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    • 2. 发明授权
    • Process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas
    • 基本上不含无甲酸的N-烷基-N'-甲基亚烷基脲的方法
    • US06554966B1
    • 2003-04-29
    • US09603195
    • 2000-06-26
    • Andreas KramerJohann-Peter MelderHeinz RütterGünter RieweWolfgang SiegelHans-Jürgen Weyer
    • Andreas KramerJohann-Peter MelderHeinz RütterGünter RieweWolfgang SiegelHans-Jürgen Weyer
    • B01D300
    • C07D239/10
    • The invention relates to a process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas of the formula with R1=H or CH3, R2=CnH2n+1 with n=1-4 and x=0 or 1, from the corresponding alkyleneureas by reaction with monomeric or polymerized formaldehyde in the presence of formic acid. This entails feeding the mixture, obtained in the reaction, of N-alkyl-N′-methylalkyleneurea and formic acid to the upper region of a distillation column, distilling without further additions and removing essentially formic acid-free N-alkyl-N′-methylalkyleneurea in the lower region of the column. The process parameters are set so that the pressure in the upper region of the column is at a higher level than in the lower region of the column, and the difference in pressure between the upper and lower regions of the column is from 10 to 100 mbar, and the temperature in the lower region of the column is higher than in the upper region of the column, with the difference in temperature between the upper and lower regions of the column being from 40° C. to 210° C.
    • 本发明涉及一种制备基本上无甲酸的N-烷基-N'-甲基亚烷基脲的方法,其中R1 = H或CH3,R2 = CnH2n + 1,其中n = 1-4和x = 0或1, 通过在甲酸存在下与单体或聚合的甲醛反应来制备相应的亚烷基脲。 这需要将N-烷基-N'-甲基亚烷基脲和甲酸的反应混合物加入到蒸馏塔的上部区域,无需进一步添加即可蒸馏除去基本上不含甲酸的N-烷基-N'- 甲基亚烷基脲在柱的下部区域。 设定工艺参数使得塔的上部区域中的压力处于比塔的下部区域更高的水平,并且塔的上部和下部区域之间的压力差为10至100mbar ,塔的下部区域的温度高于塔的上部区域,塔的上部和下部区域之间的温度差为40℃〜210℃。