公开(公告)号：EP2079717B1

公开(公告)日：2010-03-03

申请号：EP07803418.8

申请日：2007-09-12

Applicant: BASF SE

Inventor： SCHMIDTKE, Helmut ,  BUSSMANN, Oliver ,  VERSCH, Ralph ,  RHEUDE, Udo ,  LEYK, Uwe ,  JULIUS, Manfred ,  RUDLOFF, Martin ,  HENKES, Erhard

IPC: C07D295/02

CPC classification number: C07D295/027

公开(公告)号：EP2077990B1

公开(公告)日：2013-08-07

申请号：EP07803421.2

申请日：2007-09-12

Applicant: BASF SE

Inventor： SCHMIDTKE, Helmut ,  BUSSMANN, Oliver ,  VERSCH, Ralph ,  RHEUDE, Udo ,  LEYK, Uwe ,  JULIUS, Manfred ,  RUDLOFF, Martin ,  HENKES, Erhard

IPC: C07C213/10 ,  C07C217/08 ,  C07D295/02

CPC classification number: C07C213/10 ,  C07D295/023 ,  C07C217/08

公开(公告)号：EP2079717A1

公开(公告)日：2009-07-22

申请号：EP07803418.8

申请日：2007-09-12

Applicant: BASF SE

Inventor： SCHMIDTKE, Helmut ,  BUSSMANN, Oliver ,  VERSCH, Ralph ,  RHEUDE, Udo ,  LEYK, Uwe ,  JULIUS, Manfred ,  RUDLOFF, Martin ,  HENKES, Erhard

IPC: C07D295/02

CPC classification number: C07D295/027

Abstract: The invention relates to method for the continuous separation of mixtures comprising morpholine (MO), monoaminodiglycol (ADG), ammonia, and water by means of distillation, obtained by the reaction of diethylene glycol (DEG) with ammonia, wherein in a first distillation column K10 ammonia is separated at the head, the yield of K10 is fed to a second distillation column K20, in which water and organic products are separated at the head at a head temperature ranging between 45 and 198°C, and a pressure ranging between 0.1 and 15 bars, the yield of K20 is fed to a third distillation column K30, in which MO and organic products having a boiling point of 190°C (1.013 bars) are separated at the bottom, and the flow comprising the MO, which is separated in column K30 at the head or by side draw, is fed to a column K40, in which the MO is separated by side draw, organic products having a boiling point of 128°C (1.013 bars) are separated at the head, and organic products having a boiling point of 128°C (1.013 bars) are separated at the bottom.

Abstract translation: 本发明涉及通过二乙二醇（DEG）与氨反应获得的包含吗啉（MO），单氨基二甘醇（ADG），氨和水的蒸馏的连续分离混合物的方法，其中在第一蒸馏塔 K10氨在塔顶被分离，K10的产量被供给到第二蒸馏塔K20，其中水和有机产物在塔顶温度为45-198℃，压力范围为0.1 和15巴时，将K 2 O的产量加入到第三蒸馏塔K30中，其中将MO和沸点<140℃（1.013巴）的有机产物在塔顶或侧面分离，并将ADG和有机物 沸点> 190℃（1.013巴）的产物在塔底被分离，并且包含在塔K30中在塔顶或侧向塔中分离出的MO的流体进料到塔K40中，其中 MO通过侧取，有机物分离 沸点为128℃（1.013巴）的产物在塔顶分离，沸点为128℃（1.013巴）的有机产物在塔底分离。

公开(公告)号：EP2077990A1

公开(公告)日：2009-07-15

申请号：EP07803421.2

申请日：2007-09-12

Applicant: BASF SE

Inventor： SCHMIDTKE, Helmut ,  BUSSMANN, Oliver ,  VERSCH, Ralph ,  RHEUDE, Udo ,  LEYK, Uwe ,  JULIUS, Manfred ,  RUDLOFF, Martin ,  HENKES, Erhard

IPC: C07C213/10 ,  C07C217/08 ,  C07D295/02

CPC classification number: C07C213/10 ,  C07D295/023 ,  C07C217/08

Abstract: The invention relates to a method for the continuous separation by distillation of mixtures that contain morpholine (MO), monoaminodiglycol (ADG), ammonia and water, obtained by reacting diethyleneglycol (DEG) with ammonia. The method according to the invention is characterized by separating ammonia at the head of a first distillation column K10, feeding the product from the bottom of the column K10 to a second distillation column K20 in which water and organic products are removed at the head of the column at a head temperature ranging from 45 to 198°C and a pressure ranging from 0.1 to 15 bar, feeding the product from the bottom of the column K20 to a third distillation column K30, said column K30 being a divided wall column (TK) that has a partition wall (T) in the longitudinal direction of the column forming an upper common column section (1), a lower common column section (6), an inlet section (2, 4) having a rectification section (2) and a stripping section (4), and an outlet section (4, 5) having a rectification section (3) and a stripping section (5). The product from the bottom of the column of K20 is fed in the upper and middle third of the feed section (2, 4), based on the number of theoretical plates of the feed section, ADG and organic products having a boiling point > 190 °C (1.013 bar) are removed via the bottom of the column, the organic products having a boiling point ≤ 128 °C (1.013 bar) are removed via the head of the column, and the MO is removed from the middle and lower third of the outlet section (3, 5) (side stream), based on the number of theoretical plates of the outlet section.

Abstract translation: 本发明涉及一种通过蒸馏连续分离二甘醇（DEG）与氨反应得到的含有吗啉（MO），单氨基二甘醇（ADG），氨和水的混合物的方法。 根据本发明的方法的特征在于，在第一蒸馏塔K10的顶部分离氨，将产物从塔K10的底部供给到第二蒸馏塔K20，在第二蒸馏塔K20中，在第一蒸馏塔K10的头部除去水和有机产物 塔顶温度范围为45-198℃，压力范围为0.1-15巴，将产物从塔K20的底部送入第三蒸馏塔K30，所述塔K30为分隔壁塔（TK） （1），下共用塔段（6），具有精馏段（2）的入口段（2,4），和在塔的纵向方向上具有分隔壁 汽提段（4）和具有精馏段（3）和汽提段（5）的出口段（4,5）。 基于进料段的理论塔板数，ADG和沸点> 190的有机产物，来自K20塔底部的产物在进料段（2,4）的上部和中部三分之一处进料 ℃（1.013巴）通过塔底除去，通过塔顶除去沸点≤128℃（1.013巴）的有机产物，从中间和下三分之一中除去MO 基于出口部分的理论塔板的数量计算出口部分（3,5）（侧流）的流量。