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    PROCESS FOR CONTINUOUSLY PREPARING DI-C1-3-ALKYL SUCCINATES
    3.
    发明申请
    PROCESS FOR CONTINUOUSLY PREPARING DI-C1-3-ALKYL SUCCINATES 有权
    连续制备DI-C 3-烷基琥珀酸酯的方法

    公开(公告)号：US20160083328A1

    公开(公告)日：2016-03-24

    申请号：US14888954

    申请日：2014-05-07

    Applicant: BASF SE

    Inventor： Stefanie Demming ,  Suman Thotla ,  Jens Wittenberg ,  Gabriele Iffland ,  Till Christian Brueggemann ,  Yvonne Hoelzl ,  Wolfgang Siegel ,  Stephan Freyer

    IPC: C07C67/08 ,  B01D3/14 ,  C07C67/54

    CPC classification number: C07C67/08 ,  B01D3/141 ,  C07C67/54 ,  C07C69/40

    Abstract: The invention relates to a process for continuously preparing di-C1-3-alkyl succinates by reacting succinic acid with an C1-3-alkanol in the presence of a fixed-bed heterogeneous acidic esterification catalyst in a tubular reactor at a temperature in the range of from 60 to 100° C., wherein a mixture, comprising succinic acid, C1-3-alkanol, mono-C1-3-alkyl succinate, di-C1-3-alkyl succinate and water, is formed in a mixing stage and fed to the entrance of the tubular reactor, and wherein 5 to 75% of the outlet flow rate of the tubular reactor are recycled directly to the mixing stage as a recycle stream, and the molar ratio of C1-3-alkanol to succinic acid added to the mixing zone, and not including the C1-3-alkanol and succinic acid at the recycle stream, being in the range of from 2.0 to 9.5. The invention furthermore relates to a process for separating the reactor effluent of an esterification of succinic acid with an C1-3-alkanol to give di-C1-3-alkyl succinates by distillation, wherein the separation is performed in a divided wall column in which C1-3-alkanol and water are removed in a top draw of the column, di-C1-3-alkyl succinate is removed in a side draw of the column, and wherein mono-C1-3-alkyl succinate and succinic acid are removed in a bottom draw of the column.

    Abstract translation: 本发明涉及一种连续制备二-C1-烷基琥珀酸盐的方法，该方法是在固定床非均相酸性酯化催化剂存在下，在管式反应器中在一定温度范围内使琥珀酸与C 1-3烷醇反应 为60-100℃，其中在混合阶段中形成包含琥珀酸，C 1-3链烷醇，琥珀酸单C 1-3烷基酯，琥珀酸二-C 1-3烷基酯和水的混合物， 进料到管式反应器的入口，并且其中管式反应器的出口流量的5％至75％作为循环物流直接循环到混合阶段，并且加入了C 3-链烷醇与琥珀酸的摩尔比 并且在再循环流中不包括C 1-3链烷醇和琥珀酸，其浓度范围为2.0-9.5。 本发明还涉及一种将琥珀酸酯化为C 3-链烷醇的反应器流出物分离以通过蒸馏得到二-C1-烷基琥珀酸酯的方法，其中分离是在分隔壁塔中进行的，其中在 在柱的顶部萃取中除去C 1-3链烷醇和水，在柱的侧馏分中除去琥珀酸二-C1--3烷基酯，并且其中除去C 1 -C 3烷基琥珀酸酯和琥珀酸单 在列的底部绘制。

    PROCESS FOR CONTINUOUSLY PREPARING DI-C1-3-ALKYL SUCCINATES
    6.
    发明申请
    PROCESS FOR CONTINUOUSLY PREPARING DI-C1-3-ALKYL SUCCINATES 审中-公开

    公开(公告)号：US20170342015A1

    公开(公告)日：2017-11-30

    申请号：US15659058

    申请日：2017-07-25

    Applicant: BASF SE

    Inventor： Stefanie Demming ,  Suman Thotla ,  Jens Wittenberg ,  Gabriele Iffland ,  Till Christian Brueggemann ,  Yvonne Hoelzl ,  Wolfgang Siegel ,  Stephan Freyer

    IPC: C07C67/08 ,  B01D3/14 ,  C07C67/54 ,  C07C69/40

    CPC classification number: C07C67/08 ,  B01D3/141 ,  C07C67/54 ,  C07C69/40

    Abstract: The invention relates to a process for continuously preparing di-C1-3-alkyl succinates by reacting succinic acid with an C1-3-alkanol in the presence of a fixed-bed heterogeneous acidic esterification catalyst in a tubular reactor at a temperature in the range of from 60 to 100° C., wherein a mixture, comprising succinic acid, C1-3-alkanol, mono-C1-3-alkyl succinate, di-C1-3-alkyl succinate and water, is formed in a mixing stage and fed to the entrance of the tubular reactor, and wherein 5 to 75% of the outlet flow rate of the tubular reactor are recycled directly to the mixing stage as a recycle stream, and the molar ratio of C1-3-alkanol to succinic acid added to the mixing zone, and not including the C1-3-alkanol and succinic acid at the recycle stream, being in the range of from 2.0 to 9.5. The invention furthermore relates to a process for separating the reactor effluent of an esterification of succinic acid with an C1-3-alkanol to give di-C1-3-alkyl succinates by distillation, wherein the separation is performed in a divided wall column in which C1-3-alkanol and water are removed in a top draw of the column, di-C1-3-alkyl succinate is removed in a side draw of the column, and wherein mono-C1-3-alkyl succinate and succinic acid are removed in a bottom draw of the column.

    Process for continuously preparing di-C1-3-alkyl succinates
    7.
    发明授权
    Process for continuously preparing di-C1-3-alkyl succinates 有权

    公开(公告)号：US09738588B2

    公开(公告)日：2017-08-22

    申请号：US14888954

    申请日：2014-05-07

    Applicant: BASF SE

    Inventor： Stefanie Demming ,  Suman Thotla ,  Jens Wittenberg ,  Gabriele Iffland ,  Christian Brueggemann ,  Yvonne Hoelzl ,  Wolfgang Siegel ,  Stephan Freyer

    IPC: C07C67/08 ,  B01D3/14 ,  C07C67/54

    CPC classification number: C07C67/08 ,  B01D3/141 ,  C07C67/54 ,  C07C69/40

    Abstract: The invention relates to a process for continuously preparing di-C1-3-alkyl succinates by reacting succinic acid with an C1-3-alkanol in the presence of a fixed-bed heterogeneous acidic esterification catalyst in a tubular reactor at a temperature in the range of from 60 to 100° C., wherein a mixture, comprising succinic acid, C1-3-alkanol, mono-C1-3-alkyl succinate, di-C1-3-alkyl succinate and water, is formed in a mixing stage and fed to the entrance of the tubular reactor, and wherein 5 to 75% of the outlet flow rate of the tubular reactor are recycled directly to the mixing stage as a recycle stream, and the molar ratio of C1-3-alkanol to succinic acid added to the mixing zone, and not including the C1-3-alkanol and succinic acid at the recycle stream, being in the range of from 2.0 to 9.5. The invention furthermore relates to a process for separating the reactor effluent of an esterification of succinic acid with an C1-3-alkanol to give di-C1-3-alkyl succinates by distillation, wherein the separation is performed in a divided wall column in which C1-3-alkanol and water are removed in a top draw of the column, di-C1-3-alkyl succinate is removed in a side draw of the column, and wherein mono-C1-3-alkyl succinate and succinic acid are removed in a bottom draw of the column.

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