Dividing Wall Column for Morpholine Distillation

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Solution Overview

Problem

The existing processes for the separation of morpholine, monoaminodiglycol, ammonia, and water are energy-intensive and require significant apparatus, leading to inefficiencies and impurities in the separation of valuable organic components.

Innovation Solution

A continuous distillative separation process involving a three-column configuration with a dividing wall column, where ammonia is removed overhead in the first column, water and organic products are separated in the second column, and the bottom discharge is processed in a third column with a dividing wall to achieve high-purity separation of morpholine, monoaminodiglycol, and other organic products, with optional recirculation and further purification steps.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional multi-stage distillation is used to separate morpholine, monoaminodiglycol, ammonia and water, then separation completeness is improved, but energy consumption and apparatus complexity increase significantly

Engineering Contradiction:
Improveseparation completenessVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by stationary object

Solution Approach 1:

The distillation process is divided into three functional columns: K10 for ammonia removal, K20 for water and organic product separation, and K30 (dividing wall column) for high-purity organic product separation. Each column is optimized for specific separation tasks, reducing overall energy consumption compared to conventional multi-stage distillation while maintaining complete separation.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

Columns K20 and K30 are combined into a single dividing wall column structure, where the dividing wall creates separate flow paths for different organic products. This merging reduces apparatus complexity and energy consumption while achieving complete separation of morpholine, monoaminodiglycol, and other organic products from water and ammonia.

Inventive Principle:
Principle #5Merging (Combining)

2Manufacturing precision

If conventional distillation apparatus is used, then separation capability is improved, but apparatus complexity and capital outlay increase

Engineering Contradiction:
Improveseparation capabilityVSAvoidapparatus complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The dividing wall column combines multiple separation functions into a single apparatus. The dividing wall creates separate rectification and stripping sections that handle different organic products simultaneously, reducing the number of separate columns needed while maintaining high separation capability for morpholine, monoaminodiglycol, and other organic products.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The dividing wall column serves multiple functions: separating morpholine from water and ammonia, separating monoaminodiglycol from water and ammonia, and separating other organic products with boiling points >128°C from the mixture. This multi-functionality reduces apparatus complexity while maintaining comprehensive separation capability.

Inventive Principle:
Principle #6Universality (Multi-functionality)

3Manufacturing precision

If extensive distillation stages are used, then product purity is improved, but energy consumption increases

Engineering Contradiction:
Improveproduct purityVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by stationary object

Solution Approach 1:

The distillation process is segmented into three optimized columns, each handling specific separation tasks. K10 removes ammonia, K20 separates water and organic products, and K30 achieves high-purity separation. This segmentation achieves high product purity with reduced energy consumption compared to extensive single-column distillation stages.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process utilizes different pressure conditions in each column to optimize separation. K10 operates at higher pressure for ammonia removal, while K20 and K30 operate at reduced pressure to facilitate water and organic product separation. This parameter change strategy achieves high purity products with lower energy consumption.

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This process reduces energy requirements, minimizes apparatus complexity, and achieves high-purity separation of morpholine and monoaminodiglycol, along with other organic products, enhancing their quality and color quality, while reducing secondary components and energy consumption.

Implementation Method 1

The unreacted starting materials, valuable products and by-products are separated off by distillation

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 2

with the removal of ADG and organic products with a boiling point > 190 °C (1.013 bar) via the bottom, the removal of organic products with a boiling point ≤ 128 °C (1.013 bar)

Methodology Applied
Scientific EffectRectification: Distillation

Data Source

PatentEP2077990B1Method for the continuous separation by distillation of mixtures that contain morpholine (MO), monoaminodiglycol (ADG), ammonia and water
Publication Date: 2013.08.07 BASF SE
  • EP2077990B1 patent drawingFigure 1
  • EP2077990B1 patent drawingFigure 2
  • EP2077990B1 patent drawingFigure 3

AI summary

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.