Mesoporous Silica Particle Production via Sol-Gel Phase Separation

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Solution Overview

Problem

Current methods for producing mesoporous silica particles with macropores are complex and involve multiple steps, such as vacuum pumping, emulsification, and size classification, making them inefficient and material-intensive.

Innovation Solution

A simplified process using a sol-gel method where a water-soluble polymer and a metalorganic compound are mixed, leading to a gel with interconnected phases that are disintegrated into particles, allowing for controlled pore formation and calcination to create mesoporous and macroporous silica particles with uniform size distribution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional methods (vacuum pumping, emulsification, size classification) are used to produce mesoporous silica particles with macropores, then particles with desired porosity can be obtained, but the process becomes complex and material loss increases

Engineering Contradiction:
Improveporosity controlVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention divides the pore structure into two distinct segments: mesopores (2-50 nm) formed by surfactant templates and macropores (>50 nm) formed by phase separation between polymer-rich and polymer-poor phases. This segmentation allows independent control of each pore type through separate formation mechanisms, achieving complex porosity without complex processing steps

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The polymer matrix is incorporated into the sol-gel system before hydrolysis and condensation occur. The polymer phase separation happens concurrently with silica network formation, pre-establishing the macropore structure before particle drying and calcination. This preliminary action eliminates the need for subsequent size classification and reduces material loss

Inventive Principle:
Principle #10Preliminary action

2Quantity of substance

If traditional production methods are used, then mesoporous silica particles can be formed, but material loss increases due to size classification requirements

Engineering Contradiction:
Improvematerial utilizationVSAvoidmaterial loss
Core Design Contradiction:
Quantity of substanceVSLoss of substance

Solution Approach 1:

The invention changes the particle size parameter distribution by controlling the phase separation process during gel formation. By adjusting polymer concentration, molecular weight, and sol-gel conditions, a narrow particle size distribution is achieved inherently, eliminating the need for size classification and reducing material loss from discarding off-spec particles

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If multiple processing steps are used to create macroporous mesoporous silica, then desired pore structure is achieved, but production efficiency decreases

Engineering Contradiction:
Improvepore structure controlVSAvoidproduction efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The invention merges multiple functions into a single sol-gel process: mesopore formation via surfactant templating, macropore formation via polymer phase separation, particle formation, and pore structure development all occur concurrently during gelation and drying. This consolidation maintains precise pore structure control while dramatically improving production efficiency by eliminating sequential processing steps

Inventive Principle:
Principle #5Merging (Combining)

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 results in particles with a broad range of sizes and porosity, eliminating the need for size classification and reducing material loss, while enabling efficient drug loading and controlled release systems.

Implementation Method 1

mixing a metalorganic compound or a mixture of metalorganic compounds which contains hydrolyzable ligands to promote hydrolysis reaction

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 2

solidifying the mixture through a sol-gel transition, whereby a gel is prepared which has two three dimensional interconnected phase domains

Methodology Applied
Scientific EffectSol-gel transition: Gel

Implementation Method 3

removing the solvent by evaporation drying and/or heat-treatment

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 4

calcining the particles to form the porous material

Methodology Applied
Scientific EffectCalcination: Heat Treatment

Data Source

PatentEP2707329B1Process for producing inorganic particulate material
Publication Date: 2017.11.01 MERCK PATENT GMBH
  • EP2707329B1 patent drawingFigure 1

AI summary

The present invention is directed to a process for producing inorganic particulate material, the material obtainable by such process, a modified release delivery system comprising the material and the use of the material for the administration of a bioactive agent.