公开(公告)号：EP3001835B1

公开(公告)日：2017-04-05

申请号：EP14722653.4

申请日：2014-05-07

申请人： BASF SE

发明人： DEMMING, Stefanie ,  THOTLA, Suman ,  WITTENBERG, Jens ,  IFFLAND, Gabriele ,  BRÜGGEMANN, Till, Christian ,  HOELZL, Yvonne ,  SIEGEL, Wolfgang ,  FREYER, Stephan

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

CPC分类号： C07C67/08 ,  B01D3/141 ,  C07C67/54 ,  C07C69/40

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.

公开(公告)号：EP3001835A1

公开(公告)日：2016-04-06

申请号：EP14722653.4

申请日：2014-05-07

申请人： BASF SE

发明人： DEMMING, Stefanie ,  THOTLA, Suman ,  WITTENBERG, Jens ,  IFFLAND, Gabriele ,  BRÜGGEMANN, Till, Christian ,  HOELZL, Yvonne ,  SIEGEL, Wolfgang ,  FREYER, Stephan

IPC分类号： C07C67/08

CPC分类号： C07C67/08 ,  B01D3/141 ,  C07C67/54 ,  C07C69/40

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范围内的温度下使琥珀酸与C 1-3烷醇反应连续制备二-C 1-3烷基琥珀酸盐的方法 为60〜100℃，其中在混合阶段形成包含琥珀酸，C 1-3 - 链烷醇，琥珀酸单-C1-烷基酯，琥珀酸二-C1-烷基酯和水的混合物， 进料到管状反应器的入口，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 到混合区，并且不包括在再循环流中的C 1-3链烷醇和琥珀酸，其范围为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-烷基琥珀酸盐的方法，其中分离是在分隔壁塔中进行的，其中在 在柱的顶部抽出物中除去C 3-链烷醇和水，在柱的侧馏分中除去琥珀酸二-C1--烷基酯，并且其中除去琥珀酸单C 1-3 - 烷基酯和琥珀酸 在列的底部绘制。