Hybrid Core-Shell Chromatography Particles for Narrow Size Distribution

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Solution Overview

Problem

Existing processes for producing superficially porous particles lack the ability to create materials with narrow particle size distribution, desirable pore geometry, and improved chemical stability for high pH mobile phases, which are essential for efficient chromatographic separations.

Innovation Solution

A method involving the formation of a substantially nonporous inorganic/organic hybrid core with one or more layers of uniform porous shell material, using alkoxysilanes, organoalkoxysilanes, and nanoparticles to create a chromatographically enhanced material with controlled porosity and improved thermal conductivity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If high temperature thermal treatment (calcination at 500-1000°C) is used to remove additives and strengthen particles, then mechanical properties and particle strength are improved, but hybrid materials cannot be used because they are not thermally stable above 600°C

Engineering Contradiction:
Improveparticle strengthVSAvoidthermal stability
Core Design Contradiction:
StrengthVSStability of the object's composition

Solution Approach 1:

The patent changes the thermal treatment parameter from high temperature (500-1000°C) to low temperature (room temperature to 100°C), enabling the use of hybrid materials that would otherwise decompose at high temperatures. This parameter change resolves the contradiction by finding an alternative temperature regime that achieves particle strengthening without compromising hybrid material stability.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent replaces the thermal strengthening mechanism (calcination) with a chemical crosslinking mechanism using silane coupling agents. The silane groups form covalent bonds between particles, providing mechanical strength through chemical bonding rather than thermal treatment, thus enabling hybrid material usage.

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

2Shape

If conventional layering processes are used to form porous layers, then superficially porous particles can be created, but narrow particle size distribution and monodispersity are not achieved

Engineering Contradiction:
Improveporous layer formationVSAvoidparticle size distribution
Core Design Contradiction:
ShapeVSManufacturing precision

Solution Approach 1:

The patent changes the particle size distribution parameter by using monodisperse silica cores with narrow size distribution as starting material, and maintains this narrow distribution throughout the coating process by controlling deposition conditions, achieving final particles with less than 10% size distribution.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent performs preliminary size selection and monodispersity optimization of the core particles before the coating process, ensuring that the starting material already has the desired narrow size distribution, which is then preserved during subsequent coating steps.

Inventive Principle:
Principle #10Preliminary action

3Shape

If repeated centrifugation and redispersion steps are used in the coating process, then uniform porous layers can be formed, but the process becomes complex and time-consuming

Engineering Contradiction:
Improveuniform porous layerVSAvoidprocess complexity
Core Design Contradiction:
ShapeVSDevice complexity

Solution Approach 1:

The patent performs preliminary optimization of the coating process to achieve uniform layer formation in fewer steps. By optimizing parameters such as sol concentration, deposition time, and drying conditions, the patent reduces the number of repeated centrifugation and redispersion cycles needed while maintaining layer uniformity.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent implements continuous coating processes where the porous layer is deposited in a continuous manner without repeated interruption for centrifugation and redispersion. This continuous approach maintains uniformity while simplifying the overall process flow and reducing complexity.

Inventive Principle:
Principle #20Continuity of useful action

4Measurement precision

If smaller particle sizes are used for modern applications, then separation efficiency for small molecules is improved, but backpressure increases and chemical stability with high pH mobile phases decreases

Engineering Contradiction:
Improveseparation efficiencyVSAvoidbackpressure
Core Design Contradiction:
Measurement precisionVSStress or pressure

Solution Approach 1:

The patent creates particles with non-uniform porosity distribution, having a dense core and a porous shell. This local quality differentiation allows the particle to provide efficient separation in the porous shell region while the dense core maintains structural integrity and reduces backpressure, enabling smaller particle sizes without proportional pressure increases.

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The patent uses composite particles consisting of a silica core with a porous coating layer. This composite structure combines the advantages of dense particles (low backpressure, high chemical stability) with porous particles (high separation efficiency), allowing smaller particle sizes to be used effectively.

Inventive Principle:
Principle #40Composite materials

5Ease of manufacture

If surfactants and binders are added during synthesis to facilitate particle formation, then particle production is enabled, but additional removal steps are required to eliminate these additives

Engineering Contradiction:
Improveparticle formationVSAvoidadditive removal
Core Design Contradiction:
Ease of manufactureVSLoss of substance

Solution Approach 1:

The patent uses extraction methods to remove surfactant and binder additives from the particle structure after synthesis. By applying solvents or other extraction agents, the additives are selectively removed from the particle matrix, eliminating the need for complex purification steps while maintaining particle integrity.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent employs processes where additives are discarded after serving their manufacturing function. The surfactants and binders are removed in controlled steps, with the understanding that their temporary presence during synthesis facilitates particle formation, but their final removal is necessary for product purity.

Inventive Principle:
Principle #34Discarding and recovering

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 material exhibits improved column efficiency, reduced backpressure, and enhanced chemical stability, making it suitable for high pH mobile phases, with applications in chromatographic separations.

Implementation Method 1

using alkoxysilanes, organoalkoxysilanes, and nanoparticles to create a chromatographically enhanced material with controlled porosity

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 2

using alkoxysilanes, organoalkoxysilanes, and nanoparticles to create a chromatographically enhanced material with controlled porosity

Methodology Applied
Scientific EffectCondensation: Condensation

Implementation Method 3

one or more layers of uniform porous shell material surrounding the core

Methodology Applied
Scientific EffectPorosity: Porosity

Implementation Method 4

useful for chromatographic separations

Methodology Applied
Scientific EffectChromatography: Chromatography

Data Source

PatentEP4353682B1Superficially porous materials comprising a substantially nonporous hybrid core having narrow particle size distribution, useful for chromatographic separations
Publication Date: 2025.11.12 WATERS TECHNOLOGY CORP
  • EP4353682B1 patent drawingFigure 1
  • EP4353682B1 patent drawingFigure 2
  • EP4353682B1 patent drawingFigure 3

AI summary

The present i nventi on provides novel chromatographic materials, e.g., for chromatographic separati ons, processes for its preparati on and separati ons devi ces contai ni ng the chromatographic material; separati ons devi ces, chromatographic columns and ki ts compri si ng the same; and methods for the preparati on thereof. The chromatographic materials of the i nventi on are chromatographic materials compri si ng havi ng a narrow particle size distribution.