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    • 1. 发明授权
    • Process for preparing 1,6 hexanediol with a level of purity over 99%
    • 制备纯度超过99%的1,6己二​​醇的方法
    • US6008418A
    • 1999-12-28
    • US125976
    • 1998-08-28
    • Karl Gerhard BaurRolf FischerRolf PinkosFrank SteinHarald RustBoris Breitscheidel
    • Karl Gerhard BaurRolf FischerRolf PinkosFrank SteinHarald RustBoris Breitscheidel
    • B01J23/80B01J23/889C07B61/00C07C29/149C07C31/20
    • C07C29/149
    • 1,6-Hexanediol is prepared from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as a by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol by water extraction of the reaction mixture, by esterification of the acids and hydrogenation whereina) the monocarboxylic and dicarboxylic acids present in the aqueous dicarboxylic acid mixture are reacted with a low molecular weight alcohol to give the corresponding carboxylic esters,b) the resulting esterification mixture is freed of excess alcohol and low boilers in a first distillation stage,c) the bottoms are fractionated in a second distillation stage to give an ester fraction essentially free of 1,4-cyclohexanediols and a fraction comprising at least the major part of the 1,4-cyclohexanediols,d) the ester fraction essentially free of 1,4-cyclohexanediols is catalytically hydrogenated ande) in a pure distillation stage, 1,6-hexanediol is isolated from the hydrogenation product in a manner known per se.
    • PCT No.PCT / EP97 / 00980 Sec。 371日期1998年8月28日 102(e)1998年8月28日PCT PCT 1997年2月28日PCT公布。 公开号WO97 / 31882 日期1991年9月4日6,6-己二醇由包含己二酸,6-羟基己酸和少量1,4-环己二醇的羧酸混合物制备,其作为副产物在环己烷氧化成环己酮/ 环己醇通过水提取反应混合物,通过酸的酯化和氢化,其中存在于二羧酸水溶液混合物中的单羧酸和二羧酸与低分子量醇反应得到相应的羧酸酯,b)得到的 酯化混合物在第一蒸馏阶段中不含过量的醇和低沸点,c)在第二蒸馏阶段对塔底物进行分馏,得到基本上不含1,4-环己烷二醇的酯馏分和至少包含至少大部分 1,4-环己烷二醇,d)基本上不含1,4-环己烷二醇的酯馏分是催化氢化的,e)在纯蒸馏阶段, 以本身已知的方式从加氢产物中分离出1,6-己二醇。
    • 3. 发明授权
    • Continuous preparation of alkyl esters of (meth) acrylic acid
    • 连续制备(甲基)丙烯酸的烷基酯
    • US5734074A
    • 1998-03-31
    • US618817
    • 1996-03-20
    • Toni DocknerHerbert ExnerKarl Gerhard BaurChristiane Potthoff
    • Toni DocknerHerbert ExnerKarl Gerhard BaurChristiane Potthoff
    • C07C67/08C07C69/52
    • C07C67/08
    • The continuous esterification of a C.sub.1 -C.sub.8 -alkanol with (meth)acrylic acid in a molar ratio of from 1:1 to 2:1 in the presence of proton-donating catalysts in a homogeneous, liquid, solvent-free phase, in which the water of reaction and resulting alkyl (meth)acrylate are separated off continuously as part of an aqueous azeotropic mixture via the top of a rectification zone attached to the reaction zone, at a top pressure of from 0.1 to 1 atm, and worked up to give pure (meth)acrylate, is carried out by a process wherein the reaction temperature is from 100.degree. to 150.degree. C., the residence time is from 1 to 5 hours and from 5 to 20% by weight, based on the amount of reaction mixture, of sulfuric acid or an equimolar amount, based on such an amount of sulfuric acid, of an organic sulfonic acid is added as a protic acid catalyst to the reaction mixture present in the reaction zone.
    • 在质子递送催化剂存在下,在均相,液体,无溶剂相中,C1-C8-链烷醇与(甲基)丙烯酸的摩尔比为1:1至2:1的连续酯化,其中 反应水和得到的(甲基)丙烯酸烷基酯作为水性共沸混合物的一部分经由连接到反应区的精馏区的顶部,在0.1至1atm的最高压力下连续分离,并加热至 得到纯的(甲基)丙烯酸酯,其反应温度为100〜150℃,停留时间为1〜5小时,5〜20重量%,以 加入作为质子酸催化剂的硫酸或等摩尔量的基于这样量的硫酸的有机磺酸的反应混合物加入存在于反应区中的反应混合物。