Preparation of crystalline hydroxylammonium sulfate having a low
ammonium sulfate content
    3.
    发明授权
    Preparation of crystalline hydroxylammonium sulfate having a low ammonium sulfate content 失效
    制备硫酸铵含量低的结晶羟基硫酸铵

    公开(公告)号:US4997635A

    公开(公告)日:1991-03-05

    申请号:US521031

    申请日:1990-05-09

    IPC分类号: C01B21/14

    CPC分类号: C01B21/1472

    摘要: Crystalline hydroxylammonium sulfate is prepared by a process which comprises the following steps:(a) Bringing an aqueous solution which contains from 0.02 to 0.3 part by weight of ammonium sulfate and from 0.02 to 0.2 part by weight of sulfuric acid per part by weight of hydroxylammonium sulfate into contact with a basic ion exchanger and obtaining a solution which has a pH of from 3.0 to 4.0,(b) separating off the basic ion exchanger from the aqueous hydroxylammonium sulfate solution,(c) evaporating down the resulting aqueous hydroxylammonium sulfate solution under reduced pressure at

    摘要翻译: 通过包括以下步骤的方法制备结晶羟基硫酸铵:(a)将含有0.02至0.3重量份硫酸铵和0.02至0.2重量份硫酸的水溶液相对于每重量份的羟基铵 硫酸盐与碱性离子交换剂接触,得到pH为3.0〜4.0的溶液,(b)从羟基硫酸铵水溶液中分离碱式离子交换剂,(c)将所得的羟基硫酸铵水溶液 在<100℃下减压,得到浓硫酸羟基铵溶液,(d)结晶出不超过70重量%的存在于水溶液中的羟基硫酸铵,得到结晶羟基硫酸铵和母液,(e )从母液中分离和结晶的羟基硫酸铵。

    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。

    Recovery of caprolactam from polycaprolactam
    8.
    发明授权
    Recovery of caprolactam from polycaprolactam 失效
    从己内酰胺中回收己内酰胺

    公开(公告)号:US5359062A

    公开(公告)日:1994-10-25

    申请号:US54064

    申请日:1993-04-29

    IPC分类号: C07D201/12 C08G69/14

    CPC分类号: C07D201/12

    摘要: Caprolactam is recovered from polycaprolactam by hydrolyric cleavage of polycaprolactam with from 5 to 50 parts by weight of water per part by weight of polycaprolactam at from 200.degree. to 350.degree. C. under superatmospheric pressure to give an aqueous solution or suspension which contains monomeric caprolactam and oligomers thereof and may contain polycaprolactam and subsequent isolation of monomeric caprolactam from the aqueous solution or suspension by distillation or extraction, by a process in which the hydrolyric cleavage is carried out in the presence of an alkali metal hydroxide at a pH of from 5 to 10.

    摘要翻译: 己内酰胺通过在超大气压下在200-350℃下用5至50重量份的重量比的聚己内酰胺水解裂解聚己内酰胺从聚己内酰胺中回收,得到含有单体己内酰胺和 其低聚物并且可以含有聚己内酰胺并随后通过蒸馏或萃取从水溶液或悬浮液中分离单体己内酰胺,其中水解裂解在pH为5至10的碱金属氢氧化物存在下进行 。

    Work-up of aqueous mother liquors containing hydrochloric acid, sulfuric
acid and their hydroxyl-ammonium and ammonium salts
    9.
    发明授权
    Work-up of aqueous mother liquors containing hydrochloric acid, sulfuric acid and their hydroxyl-ammonium and ammonium salts 失效
    含有氢氯酸,硫酸及其羟基铵和氨基铵的水性母液的加工

    公开(公告)号:US5124138A

    公开(公告)日:1992-06-23

    申请号:US631155

    申请日:1990-12-20

    CPC分类号: C01B21/1472 C02F1/26

    摘要: A process for working up aqueous mother liquors containing hydrochloric acid, sulfuric acid and their hydroxylammonium and ammonium salts, entails the mother liquors being intimately mixed with an excess of cyclohexanone based on the content of hydroxylammonium salts, while maintaining a pH of from 3 to 5.5 by adding alkali metal hydroxide solutions, and the cyclohexanone phase which contains cyclohexanone oxime being removed and washed with water until essentially free of chloride.

    摘要翻译: 处理含有盐酸,硫酸及其羟基铵和铵盐的含水母液的方法需要使母液基于羟基铵盐的含量与过量的环己酮充分混合,同时保持pH为3至5.5 通过加入碱金属氢氧化物溶液和除去环己酮肟的环己酮相,并用水洗涤至基本上不含氯化物。

    Recovery of caprolactam from caprolactam distillation low boilers or
high boilers or mixtures thereof
    10.
    发明授权
    Recovery of caprolactam from caprolactam distillation low boilers or high boilers or mixtures thereof 失效
    从己内酰胺蒸馏低沸点锅炉或高锅炉或其混合物中回收己内酰胺

    公开(公告)号:US4882430A

    公开(公告)日:1989-11-21

    申请号:US257274

    申请日:1988-10-13

    IPC分类号: C07D201/16

    CPC分类号: C07D201/16

    摘要: Caprolactam is recovered from caprolactam distillation low boilers or high boilers or mixtures thereof by the following steps:(a) crystallizing a low or high boiler or a mixture thereof to form purified capro-lactam crystals and a mother liquor,(b) separating off the purified caprolactam crystals to leave a mother liquor,(c) recycling from 5 to 90% by weight of the mother liquor of stage (b) into stage (a) and transferring the remainder of the mother liquor into the subsequent stage (d),(d) crystallizing the remaining mother liquor portion from stage (c) to form caprolactam crystals and a mother liquor, separating off the caprolactam crystals of stage(e) (d) and recycling the same into stage (a) to leave a mother liquor,(f) recycling from 20 to 99% by weight of mother liquor of stage (e) into stage (d) and channeling out the remainder of the impurity-containing mother liquor of stage (e).

    摘要翻译: 通过以下步骤从己内酰胺蒸馏低锅炉或高锅炉或其混合物回收己内酰胺:(a)使低或高锅炉或其混合物结晶以形成纯化的己内酰胺结晶和母液,(b)将 纯化的己内酰胺晶体离开母液,(c)将阶段(b)的母液的5至90重量%循环到阶段(a)中,并将剩余的母液转移到后续阶段(d)中, (d)从阶段(c)中将剩余的母液部分结晶以形成己内酰胺晶体和母液,分离阶段(e)(d)的己内酰胺晶体并将其再循环到阶段(a)中以留下母液 ,(f)将阶段(e)的母液的20至99重量%循环到阶段(d)中,并且引出阶段(e)的含杂质母液的剩余部分。