Multitask Emulsion Crystallization for Organic Purity

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Solution Overview

Problem

Current separation processes for organic compounds face challenges in achieving high purity, especially when dealing with crude materials containing related impurities with similar structures, which are difficult to purify using classical techniques, particularly in the production of fine chemicals and active pharmaceutical ingredients.

Innovation Solution

The development of multitask emulsion crystallization (MEC) using a specific w/o reverse micelle and microemulsion system with tunable ionic and molecular transport properties, employing a continuous organic phase and non-toxic surfactants, allows for efficient separation and purification of organic compounds by controlling solubility and ionic transport properties, enabling high yields and purity levels.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If classical separation techniques are used for purifying organic compounds from crude materials, then the process is simple to operate, but the purity achievement is insufficient especially for related impurities with similar structures

Engineering Contradiction:
ImprovepurityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent changes the physical-chemical parameters of the crystallization medium by using reverse micelle systems with specific surfactants (e.g., AOT, DAS) and controlled water content (W = 0.01-100). This creates a unique crystallization environment that enables selective crystallization of organic compounds from crude materials, achieving high purity (≥95%) separation that classical techniques cannot achieve for related impurities with similar structures.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces reverse micelle systems as an intermediary medium between the crude organic compound and the crystallization process. The reverse micelle system acts as a selective mediator that allows the target compound to crystallize while retaining related impurities in the solution phase, thereby achieving high purity separation without complex multi-step processes.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If emulsion media are used for crystallization, then high purity and yield can be achieved, but the separation potential becomes lower for each additional use of the crystallization media

Engineering Contradiction:
ImprovepurityVSAvoidseparation potential
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent implements a recovery and regeneration system for the reverse micelle media. After crystallization, the media is separated from the crystallized product, purified by removing accumulated impurities, and reused in the next crystallization cycle. This recovery process maintains high separation potential across multiple uses, addressing the degradation issue of conventional emulsion media.

Inventive Principle:
Principle #34Discarding and recovering

Solution Approach 2:

The patent establishes a continuous crystallization process where the reverse micelle media is continuously regenerated and reused. The system maintains consistent crystallization performance across multiple cycles through continuous media recovery and purification, ensuring sustained high purity and yield without the diminishing separation potential observed in single-use emulsion systems.

Inventive Principle:
Principle #20Continuity of useful action

3Manufacturing precision

If multiple crystallization solvents are used for different crude products, then the purification effectiveness is maintained, but the process complexity and cost increase

Engineering Contradiction:
Improvepurification effectivenessVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent develops a universal reverse micelle system that can be applied to crystallize multiple different organic compounds from various crude materials. By adjusting parameters such as water content (W = 0.01-100), surfactant type (AOT, DAS, or combinations), and temperature, the same reverse micelle platform achieves effective purification for different target compounds, eliminating the need for multiple specialized solvents and reducing overall process complexity.

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

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

MEC achieves high purity and yield in organic compound separation, with the ability to handle different crude materials using the same system, suitable for large-scale industrial applications, and ensures the safety and efficiency of the purification process.

Implementation Method 1

The invention relates to a process for increasing the purity of organic compounds, wherein the organic compound is crystallized from a stable emulsion comprising water, hydrocarbon and a surfactant, wherein water is dispersed phase and hydrocarbon is continuous phase

Methodology Applied
Scientific EffectReverse micelle formation: Microemulsion

Implementation Method 2

the organic compound is crystallized from a stable emulsion comprising water, hydrocarbon and a surfactant

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 3

allows for efficient separation and purification of organic compounds by controlling solubility and ionic transport properties

Methodology Applied
Scientific EffectSolubility control: Solvation

Implementation Method 4

The mobility properties, ionic and molecular transport properties, of the w/o reversed micelles or w/o microemulsions are commonly investigated using electrical conductivity

Methodology Applied
Scientific EffectIonic transport: Ion Repulsion/Attraction

Implementation Method 5

since this method is very sensitive to microstructure of crystallization media

Methodology Applied
Scientific EffectElectrical conductivity: Conduction (electrical)

Implementation Method 6

the emulsions contain additives such as surface active agents lowering the interfacial tension by adsorption of surfactants and stabilizing the emulsion droplets

Methodology Applied
Scientific EffectSurfactant adsorption: Surfactant

Implementation Method 7

lowering the interfacial tension by adsorption of surfactants

Methodology Applied
Scientific EffectInterfacial tension reduction: Surface Tension

Implementation Method 8

At higher temperatures, after the impure compound has been dissolved, the emulsion is cooled to a targeted temperature where crystallization process takes place

Methodology Applied
Scientific EffectDissolution: Solvation

Implementation Method 9

the emulsion is cooled to a targeted temperature where crystallization process takes place

Methodology Applied
Scientific EffectCooling: Cooling

Data Source

PatentEP2861316B1Selective crystallization processes using reverse micelle and w/o microemulsion systems - multitask emulsion crystallization (MEC)
Publication Date: 2020.06.03 FARMA GRS D O O
  • EP2861316B1 patent drawing
  • EP2861316B1 patent drawing
  • EP2861316B1 patent drawing

AI summary

A process for increasing the purity of organic compounds is described, wherein the organic compound is crystallized from a stable emulsion comprising water, hydrocarbon and a surfactant. Preferably the emulsion consists of water, n-heptane and sodium bis(2- ethylhexyl)sulfosuccinate.