Solid Microcapsule Shell with Sub-Nanometer Pores for Active Ingredient Retention

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Solution Overview

Problem

Existing capsule technologies for active ingredients in formulated products suffer from limited retention properties, leading to leakage and instability, which compromises the performance and stability of the encapsulated substances over time.

Innovation Solution

A method for preparing solid microcapsules with a core containing an active ingredient and a solid enveloping shell less than 1 nm in pore size, achieved through a process involving the controlled emulsification and crosslinking of specific polymeric compositions, eliminating the need for surfactants and ensuring long-term retention.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional capsule manufacturing methods (spray-drying, interfacial polymerisation, solvent evaporation) are used, then capsules can be produced with active ingredients, but the retention properties are limited leading to leakage and release of active ingredients

Engineering Contradiction:
Improveretention propertiesVSAvoidmanufacturing complexity
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The invention changes the pore size parameter of the capsule shell to less than 1 nm through controlled polymerisation and crosslinking processes. This critical parameter change transforms the shell from permeable to impermeable, preventing active ingredient leakage while maintaining manufacturing feasibility through established polymer chemistry techniques.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The capsule shell is constructed as a composite polymeric material formed by polymerisation of monomers followed by crosslinking to create a dense network structure. This composite approach combines the benefits of polymer flexibility with crosslinked structural integrity, achieving both retention properties and manufacturing ease.

Inventive Principle:
Principle #40Composite materials

2Reliability

If the capsule shell is made impermeable to retain active ingredients, then retention properties improve, but the manufacturing process becomes more complex requiring precise control of polymerisation and crosslinking

Engineering Contradiction:
Improveretention propertiesVSAvoidprocess control precision
Core Design Contradiction:
ReliabilityVSManufacturing precision

Solution Approach 1:

The invention performs preliminary polymerisation of monomers to form oligomers or low molecular weight polymers before crosslinking. This preliminary action creates a precursor structure that is easier to control and process, allowing subsequent crosslinking to achieve the desired <1 nm pore size without requiring extremely precise control of the entire process at once.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The invention uses crosslinking agents as intermediaries that bridge polymer chains to form the dense crosslinked network. These crosslinking agents act as mediators that control the formation of the impermeable structure, allowing gradual and controlled achievement of the target pore size rather than requiring direct formation of the final structure.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Stability of the object's composition

If conventional capsules are used, then active ingredients can be encapsulated, but leakage occurs leading to decline in performance and stability over time

Engineering Contradiction:
ImprovestabilityVSAvoidleakage
Core Design Contradiction:
Stability of the object's compositionVSLoss of substance

Solution Approach 1:

The invention changes the pore size parameter to less than 1 nm through controlled polymerisation and crosslinking, transforming the shell from permeable to impermeable. This critical parameter change prevents active ingredient leakage while maintaining stability, directly resolving the contradiction between retention and stability.

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

The resulting microcapsules exhibit excellent retention capabilities, significantly slowing down or preventing the diffusion of compounds larger than 1 nm, thereby maintaining the integrity and performance of the active ingredients for extended periods.

Implementation Method 1

the polymerisation of the composition C2, whereby solid microcapsules dispersed in the composition C3 are obtained

Methodology Applied
Scientific EffectPolymerisation: Photopolymerisation

Implementation Method 2

the composition C2 comprising at least one monomer or polymer having an average molecular weight of less than 5000 g.mol−1, at least one crosslinking agent having an average molecular weight of less than 5000 g.mol−1

Methodology Applied
Scientific EffectCrosslinking: Chemical Bonding

Implementation Method 3

an emulsion (E1) is obtained comprising droplets of the composition C1 dispersed in the composition C2

Methodology Applied
Scientific EffectEmulsification: Emulsion

Data Source

PatentUS11033872B2Method for preparing capsules with improved retention properties and capsules obtained therefrom
Publication Date: 2021.06.15 CALYXIA

AI summary

The present invention relates to a capsule preparation method for preparing solid microcapsules, comprising the following steps:a) addition, under agitation, a composition C1, comprising at least one active ingredient, to a polymeric composition C2, the compositions C1 and C2 being mutually immiscible, whereby an emulsion (E1) is obtained comprising droplets of the composition C1 dispersed in the composition C2;b) addition, under agitation, the emulsion (E1) to a composition C3, the compositions C2 and C3 being mutually immiscible, whereby a double emulsion (E2) is obtained comprising droplets dispersed in the composition C3;c) applying shear to the emulsion (E2), whereby a double emulsion (E3) is obtained comprising size controlled droplets dispersed in the composition C3; andd) polymerising the composition C2, whereby solid microcapsules dispersed in the composition C3 are obtained.