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    • 5. 发明授权
    • Process for the preparation of di(amino phenyl)methanes
    • 制备二(氨基苯基)甲烷的方法
    • US4039581A
    • 1977-08-02
    • US590801
    • 1975-06-27
    • Floro F. FrullaAdnan A. R. SayighHenri UlrichPeter J. Whitman
    • Floro F. FrullaAdnan A. R. SayighHenri UlrichPeter J. Whitman
    • C08G12/00C07C67/00C07C209/00C07C209/54C07C209/60C07C209/78C07C211/50C08G12/08C08G73/02C07C85/08
    • C08G73/02C07C209/24C07C209/54C07C263/10C08G12/08
    • Aniline and formaldehyde are condensed (2-10 moles aniline per mole of formaldehyde) at ambient temperature in the absence of acid catalysts to give a mixture of aminals (anilinoacetals) and aniline from which the water is removed. The anhydrous aminals are contacted with a solid catalyst (clays, zeolites, diatomaceous earth) using either batch or continuous operation initially at 20.degree. C to 55.degree. C until benzylamine formation is substantially complete, then at 50.degree. C to 65.degree. C until benzylamine conversion to methylene polyphenyl polyamines is 75 - 90% complete and finally at 80.degree. C to 100.degree. C. A polyamine mixture is obtained in which diaminodiphenylmethane is the major (order of 90 percent by weight or higher) component, the bulk of the higher oligomeric polyamines being triamine. The diaminodiphenylmethane component contains of the order of 85 percent of 4,4'-isomer, the rest being 2,4'-isomer except for very small amounts (order of 2 percent or less) of 2,2'-isomer.Advantages of the process include high yield of diaminodiphenylmethane with relatively high 4,4'-isomer content, low oligomeric polyamine content, low temperature operation (energy consumption lower), no acidic reactants to cause corrosion of equipment, and rapid rates of conversion.
    • 在不存在酸催化剂的情况下,在环境温度下,苯胺和甲醛缩合(每摩尔甲醛为2-10摩尔苯胺),得到除去水的胺(苯胺基缩醛)和苯胺的混合物。 使用间歇或连续操作,在20℃至55℃下使无水胺与固体催化剂(粘土,沸石,硅藻土)接触,直到苄胺形成基本完成,然后在50℃至65℃下直至苄胺 转化为亚甲基多苯基多胺的组合物为75-90%,最后在80℃至100℃。得到多胺混合物,其中二氨基二苯基甲烷为主要成分(90%重量或更高) 低聚多胺是三胺。 二氨基二苯基甲烷组分含有约为85%的4,4'-异构体,其余为2,4'-异构体,只是非常少量(2%或更低的量级)的2,2'-异构体。