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公开(公告)号:US20160083328A1
公开(公告)日:2016-03-24
申请号:US14888954
申请日:2014-05-07
申请人: BASF SE
发明人: Stefanie Demming , Suman Thotla , Jens Wittenberg , Gabriele Iffland , Till Christian Brueggemann , Yvonne Hoelzl , Wolfgang Siegel , Stephan Freyer
摘要: 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.
摘要翻译: 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。
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公开(公告)号:US10047035B2
公开(公告)日:2018-08-14
申请号:US15659058
申请日:2017-07-25
申请人: BASF SE
发明人: Stefanie Demming , Suman Thotla , Jens Wittenberg , Gabriele Iffland , Till Christian Brueggemann , Yvonne Hoelzl , Wolfgang Siegel , Stephan Freyer
摘要: 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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公开(公告)号:US10150777B2
公开(公告)日:2018-12-11
申请号:US14778788
申请日:2014-03-03
申请人: BASF SE
发明人: Burkhard Ernst , Manfred Ehresmann , Christopher Koradin , Andreas Pletsch , Melanie Bonnekessel , Thomas Kaeding , Karin Schein-Albrecht , Stefanie Demming , Franz Weber , Wolfgang Siegel , Hartwig Schroeder , Stephan Freyer , Peter Oedman
IPC分类号: C07D493/04 , C12P17/18 , A01N43/40
摘要: The invention pertains to processes to produce dry biomass of pyripyropene producer organisms, processes to obtain pyripyropenes from such dry biomass, as well as to processes to produce compounds of Formula III and/or Formula IV and/or Formula V from the pyripyropenes obtained from the dry biomass. The invention does further pertain to the dry biomass itself, as well as processes using said dry biomass to obtain pyripyropenes for the production of compounds of Formula III and/or Formula IV and/or Formula V, including processes using said dry biomass to obtain pyripyropenes or compounds of Formula III and/or Formula IV and/or Formula V in order to produce pest control compositions, in particular insecticides, comprising such compounds.
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公开(公告)号:US20170342015A1
公开(公告)日:2017-11-30
申请号:US15659058
申请日:2017-07-25
申请人: BASF SE
发明人: Stefanie Demming , Suman Thotla , Jens Wittenberg , Gabriele Iffland , Till Christian Brueggemann , Yvonne Hoelzl , Wolfgang Siegel , Stephan Freyer
摘要: 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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公开(公告)号:US09738588B2
公开(公告)日:2017-08-22
申请号:US14888954
申请日:2014-05-07
申请人: BASF SE
发明人: Stefanie Demming , Suman Thotla , Jens Wittenberg , Gabriele Iffland , Christian Brueggemann , Yvonne Hoelzl , Wolfgang Siegel , Stephan Freyer
摘要: 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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