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    • 6. 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
    • US06072076A
    • 2000-06-06
    • US789542
    • 1997-01-27
    • Willi SchmidtMatthias GeisendorferAlexander WeckToni DocknerHolger HerbstGerhard Nestler
    • Willi SchmidtMatthias GeisendorferAlexander WeckToni DocknerHolger HerbstGerhard Nestler
    • B01J31/02C07B61/00C07C67/08C07C67/54C07C69/54C07C69/52
    • C07C67/08
    • In a process for the continuous preparation of alkyl esters of (meth)acrylic acid by reacting (meth)acrylic acid with alkanols having from 1 to 8 carbon atoms in a homogeneous, liquid, solvent-free phase at elevated temperature and in the presence of an acid esterification catalyst, in which the (meth)acrylic acid, the alkanol and the acid catalyst are fed to a reaction zone, the water formed is removed by rectification during a residence time as constituent of a mixture comprising starting alkanol in a rectification unit (III) superposed on the reaction zone, the distillate obtained is separated into an organic phase comprising alkanol and an aqueous phase comprising water, the organic phase is essentially completely returned to the rectification unit (III), the reaction mixture is discharged from the reaction zone and conveyed into a distillative separation zone comprising further rectification units and in the latter the alkyl (meth)acrylate formed is separated off.a) (Meth)acrylic acid and alkanol are reacted in a molar ratio of from 1:0.75 to 1:2, b) part of the aqueous phase obtained at the top of the rectification unit (III) is returned to the rectification unit, c) the reaction mixture discharged from the reaction zone is fed to a further rectification unit (I) and in this the reaction mixture is separated into a product (II) comprising the catalyst and a product (I) comprising the alkyl ester of (meth)acrylic acid, remaining alkanol and remaining (meth)acrylic acid, and d) the product (I) is fed to a further rectification unit (II) and in this the alkyl ester of (meth)acrylic acid is separated from the remaining alkanol and from the remaining (meth)acrylic acid and the remaining alkanol and the remaining (meth)acrylic acid are returned to the reaction zone.
    • 在(甲基)丙烯酸的烷基酯的连续制备方法中,通过使(甲基)丙烯酸与具有1至8个碳原子的链烷醇在均相,液体,无溶剂相中在升高的温度下和在 将(甲基)丙烯酸,链烷醇和酸催化剂进料到反应区中的酸酯化催化剂,在停留时间内通过精馏除去形成的水,作为在精馏单元中起始烷醇的混合物的组分 (III),将获得的馏出物分离成包含链烷醇和含水的水相的有机相,有机相基本上完全返回到精馏单元(III),将反应混合物从反应物中排出 并输送到包含进一步精馏单元的蒸馏分离区中,后者分离形成的(甲基)丙烯酸烷基酯。 a)(甲基)丙烯酸和链烷醇的摩尔比为1:0.75至1:2,b)将在精馏单元(III)顶部获得的部分水相返回至精馏单元, c)将从反应区排出的反应混合物加入到另一精馏单元(I)中,并将反应混合物分离成包含催化剂的产物(II)和包含(甲基)丙烯酸烷基酯的产物(I) )丙烯酸,残留的链烷醇和剩余的(甲基)丙烯酸,以及d)将产物(I)加入到另一精馏单元(II)中,在此将(甲基)丙烯酸的烷基酯与剩余的链烷醇 和剩余的(甲基)丙烯酸和剩余的链烷醇和剩余的(甲基)丙烯酸返回到反应区。