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    • 5. 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
    • Aqueous phase process for preparing N-substituted imidazoles
    • 制备N-取代咪唑的水相方法
    • US5877326A
    • 1999-03-02
    • US914187
    • 1997-08-19
    • Gisela HieberKlaus EbelJurgen SchroderToni DocknerCarsten GroningBernd Ruge
    • Gisela HieberKlaus EbelJurgen SchroderToni DocknerCarsten GroningBernd Ruge
    • C07D233/58B01J21/12B01J27/16C07D233/54C07D233/68C07D233/90C07D233/91C07D233/92C07D235/06C07D235/08C07D233/56
    • C07D235/08C07D233/54C07D233/56C07D233/64C07D233/68C07D233/90C07D233/91C07D233/92C07D235/06
    • A process for preparing substituted imidazoles of the formula I ##STR1## R.sup.1, R.sup.2 and R.sup.3 are identical or different and are each hydrogen, halogen, NO.sub.2, CN or a C.sub.1 -C.sub.20 -hydrocarbon radical which is unsubstituted or substituted by one or more halogens or R.sup.1 and R.sup.2 together are members of a 3- to 20-membered hydrocarbon ring which is unsubstituted or substituted by one or more halogens and/or C.sub.1 -C.sub.8 -alkyl groups and which may contain 1, 2 or 3 heteroatoms from the group consisting of nitrogen, oxygen and sulfur, andR.sup.4 is a C.sub.1 -C.sub.20 -hydrocarbon radical which is unsubstituted or substituted by one or more halogens,comprises using an aqueous phase of the imidazoles of the formula II ##STR2## where R.sup.1, R.sup.2 and R.sup.3 are as defined above with compounds of the formula IIIR.sup.4 --O--R.sup.5 IIIwhereR.sup.4 is as defined above andR.sup.5 is hydrogen or R.sup.4, it being possible in the latter case for the two R.sup.4 substituents to be identical or different,and reacting it at from 200.degree. to 550.degree. C. in the presence of a catalyst comprising oxides and/or phosphates of one or more metals of the 2nd, 3rd and 4th main group and the 4th subgroup of the Periodic Table in the presence or absence of phosphoric acid and/or phosphoric esters.
    • 制备式I的取代咪唑的方法R1,R2和R3相同或不同,各自为氢,卤素,NO2,CN或C1-C20-烃基,其未被取代或被一个或多个 卤素或R 1和R 2一起是3至20元烃环的成员,其未被取代或被一个或多个卤素和/或C 1 -C 8烷基取代,并且可以含有1,2或3个来自该基团的杂原子 由氮,氧和硫组成,R4是未被取代或被一个或多个卤素取代的C 1 -C 20烃基,包括使用式II的咪唑的水相,其中R 1,R 2和 R 3如上所定义,与式III的R4-O-R5III化合物,其中R 4如上定义,R 5是氢或R 4,在后一种情况下,两个R 4取代基可以相同或不同, 在约200℃〜550℃下, 在磷酸和/或磷酸酯存在或不存在的条件下,包含第2,第3和第4主族和第4族的周期表中的一种或多种金属的氧化物和/或磷酸盐。
    • 10. 发明授权
    • Preparation of acylated imidazoles
    • 酰化咪唑的制备
    • US4924000A
    • 1990-05-08
    • US321110
    • 1989-03-09
    • Michael HesseWolfgang HoelderichToni DocknerHermann Koehler
    • Michael HesseWolfgang HoelderichToni DocknerHermann Koehler
    • B01J21/00B01J21/04B01J21/06B01J21/08B01J23/20B01J27/18B01J29/04C07B61/00C07D233/54C07D233/64
    • C07D233/64
    • Acylated imidazoles of the formula ##STR1## where R.sup.1 and R.sup.3 are each H, alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, R.sup.4 is H, alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, and R.sup.5 is alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl, alkylaryl or carboxyl, are prepared by reacting imidazoles of the formula ##STR2## where R.sup.1, R.sup.2 and R.sup.3 are each alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, at least one of the radicals R.sup.1, R.sup.2 and R.sup.3 being hydrogen, and R.sup.4 is H, alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, with widely used acylating agents of the formula ##STR3## where R.sup.5 is as defined above and Y is halide, alkoxy, acyloxy or hydroxyl, in the presence of acidic metal oxides and/or phosphates, preferably in the gas phase.
    • 其中R 1和R 3各自为H,具有1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,R 4为H,1至12的烷基, 碳原子,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,R5是1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基,烷基芳基或羧基, 使式(Ia)的咪唑与R1,R2和R3各自为1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,基团R1,R2和 R3为氢,R4为H,1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,以及广泛使用的通式为“IMAGE”的酰化剂,其中R5如上定义 在酸性金属氧化物和/或磷酸盐的存在下,优选在气相中,Y是卤化物,烷氧基,酰氧基或羟基。