Refining process and refining system of caprolactam

    公开(公告)号:US11459302B2

    公开(公告)日:2022-10-04

    申请号:US17208073

    申请日:2021-03-22

    Abstract: A refining process includes steps of subjecting crude caprolactam to a first evaporative crystallization and a first solid-liquid separation to obtain a first caprolactam crystal and a first crystallization mother liquor; washing the first caprolactam crystal to obtain a second caprolactam crystal; optionally concentrating the first crystallization mother liquor to perform a second evaporative crystallization and a second solid-liquid separation to obtain a third caprolactam crystal and a second crystallization mother liquor; subjecting the third caprolactam crystal to a second washing to obtain a fourth caprolactam; optionally concentrating the second crystallization mother liquor to perform thermostatic crystallization, performing separation to obtain a fifth caprolactam crystal and a third crystallization mother liquor; washing the fifth caprolactam crystal to obtain a sixth caprolactam crystal; and subjecting the second caprolactam crystal to a hydrogenation reaction.

    Method for preparing caprolactam by using a microreactor under lewis acid catalysis

    公开(公告)号:US09624176B2

    公开(公告)日:2017-04-18

    申请号:US15192869

    申请日:2016-06-24

    CPC classification number: C07D223/10 Y02P20/52

    Abstract: A method for preparing caprolactam by using a microreactor under Lewis acid catalysis, wherein a hydroxyl group in a cyclohexanone oxime is activated to obtain a cyclohexanone oxime sulfonates intermediate, then rearranged under Lewis acid catalysis to prepare the caprolactam. The method of this invention has a simple process and a high operation safety and selectivity, the reaction condition is mild, an efficient reaction can take place even at room temperature, the reaction time is short, the conversion of the cyclohexanone oxime can reach 100% within a short time, the selectivity of the caprolactam can reach 99%, the energy consumption is greatly reduced in the premise of maintaining a high yield, and the production cost is reduced, being an efficient and green and environmentally friendly method of for synthesizing the caprolactam.

    Method for producing amide compound
    5.
    发明授权
    Method for producing amide compound 有权
    酰胺化合物的制备方法

    公开(公告)号:US09242931B2

    公开(公告)日:2016-01-26

    申请号:US14141867

    申请日:2013-12-27

    CPC classification number: C07D201/06 C07D201/04 C07D225/02

    Abstract: A method for producing a high purity, high quality amide compound, particularly a lactam. An amount of each of a halide, an aldehyde compound, an alcohol compound and a nitrile compound contained in a solution recycled into an oxime-forming step is controlled to an amount of 0.4 mol % or less based on the ketone as a starting material. One or more of a ketone, an oxime and an amide compound are purified by hydrogenation and/or crystallization for eliminating impurities containing a double bond. A content of impurities having a cyclic bridge structure is controlled using a cycloalkanone purified by recrystallization.

    Abstract translation: 一种生产高纯度,优质酰胺化合物,特别是内酰胺的方法。 以循环到肟形成步骤的溶液中所含的卤化物,醛化合物,醇化合物和腈化合物中的每一种的量基于作为起始原料的酮被控制为0.4摩尔%以下的量。 通过氢化和/或结晶来纯化酮,肟和酰胺化合物中的一种或多种,​​以消除含有双键的杂质。 使用通过重结晶纯化的环烷酮控制具有环状桥结构的杂质含量。

    Process for deactivating catalytically active sites on the external
surface of crystalline silicate catalysts, as well as crystalline
silicate catalysts the catalytic properties of the external surface of
which differ from those of the pore surface
    7.
    发明授权
    Process for deactivating catalytically active sites on the external surface of crystalline silicate catalysts, as well as crystalline silicate catalysts the catalytic properties of the external surface of which differ from those of the pore surface 失效
    结晶硅酸盐催化剂外表面催化活性位点失活的方法以及结晶硅酸盐催化剂,其外表面的催化性能与孔表面的催化性质不同

    公开(公告)号:US4472516A

    公开(公告)日:1984-09-18

    申请号:US467214

    申请日:1983-02-17

    Abstract: Disclosed is a method for selectively deactivating catalytically active sites which occur only on the surface of a zeolite of boralite catalyst. Active sites occurring on the interior of the pores are masked by saturating the catalyst with an organic compound which fills substantially the whole of the catalyst pore volume. The catalyst so treated is then exposed to a deactivating agent, such as a solution of an alkali metal salt which is substantially immiscible with, substantially insoluble in, and which is otherwise unreactive to said pore-filling compound. The catalyst is then treated to drive off the pore-filling compound, yielding a catalyst selectively deactivated only on the external surface, but which is not deactivated within the pores. The treatment enables the catalyst to be used for e.g. hydrocarbon conversion for long time periods without carbon buildups around the pore entrances, which buildup would otherwise either restrict entry into the pores by reactants or exit therefrom by product.

    Abstract translation: 公开了一种选择性地使仅发生在硼石催化剂的沸石表面上的催化活性位点的方法。 通过用充满基本上整个催化剂孔体积的有机化合物使催化剂饱和来掩盖在孔内部发生的活性位点。 然后将如此处理的催化剂暴露于钝化剂,例如碱性金属盐的溶液,其基本上不混溶,基本上不溶于,并且否则对所述孔填充化合物是不反应的。 然后处理催化剂以排出孔隙填充化合物,产生仅在外表面上选择性地失活的催化剂,但在孔内未失活。 该处理使得催化剂可以用于例如 碳氢化合物转化长时间没有在孔入口周围的碳积累,否则这些积聚将限制通过反应物进入孔或通过产物从其中排出。

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