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    • 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
    • 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。
    • 6. 发明授权
    • Preparation of (meth)acrylates
    • (甲基)丙烯酸酯的制备
    • US06512138B1
    • 2003-01-28
    • US09567983
    • 2000-05-10
    • Albrecht DamsHeinrich AichingerHolger HerbstGerhard NestlerJürgen Schröder
    • Albrecht DamsHeinrich AichingerHolger HerbstGerhard NestlerJürgen Schröder
    • C07C6952
    • C07C67/08C07C67/327C07C69/54
    • The process for the esterification of (meth)acrylic acid with an alkanol in the presence of an esterification catalyst, in which unconverted starting compounds and the (meth)acrylate to be formed are separated off by distillation and an oxyester-containing bottom product is formed and is separated off, and (a) in the bottom product separated off, the oxyesters present are cleaved, if required after the addition of (meth)acrylic acid and/or oligomeric (meth)acrylic acid, directly in the presence of acid catalysts differing from (meth)acrylic acid and/or oligomeric (meth)acrylic acid, and the cleavage products are removed, a cleavage residue remaining, or (b) the oxyesters are first removed by distillation from the cleavage product separated off, a distillation residue remaining, and the oxyesters removed are cleaved, if required after addition of (meth)acrylic acid and/or oligomeric (meth)acrylic acid, in the presence of acid catalysts differing from (meth)acrylic acid and/or oligomeric (meth)acrylic acid, and the cleavage products are removed, a cleavage residue remaining, is carried out in such a way that the cleavage residue obtained in step (a) or the cleavage residue obtained in step (b) is hydrolytically cleaved together with the resulting distillation residue in the presence of water and acids or bases.
    • 在酯化催化剂存在下,(甲基)丙烯酸与烷醇的酯化反应的方法,其中未转化的起始化合物和待形成的(甲基)丙烯酸酯通过蒸馏和含有含氧酯的底部产物分离出来 并分离出来,(a)在分离出的底部产物中,如果需要,在酸催化剂存在下直接加入(甲基)丙烯酸和/或低聚(甲基)丙烯酸后,存在的氧化酯被切割 与(甲基)丙烯酸和/或低聚(甲基)丙烯酸不同,除去裂解产物,剩余的裂解残余物或(b)氧酯首先通过蒸馏从分离的裂解产物中除去,蒸馏残余物 除去(甲基)丙烯酸和/或低聚(甲基)丙烯酸之外,如果需要,在不同于(甲基)丙烯酸和/或低聚(甲基)丙烯酸的酸催化剂的存在下, 甲基)丙烯酸,并且去除裂解产物,残留切割残余物,使得步骤(a)中获得的裂解残基或步骤(b)中获得的裂解残基与 在水和酸或碱的存在下产生蒸馏残余物。