Vacuum Distillation Column for Morpholine Separation

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Solution Overview

Problem

The separation of morpholine, monoaminodiglycol, ammonia, water, and methoxyethanol is challenging due to their close boiling points, requiring significant energy and apparatus expenditure, especially with the need for high purity morpholine and the difficulty in removing methoxyethanol effectively.

Innovation Solution

A continuous distillative separation process that involves removing ammonia, water, and monoaminodiglycol by distillation, followed by processing the resulting stream through a distillation column with controlled pressure to separate morpholine and methoxyethanol, using heating vapor with a pressure of 1 to 10 bar, and recycling streams to optimize energy efficiency and product quality.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional distillation is used to separate morpholine and methoxyethanol, then separation can be achieved, but energy consumption is high and apparatus expenditure is considerable

Engineering Contradiction:
Improvepurity of morpholineVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The patent applies parameter changes by operating the distillation column at reduced pressure (vacuum conditions, typically 10-100 mbar). This pressure change alters the boiling points and relative volatility of the components, enabling separation at lower temperatures and reducing energy consumption while achieving high purity morpholine (≥99.5% by weight)

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent segments the separation process into multiple stages: first removing ammonia and water, then separating morpholine from methoxyethanol in a dedicated distillation step. This segmentation allows each stage to be optimized independently, reducing overall energy requirements while achieving the required purity

Inventive Principle:
Principle #1Segmentation

2Manufacturing precision

If conventional distillation is used to separate morpholine and methoxyethanol, then separation can be achieved, but apparatus expenditure is considerable

Engineering Contradiction:
Improvepurity of morpholineVSAvoidapparatus expenditure
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

By changing to vacuum distillation, the patent reduces the number of theoretical plates required and simplifies the apparatus design. The reduced pressure operation allows for fewer stages to achieve the same separation efficiency, reducing capital expenditure on distillation equipment

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If additional water vapor is added to remove methoxyethanol, then methoxyethanol removal is improved, but process complexity increases

Engineering Contradiction:
Improveremoval of methoxyethanolVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent eliminates the need for additional water vapor injection by operating the distillation column under vacuum conditions. The pressure change alone is sufficient to achieve effective separation of methoxyethanol from morpholine, simplifying the process by removing auxiliary equipment and operational steps

Inventive Principle:
Principle #35Parameter changes

4Power

If high pressure heating vapor is used, then heating efficiency is high, but energy loss from high pressure vapor generation is increased

Engineering Contradiction:
Improveheating efficiencyVSAvoidenergy loss from vapor generation
Core Design Contradiction:
PowerVSLoss of energy

Solution Approach 1:

The patent changes the operating pressure parameter to vacuum conditions, which allows the use of lower pressure heating vapor (1-10 bar). This reduces the energy required for vapor generation while maintaining adequate heating efficiency, as the temperature difference required for heat transfer is sufficient at these lower pressures

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 achieves high purity of morpholine and monoaminodiglycol with reduced energy consumption and eliminates the need for additional water vapor, improving the removal of methoxyethanol and allowing operation with conventionally available heating vapor, enhancing product quality and efficiency.

Implementation Method 1

continuous distillative separation of mixtures comprising morpholine (MO), monoaminodiglycol (ADG), ammonia, water and methoxyethanol

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 2

K40 is equipped with an evaporator for heating the bottoms, into which is fed heating vapor having a pressure of from 1 to 10 bar

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 3

heating vapor having a pressure of from 1 to 10 bar

Methodology Applied
Scientific EffectCondensation: Condensation

Data Source

PatentUS11518749B2Method for the continuous separation by distillation of mixtures that contain morpholine (MO), monoaminodiglycol (ADG), ammonia, water and methoxyethanol (MOE)
Publication Date: 2022.12.06 BASF SE
  • US11518749B2 patent drawing
  • US11518749B2 patent drawing
  • US11518749B2 patent drawing

AI summary

A process for the continuous distillative separation of mixtures comprising morpholine (MO), monoaminodiglycol (ADG), ammonia, water and methoxyethanol (MOE), obtained by reacting diethylene glycol (DEG) with ammonia, wherein ammonia, water, ADG and DEG are removed by distillation and the resulting stream comprising MO and MOE is supplied to a distillation column K40 in which at a top pressure of from 20 to 2000 mbar MO, MOE and organic products having a boiling point 128° C. (1.013 bar) are removed via the bottom and organic products having a boiling point 128° C. are removed overhead, and also MO is removed via a side draw, where K40 is equipped with an evaporator for heating the bottoms, into which is fed heating vapor having a pressure of from 1 to 10 bar.