Basf Se Corporation

Ralph Versch

Helmut Schmidtke

Manfred Julius

Udo Rheude

Erhard Henkes

Martin Rudloff

Oliver Buβmann

Uwe Leyk

Karl Ott

Ronald Drews

Stephanie Mollner

Silke Simon

Processes for the continuous fractional distillation of a mixture containing morpholine (MO), monoaminodiglycol (ADG), ammonia and water from a reaction of diethylene glycol (DEG) with ammonia, the process including: (i) separating off ammonia from the mixture at a top of a first distillation column K; (ii) feeding a bottom fraction from Kto a second distillation column K, in which water and an organic product are separated off at the top at a temperature at the top in the range from 45 to 198&#xb0; C. and a pressure in the range from 0.1 to 15 bar; (iii) feeding a bottom fraction from Kto a third distillation column K, wherein the column Kis a dividing wall column (DWC)which preferably has a dividing wall (DW) in the longitudinal direction of the column to form an upper combined column region (), a lower combined column region (), an inflow part () having an enrichment section () and a stripping section (), and also an offtake part () having an enrichment section () and a stripping section (), with the bottoms from Kbeing fed in in the upper or middle third of the inflow part (), based on the number of theoretical plates of the inflow part, ADG and organic products having a boiling point of &#x3e;190&#xb0; C. (1.013 bar) being discharge at the bottom, organic products having a boiling point of &#x2266;128&#xb0; C. (1.013 bar) being discharge at a top and MO being discharge from the middle or lower third of the offtake part () (side offtake), based on the number of theoretical plates of the offtake part.

Method for the continuous separation by distillation of mixtures that contain morphonline (MO), monoaminodiglycol (ADG), ammonia and water by means of distillation

Processes for the continuous fractional distillation of a mixture comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water from a reaction of diethylene glycol (DEG) with ammonia, the process comprising: (i) separating off ammonia from the mixture at a top of a first distillation column K; (ii) feeding a bottom fraction from the first distillation column to a second distillation column K, wherein water and an organic product are separated off at a top of the second distillation column at a top temperature of 45 to 198&#xb0; C. and a pressure in the range from 0.1 to 15 bar; (iii) feeding a bottom fraction from the second distillation column to a third distillation column K, wherein morpholine and an organic product having a boiling point of &#x3c;140&#xb0; C. (1.013 bar) are separated off at a point selected from a top and a side offtake of the third distillation column, and monoaminodiglycol and an organic product having a boiling point of &#x3e;190&#xb0; C. (1.013 bar) are separated off at a bottom of the third distillation column, and (iv) feeding the morpholine-comprising stream from the third distillation column to a fourth column K, wherein morpholine is separated off at a side offtake of the fourth column, an organic product having a boiling point of &#x2266;128&#xb0; C. (1.013 bar) is separated off at a top of the fourth distillation column and an organic product having a boiling point of &#x2267;128&#xb0; C. (1.013 bar) is separated off at a bottom of the fourth distillation column.

Method for the continuous separation of mixtures comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water by means of distillation

Process for the continuous fractional distillation of mixtures including morpholine (MO), monoaminodiglycol (ADG), ammonia and water obtained by reaction of diethylene glycol (DEG) with ammonia, which includes separating off ammonia at the top of a first distillation column K10, feeding the bottoms from K10 to a second distillation column K20 in which water and organic products are separated off at the top at a temperature at the top in the range from 45 to 198&#xb0; C. and a pressure in the range from 0.1 to 15 bar, feeding the bottoms from K20 to a third distillation column K30 in which MO and organic products having a boiling point of &#x3c;140&#xb0; C. (1.013 bar) are separated off at the top or at a side offtake and ADG and organic products having a boiling point of &#x3e;190&#xb0; C. (1.013 bar) are separated off at the bottom, feeding the MO including stream which is separated off at the top or at a side offtake of the column K30 to a fourth column K40 in which organic products having a boiling point of &#x2266;128&#xb0; C. (1.013 bar) are separated off at the top and MO and organic products having a boiling point of &#x2267;128&#xb0; C. (1.013 bar) are separated off at the bottom and the bottoms from K40 are fed to a fifth distillation column K55 in which MO is separated off at the top and organic products having a boiling point of &#x2267;128&#xb0; C. (1.013 bar) are separated off at the bottom.

Processes for continuous fractional distillation of mixtures comprising morpholine, monoaminodiglycol, ammonia and water

Process for the continuous preparation of N-ethyl-2-pyrrolidone (NEP) by reacting gamma-butyrolactone (GBL) with monoethylamine (MEA) in the liquid phase, wherein GBL and MEA are used in a molar ratio in the range from 1:1.08 to 1:2 an the reaction is carried out at a temperature in the range from 320 to 420&#xb0; C. and an absolute pressure in the range from 70 to 120 bar.

Process for continuously preparing N-ethyl-2-pyrrolidone (NEP)

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Eppelsheim, Germany

Ralph Versch