 一种通过用无机盐的水溶液处理来环己酮肟部分脱水的方法,其中将粗环己酮肟在其熔点以上提取,浓缩的铵盐溶液和/或羟基铵盐溶液在提取塔中逆流, 然后将盐溶液与部分脱水的环己酮肟分离,通过蒸发浓缩并再循环至肟脱水过程。 已经脱水至约4〜6重量%的含水量的环己酮肟熔体用高于其熔点的加热惰性气体处理,并将废气洗涤以除去夹带的环己酮肟。

    Recovery of caprolactam from oligomers and/or polymers of caprolactam
    7.
    发明授权
    Recovery of caprolactam from oligomers and/or polymers of caprolactam 失效
    从己内酰胺的低聚物和/或聚合物中回收己内酰胺

    公开(公告)号:US5700358A

    公开(公告)日:1997-12-23

    申请号:US396623

    申请日:1995-03-01

    CPC分类号: C07D201/12 C07D201/16

    摘要: Caprolactam is recovered from oligomers and/or polymers of caprolactam by cleavage of oligomers and/or polymers of caprolactam and subsequent working up by distillation of the caprolactam obtained in the cleavage, by a process including (a) cleaving oligomers and/or polymers of caprolactam to obtain an aqueous reaction mixture which contains caprolactam, (b) removing water from the reaction mixture obtained under (a) to obtain a residue, (c) distilling the residue obtained under (b) in an acidic medium and (d) then distilling the distillate in an alkaline medium to obtain caprolactam, or (c') distilling the residue obtained under (b) in an alkaline medium and (d') then distilling the distillate in an acidic medium to obtain caprolactam.

    摘要翻译: 通过裂解己内酰胺的低聚物和/或聚己内酯并随后通过蒸馏在切割中获得的己内酰胺来处理己内酰胺从己内酰胺的低聚物和/或聚合物中回收己内酰胺,方法包括(a)裂解己内酰胺的低聚物和/或聚合物 得到含有己内酰胺的水性反应混合物,(b)从(a)得到的反应混合物中除去水,得到残渣,(c)将酸性介质中的(b)得到的残渣蒸馏,然后蒸馏 在碱性介质中的馏出物得到己内酰胺,或(c')将在(b)获得的残余物在碱性介质中蒸馏,然后(d'),然后在酸性介质中蒸馏出馏出物,得到己内酰胺。

    Preparation of caprolactam
    9.
    发明授权
    Preparation of caprolactam 失效
    己内酰胺的制备

    公开(公告)号:US4268440A

    公开(公告)日:1981-05-19

    申请号:US129827

    申请日:1980-03-13

    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。