Morpholine Distillation Column Segmentation

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Solution Overview

Problem

The existing processes for preparing morpholine and monoaminodiglycol are inefficient due to the formation of secondary components, requiring significant apparatus and energy for separation through distillation, and do not achieve high purity and quality of individual organic components.

Innovation Solution

A continuous fractional distillation process involving multiple columns (K10, K20, K30, K40, K50, K60, K70) with specific operating conditions and recirculation of streams to separate morpholine, monoaminodiglycol, ammonia, and water, allowing for high-purity separation of organic products, including N-ethylmorpholine and 1,2-ethylenediamine, with heat integration measures to reduce energy requirements.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional distillation methods are used to separate morpholine and monoaminodiglycol from reaction mixtures, then separation can be achieved, but the process requires considerable apparatus and energy outlay

Engineering Contradiction:
Improvepurity of morpholine and monoaminodiglycolVSAvoidapparatus complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The distillation process is divided into multiple sequential stages using several columns (K10, K20, K30, K40, K50, K60, K70), each dedicated to separating specific components at different boiling points. This segmentation allows complex mixture separation to be achieved through simpler, specialized stages rather than one complex apparatus

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process utilizes changes in temperature and pressure parameters across different distillation columns to separate components. Each column operates at optimized temperature and pressure conditions suitable for separating specific pairs of components, enabling efficient separation without requiring overly complex apparatus

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If traditional distillation methods are used to separate morpholine and monoaminodiglycol from reaction mixtures, then separation can be achieved, but significant energy is consumed

Engineering Contradiction:
Improvepurity of morpholine and monoaminodiglycolVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The process performs preliminary separation actions by removing ammonia and water in earlier distillation stages (columns K10 and K20) before the main morpholine and monoaminodiglycol separation. This preliminary action reduces the energy required in subsequent stages by working with smaller, less energy-intensive streams

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The process exploits phase transitions (vaporization and condensation) at different temperature and pressure conditions across multiple columns to separate components. By utilizing phase changes at optimized conditions, the process achieves efficient separation with reduced energy consumption compared to conventional single-stage distillation

Inventive Principle:
Principle #36Phase transitions

3Productivity

If conventional distillation processes are used, then separation of components is achieved, but high-purity products are not obtained

Engineering Contradiction:
Improveproduction efficiencyVSAvoidpurity and quality of organic components
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The separation process is segmented into multiple specialized stages, with later columns (K40, K50, K60, K70) specifically designed for high-purity separation of morpholine and monoaminodiglycol. This segmentation enables achieving high purity products while maintaining productivity through optimized separation stages

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The process incorporates feedback mechanisms where streams are recirculated between columns (e.g., from K40 to K30, from K60 to K50) to continuously refine product purity. This feedback loop ensures high-purity products are obtained while maintaining efficient production by reusing separated components

Inventive Principle:
Principle #23Feedback

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

The process achieves high purity and quality of morpholine and monoaminodiglycol, reduces energy consumption, and minimizes the accumulation of individual components in the production plant, enabling efficient production with lower heat requirements and fewer columns compared to traditional methods.

Implementation Method 1

continuous fractional distillation of mixtures comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 2

continuous fractional distillation

Methodology Applied
Scientific EffectFractionation: Fractionation

Implementation Method 3

heat integration measures to reduce energy requirements

Methodology Applied
Scientific EffectHeat integration: Heat Exchanger

Data Source

PatentUS8246793B2Method for the continuous separation of mixtures comprising morpholine (MO), monoaminodiglycol (ADG), ammonia and water by means of distillation
Publication Date: 2012.08.21 BASF SE
  • US8246793B2 patent drawing
  • US8246793B2 patent drawing
  • US8246793B2 patent drawing

AI summary

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 K10; (ii) feeding a bottom fraction from the first distillation column to a second distillation column K20, 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° 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 K30, wherein morpholine and an organic product having a boiling point of <140° 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 >190° 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 K40, wherein morpholine is separated off at a side offtake of the fourth column, an organic product having a boiling point of ≦̸128° C. (1.013 bar) is separated off at a top of the fourth distillation column and an organic product having a boiling point of ≧128° C. (1.013 bar) is separated off at a bottom of the fourth distillation column.