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    PREPARATION OF C8-C22 ALKYL (METH)ACRYLATES
    1.
    发明申请
    PREPARATION OF C8-C22 ALKYL (METH)ACRYLATES 审中-公开
    C8-C22烷基（甲基）丙烯酸酯的制备

    公开(公告)号：US20160122276A1

    公开(公告)日：2016-05-05

    申请号：US14883803

    申请日：2015-10-15

    Applicant: BASF SE

    Inventor： Andrea MISSKE ,  Hannelore Schirra ,  Christoph Fleckenstein ,  Martin Kaller ,  Ulrik Stengel ,  Mathieu Blanchot ,  Friederike Fleischhaker ,  Ritesh Nair

    IPC: C07C67/02

    CPC classification number: C07C67/58 ,  C07C67/03 ,  C07C69/54

    Abstract: The invention relates to a method of preparing a C8-C22 alkyl (meth)acrylate by transesterification of C1-C2 alkyl (meth)acrylate with a C8-C22 alkanol, said method comprising the steps of(i) reacting C1-C2 alkyl (meth)acrylate with the C8-C22 alkanol in the presence of a particulate potassium phosphate heterogeneous catalyst and a stabilizer thus releasing C1-C2 alkanol,(ii) continuously distilling off the azeotrope of C1-C2 alkyl (meth)acrylate and the C1-C2 alkanol,wherein steps (i) and (ii) are carried out simultaneously until substantially all of the C8-C22 alkanol has reacted,(iii) distilling off unconverted C1-C2 alkyl (meth)acrylate,(iv) washing the C8-C22 alkyl (meth)acrylate-comprising product mixture obtained in steps (i) through (iii) with an aqueous phase to separate off the catalyst and the stabilizer from the product mixture with the aqueous phase and optionally adding a stabilizer,(v) distilling off water from the product mixture,wherein step (iii) may also be effected after step (iv) and together with step (v) and step (v) affords a product having a purity of >98 wt %.

    Abstract translation: 本发明涉及通过C 1 -C 2烷基（甲基）丙烯酸酯与C 8 -C 22烷醇的酯交换反应制备C 8 -C 22烷基（甲基）丙烯酸酯的方法，所述方法包括以下步骤：（ⅰ）使C 1 -C 2烷基（ 甲基）丙烯酸酯与C8-C22烷醇在颗粒状磷酸钾多相催化剂和稳定剂存在下反应，从而释放C1-C2链烷醇，（ii）连续蒸馏出（甲基）丙烯酸C1-C2烷基酯和C1- C 2链烷醇，其中步骤（i）和（ii）同时进行，直到基本上所有的C 8 -C 22烷醇已反应，（iii）蒸馏未转化的（甲基）丙烯酸C 1 -C 2烷基酯，（iv）洗涤C8- 在步骤（i）至（iii）中获得的（甲基）丙烯酸C 22烷基酯产物混合物与水相分离催化剂和稳定剂与产物混合物与水相并任选地加入稳定剂，（v）蒸馏 来自产物混合物的脱水，其中步骤（iii）也可以是ef 在步骤（iv）之后并与步骤（v）和步骤（v）一起得到纯度> 98wt％的产物。

    Process for preparing isosorbide ethoxylate di(meth)acrylate
    4.
    发明授权
    Process for preparing isosorbide ethoxylate di(meth)acrylate 有权
    异山梨醇乙氧基化二（甲基）丙烯酸酯的制备方法

    公开(公告)号：US09562054B2

    公开(公告)日：2017-02-07

    申请号：US15051974

    申请日：2016-02-24

    Applicant: BASF SE

    Inventor： Andrea Misske ,  Friederike Fleischhaker ,  Christoph Fleckenstein ,  Martin Kaller ,  Ulrik Stengel ,  Mathieu Blanchot ,  Claudia Stoer ,  Ritesh Nair

    IPC: C07D493/04 ,  C08F24/00 ,  C09J4/06 ,  C08F222/10 ,  C09J4/00

    CPC classification number: C07D493/04 ,  C08F222/1006 ,  C09J4/00 ,  C09J4/06

    Abstract: A process for preparing isosorbide ethoxylate di(meth)acrylate by transesterifying alkyl (meth)acrylate with isosorbide ethoxylate, comprising the steps of: (i) ethoxylating isosorbide to give isosorbide ethoxylate, (ii) reacting alkyl (meth)acrylate with isosorbide ethoxylate in the presence of potassium phosphate as catalyst and a stabilizer and in the presence of an azeotroping agent which forms an azeotrope with the alcohol bound in the alkyl (meth)acrylate, (iii) continuously distilling off the azeotrope of azeotroping agent and alcohol, wherein steps (ii) and (iii) are conducted simultaneously until the isosorbide ethoxylate has been essentially fully converted, (iv) removing the catalyst from the product mixture comprising isosorbide ethoxylate di(meth)acrylate, (v) distilling unconverted alkyl (meth)acrylate and azeotroping agent out of the product mixture.

    Abstract translation: 包括以下步骤：（i）乙氧基化异山梨醇，得到异山梨醇乙氧基化物，（ii）使（甲基）丙烯酸烷基酯与异山梨醇乙氧基化物反应，得到异山梨醇乙氧基化物 在与（甲基）丙烯酸烷基酯结合的醇形成共沸物的共沸物存在下，连续蒸馏共沸剂和醇的共沸物，其中步骤 （ii）和（iii）同时进行，直到异山梨醇乙氧基化物已经基本上完全转化，（iv）从包含异山梨醇乙氧基化物二（甲基）丙烯酸酯的产物混合物中除去催化剂，（v）蒸馏未转化的（甲基） 共沸剂排出产品混合物。

    Process for preparing isosorbide di(meth)acrylate
    6.
    发明授权
    Process for preparing isosorbide di(meth)acrylate 有权

    公开(公告)号：US10370383B2

    公开(公告)日：2019-08-06

    申请号：US15054506

    申请日：2016-02-26

    Applicant: BASF SE

    Inventor： Andrea Misske ,  Friederike Fleischhaker ,  Christoph Fleckenstein ,  Martin Kaller ,  Ritesh Nair ,  Ulrik Stengel ,  Mathieu Blanchot

    IPC: C07D493/04 ,  C09K8/42 ,  C09K8/44 ,  C08F22/20 ,  C09J4/00

    Abstract: A process for preparing isosorbide di(meth)acrylate by transesterifying alkyl (meth)acrylate with isosorbide, comprising the steps of: (i) reacting alkyl (meth)acrylate with isosorbide in the presence of a catalyst comprising titanium(IV) or zirconium(IV) and a stabilizer in the presence of an azeotroping agent which forms an azeotrope with the alcohol bound in the alkyl (meth)acrylate, (ii) continuously distilling off the azeotrope of azeotroping agent and alcohol, wherein steps (i) and (ii) are conducted simultaneously until the isosorbide has been essentially fully converted, (iii) adding water to the product mixture which comprises isosorbide (meth)acrylate and is obtained in steps (i) and (ii) and removing the hydrolyzate of the catalyst comprising titanium(IV) or zirconium(IV), (iv) distilling unconverted alkyl (meth)acrylate and azeotroping agent out of the product mixture, (v) distilling off water from the product mixture, wherein step (iv) can also be conducted before step (iii) and steps (iv) and (v) can also be conducted in one distillation step.

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