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    Continuous preparation of alkyl esters of (meth)acrylic acid
    1.
    发明授权
    Continuous preparation of alkyl esters of (meth)acrylic acid 失效
    连续制备（甲基）丙烯酸的烷基酯

    公开(公告)号：US5883288A

    公开(公告)日：1999-03-16

    申请号：US791052

    申请日：1997-01-28

    申请人： Gabriele Iffland ,  Albrecht Dams ,  Alexander Weck ,  Heinrich Aichinger ,  Holger Herbst ,  Gerhard Nestler ,  Herbert Exner ,  Willi Schmidt ,  Matthias Geisendorfer ,  Toni Dockner

    发明人： Gabriele Iffland ,  Albrecht Dams ,  Alexander Weck ,  Heinrich Aichinger ,  Holger Herbst ,  Gerhard Nestler ,  Herbert Exner ,  Willi Schmidt ,  Matthias Geisendorfer ,  Toni Dockner

    IPC分类号： B01J27/02 ,  B01J31/02 ,  C07B61/00 ,  C07C67/08 ,  C07C67/54 ,  C07C69/54 ,  C07C69/52

    CPC分类号： C07C67/08

    摘要： In the process for the continuous preparation of alkyl esters of (meth)acrylic acid by reacting (meth)acrylic acid with monohydric alkanols having from 1 to 8 carbon atoms in the presence of an acid esterification catalyst in a reaction zone, there is discharged from the reaction zone a product mixture which comprises the alkyl (meth)acrylate formed, the catalyst and the by-products formed during the course of the esterification having boiling points higher than that of the alkyl (meth)acrylate, and from which the alkyl (meth)acrylate is separated by distillation in a separation zone. The product mixture discharged from the reaction zone is fed to a rectification unit (I), in this unit the product mixture discharged is separated by rectification into at least one product (I) comprising the alkyl ester of (meth)acrylic acid and a product (II) comprising the catalyst, the product (I) is fed to a further rectification unit (II) and in this the alkyl ester of (meth)acrylic acid is separated off by rectification.

    摘要翻译： 在反应区酸性酯化催化剂存在下，使（甲基）丙烯酸与具有1〜8个碳原子的一元链烷醇反应连续制备（甲基）丙烯酸烷基酯的方法中， 所述反应区包含形成的（甲基）丙烯酸烷基酯，在酯化过程中形成的催化剂和副产物的沸点高于（甲基）丙烯酸烷基酯的产物混合物，并且烷基（ 甲基）丙烯酸酯在分离区中蒸馏分离。 将从反应区排出的产物混合物供给到精馏单元（I），在该单元中，排出的产物混合物通过精馏分离成至少一种包含（甲基）丙烯酸的烷基酯的产物（I）和产物 （II），将产物（I）进料到另一精馏单元（II）中，通过精馏分离（甲基）丙烯酸的烷基酯。

    Continuous preparation of alkyl esters of (meth)acrylic acid
    2.
    发明授权
    Continuous preparation of alkyl esters of (meth)acrylic acid 失效
    连续制备（甲基）丙烯酸的烷基酯

    公开(公告)号：US06072076A

    公开(公告)日：2000-06-06

    申请号：US789542

    申请日：1997-01-27

    申请人： Willi Schmidt ,  Matthias Geisendorfer ,  Alexander Weck ,  Toni Dockner ,  Holger Herbst ,  Gerhard Nestler

    发明人： Willi Schmidt ,  Matthias Geisendorfer ,  Alexander Weck ,  Toni Dockner ,  Holger Herbst ,  Gerhard Nestler

    IPC分类号： B01J31/02 ,  C07B61/00 ,  C07C67/08 ,  C07C67/54 ,  C07C69/54 ,  C07C69/52

    CPC分类号： C07C67/08

    摘要： 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.

    摘要翻译： 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。

    Separation of a diester of (meth)acrylic acid with a C.sub.4 -C.sub.6 -alkanediol
    4.
    发明授权
    Separation of a diester of (meth)acrylic acid with a C.sub.4 -C.sub.6 -alkanediol 失效
    （甲基）丙烯酸的二酯与C4-C6-链烷二醇的分离

    公开(公告)号：US5663421A

    公开(公告)日：1997-09-02

    申请号：US541703

    申请日：1995-10-10

    申请人： Toni Dockner ,  Helmut Lermer ,  Ulrich Rauh ,  Gerhard Nestler

    发明人： Toni Dockner ,  Helmut Lermer ,  Ulrich Rauh ,  Gerhard Nestler

    IPC分类号： C07C57/07 ,  C07C67/08 ,  C07C67/58 ,  C07C69/54 ,  C07C67/48

    CPC分类号： C07C67/58

    摘要： A diester of (meth)acrylic acid with a C.sub.4 -C.sub.6 -alkanediol is separated from a mixture which essentially consists of the C.sub.4 -C.sub.6 -alkanediol, the monoester of (meth)acrylic acid with the C.sub.4 -C.sub.6 -alkanediol and the diester of (meth)acrylic acid with the C.sub.4 -C.sub.6 -alkanediol by extraction with an organic solvent in the presence of water, by a process in which the diester-containing mixture is added continuously in the middle section of an extraction column and in addition water and the organic extracting agent are passed continuously countercurrent in the extraction column.

    摘要翻译： （甲基）丙烯酸与C4-C6-链烷二醇的二酯与C4-C6-链烷二醇，（甲基）丙烯酸与C4-C6-链烷二醇的单酯和 （甲基）丙烯酸与C4-C6-链烷二醇的有机溶剂在水的存在下萃取，其中将含二酯的混合物连续加入萃取塔的中间部分，另外加入水和 有机提取剂在提取塔中持续逆流通过。

    Aqueous phase process for preparing N-substituted imidazoles
    8.
    发明授权
    Aqueous phase process for preparing N-substituted imidazoles 失效
    制备N-取代咪唑的水相方法

    公开(公告)号：US5877326A

    公开(公告)日：1999-03-02

    申请号：US914187

    申请日：1997-08-19

    申请人： Gisela Hieber ,  Klaus Ebel ,  Jurgen Schroder ,  Toni Dockner ,  Carsten Groning ,  Bernd Ruge

    发明人： Gisela Hieber ,  Klaus Ebel ,  Jurgen Schroder ,  Toni Dockner ,  Carsten Groning ,  Bernd Ruge

    IPC分类号： C07D233/58 ,  B01J21/12 ,  B01J27/16 ,  C07D233/54 ,  C07D233/68 ,  C07D233/90 ,  C07D233/91 ,  C07D233/92 ,  C07D235/06 ,  C07D235/08 ,  C07D233/56

    CPC分类号： C07D235/08 ,  C07D233/54 ,  C07D233/56 ,  C07D233/64 ,  C07D233/68 ,  C07D233/90 ,  C07D233/91 ,  C07D233/92 ,  C07D235/06

    摘要： 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.

    摘要翻译： 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。

    Preparation of N-substituted pyrazoles
    9.
    发明授权
    Preparation of N-substituted pyrazoles 失效
    N-取代吡唑的制备

    公开(公告)号：US5468871A

    公开(公告)日：1995-11-21

    申请号：US334613

    申请日：1994-11-07

    申请人： Klaus Ebel ,  Juergen Schroeder ,  Carsten Groening ,  Toni Dockner ,  Hans R. Merkle

    发明人： Klaus Ebel ,  Juergen Schroeder ,  Carsten Groening ,  Toni Dockner ,  Hans R. Merkle

    IPC分类号： B01J21/12 ,  C07B61/00 ,  C07D231/12 ,  C07D521/00

    CPC分类号： C07D231/12 ,  C07D233/56 ,  C07D249/08

    摘要： N-substituted-pyrazoles of the formula ##STR1## wherein R.sup.1 is C.sub.1 -C.sub.12 -alkyl or C.sub.7 -C.sub.20 -alkyl, and R.sup.2, R.sup.3 and R.sup.4 independently denote hydrogen, C.sub.1 -C.sub.12 -alkyl, phenyl, C.sub.7 -C.sub.20 -alkylphenyl and C.sub.7 -C.sub.20 -phenylalkyl, are prepared by reacting a pyrazole of the formula ##STR2## wherein R.sup.2, R.sup.3 and R.sup.4 have the meanings above, with an alcohol or ether of the formulaR.sup.1 --O--R.sup.5 III,wherein R.sup.5 is hydrogen or R.sup.1, at a temperature of from 200.degree. to 550.degree. C. and a pressure of from 0.001 to 50 bar in the presence of a heterogeneous catalyst, preferably one which contains acid centers such as the oxides of aluminum, silicon, titanium and/or zirconium, optionally doped with phosphoric acid.

    摘要翻译： 其中R 1是C 1 -C 12 - 烷基或C 7 -C 20 - 烷基，R 2，R 3和R 4独立地表示氢，C 1 -C 12 - 烷基，苯基，C 7 -C 20 - 烷基苯基 和C 7 -C 20 - 苯基烷基，其通式如下：其中R2，R3和R4具有上述含义的吡唑与式R1-O-R5III的醇或醚反应制备，其中R 5是氢或 R1在200〜550℃的温度和0.001〜50巴的压力下，在非均相催化剂存在下，优选含有酸中心的铝，硅，钛和/或氧化物的氧化物 锆，任选掺杂有磷酸。