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    • 2. 发明授权
    • Preparation of .epsilon.-caprolactone
    • ε-己内酯的制备
    • US4341709A
    • 1982-07-27
    • US150260
    • 1980-05-15
    • Willi HofenHerbert KlenkGerd SchreyerOtto WeibergHelmut WaldmannHermann SeifertKarl-Hermann ReissingerWolfgang Swodenk
    • Willi HofenHerbert KlenkGerd SchreyerOtto WeibergHelmut WaldmannHermann SeifertKarl-Hermann ReissingerWolfgang Swodenk
    • C07D313/04C07D315/00C07D313/02
    • C07D315/00
    • A process for the preparation of .epsilon.-caprolactone comprising:(a) reacting cyclohexanone with a solution of perpropionic acid in an organic solvent at a molar ratio of cyclohexanone;perpropionic acid of about 1.1-5:1 at a temperature of about 10.degree. to 80.degree. C. to form a reaction mixture consisting essentially of .epsilon.-caprolactone, propionic acid and organic solvent,(b) distilling the reaction mixture from (a) in a first distillation unit to obtain a distillate comprising the organic solvent and a distillation residue,(c) introducing the distillation residue from (b) at a point into a second distillation unit to obtain a distillate comprising propionic acid and unreacted cyclohexanone, removing from the second distillation unit, separately from one another and at a point below the point of introduction into the second distillation unit, .epsilon.-caprolactone and any high-boiling constituents, and,(d) distilling in a third distillation unit the distillate from (c) to obtain a distillate consisting essentially of propionic acid and a distillation residue comprising a mixture of propionic acid and cyclohexanone.
    • 一种制备ε-己内酯的方法,包括:(a)使环己酮与过丙酸在有机溶剂中的溶液以环己酮的摩尔比约1.1-5:1的约0.1〜5:1的摩尔比在约10℃〜 形成基本上由ε-己内酯,丙酸和有机溶剂组成的反应混合物,(b)在第一蒸馏单元中将反应混合物从(a)中蒸馏,得到包含有机溶剂和蒸馏残余物的馏出物 (c)在一点将来自(b)的蒸馏残余物引入第二蒸馏单元以获得包含丙酸和未反应的环己酮的馏出物,从第二蒸馏单元彼此分离并在低于 引入第二蒸馏装置,ε-己内酯和任何高沸点组分,和(d)在第三蒸馏装置中蒸馏出馏出物(c)得到 基本上由丙酸组成的馏出物和包含丙酸和环己酮的混合物的蒸馏残渣。
    • 3. 发明授权
    • Process for the manufacture of very pure .epsilon.-caprolactone
    • 用于制造非常纯的ε-己内酯的方法
    • US4313879A
    • 1982-02-02
    • US179622
    • 1980-08-20
    • Herbert KlenkRolf WirthweinGerd SiekmannWulf Schwerdtel
    • Herbert KlenkRolf WirthweinGerd SiekmannWulf Schwerdtel
    • C07D313/04C07D315/00
    • C07D315/00
    • The invention relates to a process for the production of .epsilon.-caprolactone having a purity of 99.9% and increased color and storage stability which comprises feeding .epsilon.-caprolactone, which has been made by reacting cyclohexanone with a solution of a percarboxylic acid, into a first distillation unit, operating at 0.1 to 500 mbars and drawing off as the top product a mixture consisting of .epsilon.-caprolactone and lower-boiling impurities, feeding the bottom product of said first distillation unit into a second distillation unit, operating at 0.1 to 500 mbars and then drawing off the pure .epsilon.-caprolactone as the top product. The .epsilon.-caprolactone is useful as an intermediate for the production of known useful compounds such as polyesterols which are subsequently converted to polyurethanes.
    • 本发明涉及一种生产纯度为99.9%,颜色和储存稳定性提高的ε-己内酯的方法,包括将环己酮与过羧酸反应制得的ε-己内酯进料到第一 蒸馏单元,操作为0.1至500mbar,并作为顶部产物抽出由ε-己内酯和低沸点杂质组成的混合物,将所述第一蒸馏单元的底部产物进料到第二蒸馏单元中,操作为0.1至500mbar 然后取出纯ε-己内酯作为顶级产品。 ε-己内酯可用作生产已知有用化合物如聚酯的中间体,随后将其转化为聚氨酯。