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    • 5. 发明授权
    • Removal of cyclohexanol from aqueous solutions containing it and
aromatic sulfonic acids
    • 从含有它的水溶液和芳族磺酸中除去环己醇
    • US4982018A
    • 1991-01-01
    • US400530
    • 1989-08-30
    • Hans-Juergen GoschRolf FischerHermann Luyken
    • Hans-Juergen GoschRolf FischerHermann Luyken
    • B01J31/34C07B61/00C07C27/00C07C29/04C07C29/80C07C29/84C07C35/08C07C67/00
    • C07C29/80C07C2101/14
    • Cyclohexanol is removed from aqueous solutions containing it and aromatic sulfonic acids, obtained by hydrating cyclohexene in aqueous solutions of aromatic sulfonic acids at elevated temperatures and subsequent removal of excess cyclohexene, by(a) feeding the aqueous solution which contains the cyclohexanol and the aromatic sulfonic acid into the upper third of a first column and from 1 to 50 parts by weight of steam per part by weight of cyclohexanol into the bottom third of the column, withdrawing at the top of the column a vapor which consists essentially of cyclohexanol, cyclohexene and water, and obtaining as a bottom product an aqueous solution of the aromatic sulfonic acid,(b) condensing the vapor which consists essentially of cyclohexanol, cyclohexene and water and(b1) obtaining a cyclohexanol-rich phase and(b2) an aqueous phase,(c) utilizing the aqueous phase (b2) for generating the steam required in stage (a) and any remainder for the hydration of cyclohexene, and(d) distilling off from the cyclohexanol-rich phase (b1) in a second column a mixture of cyclohexene and water with or without cyclohexanol as top product, leaving cyclohexanol as bottom product.
    • 通过(a)将含有环己醇和芳香族磺酸的水溶液进料,将环己醇从含有它的水溶液和芳族磺酸中除去,通过在高温下将环己烯在芳族磺酸的水溶液中水合并随后除去过量的环己烯而得到 酸进入第一塔的上三分之一,并且每重量份1至50重量份的环己醇的环己醇至塔的底部三分之一,在塔的顶部抽出基本上由环己醇,环己烯和 水,并且作为底部产物获得芳族磺酸的水溶液,(b)使基本上由环己醇,环己烯和水组成的蒸气冷凝,和(b1)获得富含环己醇的相和(b2)水相, (c)使用水相(b2)产生阶段(a)中所需的蒸汽和用于环己烯水合的任何剩余物,和(d)d 在第二列中从环己醇富含相(b1)中除去环己醇和水的混合物,其中有或没有环己醇作为顶部产物,留下环己醇作为底部产物。
    • 7. 发明授权
    • Separation of 1,4-butanediol from hydrogenation mixtures
    • 从氢化混合物中分离出1,4-丁二醇
    • US5342488A
    • 1994-08-30
    • US18496
    • 1993-02-17
    • Hans-Juergen GoschHarald RustRolf FischerClaus HechlerRolf Pinkos
    • Hans-Juergen GoschHarald RustRolf FischerClaus HechlerRolf Pinkos
    • C07C29/80C07C29/82C07C31/20B01D3/00C07C27/00
    • C07C29/80Y10S203/20
    • A process for the separation of 1,4-butanediol from mixtures obtained by the catalytic hydrogenation of maleates, fumarates, and/or succinates, which also contain tetrahydrofuran, water, C.sub.1 -C.sub.4 alcohols, succinic diesters, hydroxybutyrates, alkylhydroxyalkyl succinates, gamma-butyrolactone and butyrates, in addition to 1,4-butanediol, comprising the following steps:a) separating, in a first column having an actual number of plates of from 20 to 70 and operated at a top pressure of from 50 to 1100 mbar and preferably from 50 to 500 mbar and a top temperature of from 40.degree. to 120.degree. C., alcohol, water and tetrahydrofuran, as overhead product,b) feeding the bottom product of the first column into a second column having an actual number of plates of from 30 to 90 and withdrawing the overhead product consisting of alcohol and butyrate and obtained at a top pressure of from 45 to 250 mbar and a top temperature of from 45.degree. to 120.degree. C., and withdrawing gamma-butyrolactone and butyrates through a side outlet, and feeding the bottom product to a phase separator,c) feeding the 1,4-butanediol-enriched bottom phase of the liquid two-phase mixture coming from the phase separator to a third column having an actual number of plates of from 30 to 90, alcohol being distilled off as overhead product at a top pressure of from 45 to 250 mbar and a top temperature of from 45.degree. to 120.degree. C., and the azeotrope comprising 1,4 -butanediol and succinic diester is withdrawn as a sidestream and recycled to the phase separator, whilst 1,4-butanediol is removed together with alkyl-hydroxyalkyl succinate, butyl hydroxybutyrate, and high-boiling fractions as bottoms, andd) separating the succinate-enriched top phase in the phase separator.
    • 还含有四氢呋喃,水,C 1 -C 4醇,琥珀酸二酯,羟基丁酸酯,琥珀酸烷基羟基烷基酯,γ-丁内酯和/或琥珀酸酯的马来酸盐,富马酸盐和/或琥珀酸盐的催化氢化得到的混合物的分离方法, 丁内酯和丁酸酯除了1,4-丁二醇外还包括以下步骤:a)在具有20至70的实际板数的第一塔中分离并在50至1100毫巴的最高压力下操作,以及 优选为50至500毫巴,顶部温度为40至120℃,醇,水和四氢呋喃作为塔顶产物,b)将第一塔的底部产物进料到具有实际数量的板的第二塔 30至90份,并取出由醇和丁酸盐组成的塔顶产物,并在顶部压力为45至250毫巴,顶部温度为45至120℃下获得,并将γ-丁内酯和丁酸酯 通过侧出口将底部产物供给到相分离器中,c)将来自相分离器的液体两相混合物的富含1,4-丁二醇的底相进料到具有实际数量的板的第三塔 为30至90,在顶部压力为45至250毫巴,顶部温度为45至120℃的条件下,蒸馏出作为塔顶产物的醇,由1,4-丁二醇和琥珀酸二酯组成的共沸物为 作为侧流回收并循环到相分离器中,而1,4-丁二醇与琥珀酸烷基 - 羟基烷基酯,羟基丁酸丁酯和作为塔底产物的高沸点馏分一起除去,以及d)在相中分离富含琥珀酸酯的顶相 分隔器。