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    • 7. 发明授权
    • Method for purifying trimethylolpropane, which is produced by hydrogenation, by means of continuous distillation
    • 通过连续蒸馏通过氢化制备三羟甲基丙烷的方法
    • US06692616B2
    • 2004-02-17
    • US10168980
    • 2002-06-26
    • Matthias DernbachDetlef KratzAchim StammerHarald RustGerhard Schulz
    • Matthias DernbachDetlef KratzAchim StammerHarald RustGerhard Schulz
    • B01D314
    • C07C29/80C07C31/225C07C31/12C07C31/245C07C31/04
    • A process is disclosed for the purification, by distillation, of trimethylolpropane originating from the hydrogenation of 2,2-dimethylolbutanal, said process including the following steps: (a) reaction of n-butyraldehyde with formaldehyde in the presence of catalytic amounts of a tertiary amine, and hydrogenation of the resulting mixture to give a mixture containing trimethylolpropane; (b) separation of water, methanol, trialkylamine and/or trialkylammonium formate by distillation; (c) heating of the residue obtained in (b) under reduced pressure to a temperature at which TMP is volatile and compounds boiling above TMP are cleaved, in order to separate off, by distillation, TMP and compounds more volatile than TMP; (d) distillation of the distillate obtained in (c) in order to separate off the more volatile compounds and recover pure TMP; and (e) optional distillation of the TMP obtained in (d) in order to recover TMP with a low APHA color index. A process is also disclosed in which trialkylammonium formate is distilled under mild conditions from crude mixtures of polyhydric alcohols, predominantly trimethylolpropane.
    • 公开了一种通过蒸馏纯化来自2,2-二羟甲基丁烷的氢化的三羟甲基丙烷的方法,所述方法包括以下步骤:(a)在催化量的叔碳酸存在下,正丁醛与甲醛的反应 胺,并氢化得到的混合物,得到含有三羟甲基丙烷的混合物;(b)通过蒸馏分离水,甲醇,三烷基胺和/或三烷基铵甲酸盐;(c)将(b)中得到的残余物在减压下加热至 TMP挥发的温度和TMP沸点高的化合物被切割,以便通过蒸馏分离TMP和比TMP更易挥发的化合物;(d)蒸馏(c)中获得的馏出物,以分离出更多的 挥发性化合物,回收纯TMP; 为了回收具有低APHA颜色指数的TMP,还可以任选地蒸馏(d)中获得的TMP。还公开了一种方法,其中在温和条件下从多元醇,主要是三羟甲基丙烷的粗混合物中蒸馏出三烷基铵甲酸盐。
    • 8. 发明授权
    • Method for producing polyalcohols
    • 生产多元醇的方法
    • US06187971B1
    • 2001-02-13
    • US09331370
    • 1999-06-21
    • Detlef KratzAchim StammerGerhard SchulzGuido Voit
    • Detlef KratzAchim StammerGerhard SchulzGuido Voit
    • C07C3118
    • C07C45/75C07C29/141Y02P20/582C07C31/04C07C31/12C07C31/125C07C31/20C07C31/22
    • Methylolalkanal of the formula II (R=CH2OH, C1-C22-alkyl, aryl or C6-C22-aralkyl) is prepared spe-wise by a) reacting a C2-C24-aldehyde with formaldehyde in the presence of a tertiary amine, b) separating the reaction mixture i) into a bottom fraction comprising the compound of formula II and an incompletely methylolated compound of the formula III and a distillate stream comprising unconverted or partially converted starting materials, or ii) into an aqueous phase and an organic phase, and recycling the distillate stream or the organic phase to a), and c) subjecting the bottom fraction or the aqueous phase i) to a catalytic or thermal reaction to convert the compound of formula III to the compound of formula II and to a corresponding methylene compound of formula IV (R′=H or R) and ii) separating the reaction product into an overhead stream comprising the compound of formula IV and unconverted formaldehyde which is recycled to a), and a bottom fraction comprising the compound of formula II.
    • 在叔胺存在下,通过使C2-C24-醛与甲醛反应制备式II的(C 1 -C 22 - 烷基,芳基或C 6 -C 22 - 芳烷基)的羟甲基烷醛,b) 将反应混合物分离)至包含式II化合物的底部馏分和式III的不完全羟甲基化的化合物和包含未转化的或部分转化的起始物质的馏出物流,或ii)进入水相和有机相,并将馏出物 流或有机相至a),和c)使底部馏分或水相)进行催化或热反应以将式III化合物转化为式II化合物和相应的式IV的亚甲基化合物(R '= H或R)和ii)将反应产物分离成包含式IV化合物和未转化甲醛的塔顶物流,将其再循环至a),以及包含式II化合物的塔底馏分。