Ionic Gelation on Solids for Microcapsule Shell Consolidation

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Solution Overview

Problem

Existing microencapsulation methods, such as ionic gelation, face challenges with high porosity of the gel matrix, leading to quick diffusion of encapsulated compounds and limitations due to sensitivity to environmental conditions like heating and acidification, which restrict their range of applications.

Innovation Solution

A process involving the controlled adsorption of negatively charged macromolecules onto water-insoluble solids in the presence of polyvalent ions at low temperature, followed by thermal treatment to consolidate the shell, achieving high adsorption (>80%) without colloidal destabilization, and allowing for the formation of stable microcapsules that can be dried to produce individual or agglomerated microspheres.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If ionic gelation is used to encapsulate water-insoluble solids, then the encapsulation efficiency is improved, but the porosity of the gel matrix increases causing quick diffusion of encapsulated compounds

Engineering Contradiction:
Improveencapsulation efficiencyVSAvoidmatrix porosity
Core Design Contradiction:
ReliabilityVSStability of the object's composition

Solution Approach 1:

The patent changes the physical-chemical parameters of the gelation process by using divalent ions (Ca2+, Mg2+) at controlled concentrations (1-10 mM) and specific pH ranges (5-8) to form a gel matrix with optimized porosity. The temperature control during gelation (4-25°C) and the gradual addition of ions allow formation of a less porous matrix compared to conventional rapid gelation, thereby reducing compound diffusion while maintaining encapsulation efficiency

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite gel matrix by combining charged macromolecules (polysaccharides, proteins, or synthetic polyelectrolytes) with divalent ions to form an ionic cross-linked network. This composite structure utilizes the electrostatic interaction between negatively charged macromolecule groups and divalent cations to create a matrix with controlled porosity and improved stability, preventing both compound leakage and colloidal destabilization

Inventive Principle:
Principle #40Composite materials

2Stability of the object's composition

If heating or acidification is used to reduce gel matrix porosity, then the diffusion of encapsulated compounds is reduced, but thermolabile compounds degrade

Engineering Contradiction:
Improvematrix porosityVSAvoidcompound degradation
Core Design Contradiction:
Stability of the object's compositionVSObject-affected harmful factors

Solution Approach 1:

The patent replaces thermal and chemical (acidification) methods with an ionic cross-linking mechanism using divalent ions to control gel matrix porosity. Instead of applying heat or acid to reduce porosity, the method uses electrostatic cross-linking between divalent cations and charged macromolecules to form a stable, low-porosity matrix at mild temperatures and neutral pH, thereby protecting thermolabile compounds from degradation

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent optimizes the pH range (5-8) and ionic strength during gelation to achieve appropriate matrix cross-linking density without extreme conditions. By controlling these parameters, the gel matrix forms with reduced porosity through ionic cross-linking rather than thermal or acidic treatment, maintaining compound integrity while achieving controlled release properties

Inventive Principle:
Principle #35Parameter changes

3Productivity

If conventional drying processes are used for microcapsules, then the production efficiency is improved, but aggregate or lump formation occurs causing colloidal destabilization

Engineering Contradiction:
Improvedrying efficiencyVSAvoidcolloidal stability
Core Design Contradiction:
ProductivityVSStability of the object's composition

Solution Approach 1:

The patent performs preliminary stabilization of the colloidal suspension before drying by optimizing the ionic cross-linking of the gel matrix. The divalent ion treatment creates a robust shell structure that pre-prevents aggregate formation during subsequent drying, allowing efficient drying processes without colloidal destabilization. The shell acts as a protective barrier that maintains particle separation during water removal

Inventive Principle:
Principle #10Preliminary action

4Device complexity

If only one charged macromolecule is used in ionic gelation, then the process complexity and costs are reduced, but control over gel matrix properties is limited

Engineering Contradiction:
Improveprocess complexityVSAvoidgel matrix control
Core Design Contradiction:
Device complexityVSAdaptability or versatility

Solution Approach 1:

The patent achieves versatile control over gel matrix properties by systematically varying parameters such as divalent ion concentration (1-10 mM), pH (5-8), temperature (4-25°C), and macromolecule-to-ion ratios, rather than using multiple different macromolecules. These parameter adjustments allow fine-tuning of matrix porosity, cross-linking density, and release kinetics while maintaining process simplicity and using a single charged macromolecule system

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 method enables the efficient retention of shell-forming material on the surface of microcapsules, maintaining the integrity of encapsulated compounds and allowing for controlled release, while avoiding aggregate formation, thus enhancing the stability and versatility of the encapsulation process.

Implementation Method 1

charged macromolecules, such as proteins, polysaccharides or synthetic polyelectrolites that interact electrostatically with other macromolecules or oppositely charged ions in the solution or on the surface of the solid to be encapsulated

Methodology Applied
Scientific EffectElectrostatic interaction: Ion Repulsion/Attraction

Implementation Method 2

an aqueous suspension of the insoluble solid, followed by a thermal treatment and the addition of divalent ions

Methodology Applied
Scientific EffectSuspension: Suspension

Implementation Method 3

followed by a thermal treatment and the addition of divalent ions to form a shell that covers the solid

Methodology Applied
Scientific EffectHeating: Heating

Data Source

PatentEP3040373B1Ionic gelation on solids
Publication Date: 2020.12.16 UNIVERSITY OF ANTIOQUIA
  • EP3040373B1 patent drawingFigure 1
  • EP3040373B1 patent drawingFigure 2
  • EP3040373B1 patent drawingFigure 3

AI summary

The invention relates to a method for ionic gelation on solids for encapsulating water-insoluble solids. The method uses negatively charged macromolecules and soluble salts of polyvalent cations as shell-forming materials having a high adsorption on the surface of the solid when subjected to thermal treatment. The shell-forming material represents at least 10% of the weight of the dry microcapsule obtained. The obtained microcapsule can be redispersed in water and treated by altering the environment thereof in order to be used as an encapsulating medium for water-soluble compounds and they can also be used as active ingredients and/or excipients in the production of pharmaceutical or nutraceutical compositions.