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    • 1. 发明授权
    • Process for the production of pure vinyl pyrrolidone
    • 生产纯乙烯基吡咯烷酮的方法
    • US5329021A
    • 1994-07-12
    • US81947
    • 1993-02-04
    • Jeffrey M. CohenRussell B. Biss
    • Jeffrey M. CohenRussell B. Biss
    • C07D207/26C07D207/267
    • C07D207/267
    • This invention relates to a process for the purification of a crude liquid N-vinylpyrrolidone product which comprises (I) product rectification by (a) subjecting said crude product containing at least 0.3 weight % of impurities to a temperature of between about 1.degree. and 5.degree. below the freezing point of said crude liquid to form a vinyl pyrrolidone crystalline phase and a liquid residue phase in a first crystallization step; (b) separating said liquid phase from said crystalline phase; (c) allowing said separated crystalline phase to warm gradually so as to liquify said crystals and (d) subjecting the liquified crystals of vinyl pyrrolidone to between 1 and 3 additional crystallization steps, each carried out by gradually cooling the liquified vinyl pyrrolidone to a temperature above that of the preceding crystallization step up to a temperature of 14.4.degree. C. so as to form additional vinyl pyrrolidone crystalline and liquid residue phases with separation of vinyl pyrrolidone crystals and liquid residue phases and liquification of vinyl pyrrolidone crystals between each additional recrystallization step, recovery of N-vinyl-pyrrolidone product from the final crystallization step and (II) collecting said separated liquid residues from each crystallization step and subjecting them, sequentially, individually or collectively, to fractional crystallization in order to recover additional amounts of purified vinyl pyrrolidone product. The present process is capable of achieving up to 99.999% purity of vinyl pyrrolidone in about 98% recovery.
    • 本发明涉及纯液体N-乙烯基吡咯烷酮产物的纯化方法,该方法包括(I)通过(a)将含有至少0.3重量%杂质的所述粗产物处理至约1至5℃的温度来进行产物精馏 DEG低于所述粗液体的凝固点,以在第一结晶步骤中形成乙烯基吡咯烷酮结晶相和液体残余相; (b)从所述结晶相分离所述液相; (c)使所述分离的结晶相逐渐温热以使所述晶体液化,和(d)使乙烯基吡咯烷酮的液化晶体经受1至3个另外的结晶步骤,每个结晶步骤通过将液化的乙烯基吡咯烷酮逐渐冷却至温度 高于上述结晶步骤的温度至14.4℃,以便在每次附加的重结晶步骤之间分离乙烯基吡咯烷酮晶体和液体残余相并乙烯基吡咯烷酮晶体的液化形成另外的乙烯基吡咯烷酮结晶和液体残余相, 从最终结晶步骤回收N-乙烯基 - 吡咯烷酮产物,和(II)从每个结晶步骤收集所述分离的液体残余物,并依次单独或共同地对其进行分级结晶,以便回收额外量的纯化的乙烯基吡咯烷酮产物 。 本方法能够以约98%的回收率实现高达99.999%的乙烯基吡咯烷酮纯度。