Superficially Porous Metal Oxide Particles via Pseudomorphic Transformation

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Solution Overview

Problem

Conventional methods for producing superficially porous silica particles result in particles with broad particle size distributions, rough surfaces, and randomly distributed pores, leading to inefficiencies in chromatography due to high film mass transfer resistance and reduced packing density.

Innovation Solution

A method involving pseudomorphic transformation of solid metal oxide particles in an aqueous solution with surfactants and swelling agents to create particles with ordered pores and narrow size distributions, maintaining the original particle size and morphology while forming a porous outer shell.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional methods (spray-drying, multilayer technology, coacervation) are used to prepare superficially porous silica particles, then particles with porous outer shells are produced, but the particles exhibit broad particle size distributions and rough surfaces

Engineering Contradiction:
Improveparticle size distributionVSAvoidsurface smoothness
Core Design Contradiction:
Manufacturing precisionVSShape

Solution Approach 1:

The invention changes the chemical composition parameters of the silica sol, specifically using a silica sol with a SiO2/Al2O3 ratio of 95:5 or higher and a pH of 7-9, which enables controlled hydrolysis and condensation reactions that produce smooth surfaces and narrow particle size distributions during the coating process

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention replaces mechanical coating methods with chemically controlled coating by utilizing controlled hydrolysis and condensation reactions of silica sol on the particle surfaces, which naturally produce uniform and smooth coatings without mechanical roughness

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

2Speed

If conventional methods are used to create porous outer shells, then mass transfer is improved, but pores are randomly distributed leading to high film mass transfer resistance

Engineering Contradiction:
Improvemass transfer rateVSAvoidpore distribution uniformity
Core Design Contradiction:
SpeedVSManufacturing precision

Solution Approach 1:

The invention uses a controlled chemical reaction process where silica sol acts as an intermediary that uniformly deposits on particle surfaces through hydrolysis and condensation, creating evenly distributed pores rather than random pore formation

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

By controlling the pH (7-9) and composition (SiO2/Al2O3 ≥ 95:5) of the silica sol, the invention achieves uniform pore distribution while maintaining high mass transfer rates through the porous shell

Inventive Principle:
Principle #35Parameter changes

3Quantity of substance

If rough particle surfaces are produced by conventional methods, then porous structure is achieved, but packing density is reduced due to increased friction forces

Engineering Contradiction:
Improveporous shell contentVSAvoidsurface roughness
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The invention changes the silica sol parameters (pH 7-9, SiO2/Al2O3 ≥ 95:5) to enable controlled chemical coating that produces smooth surfaces while maintaining adequate porous shell content for chromatographic function

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention replaces mechanical mixing and coating methods with chemically controlled deposition, where silica sol naturally coats particles through hydrolysis and condensation, producing smooth surfaces that reduce inter-particle friction and improve packing density

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

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 particles exhibit improved chromatographic performance with faster separation, lower pressure drop, and higher efficiency, maintaining mechanical strength and stability at high pH.

Implementation Method 1

subjecting substantially solid metal oxide particles to pseudomorphic transformation in an aqueous solution with surfactants and swelling agents to create particles with ordered pores and narrow size distributions

Methodology Applied
Scientific EffectPseudomorphic transformation:

Implementation Method 2

micelle-templated synthesis produces a more ordered pore framework involving preformed micellar structures via a liquid crystal templating mechanism

Methodology Applied
Scientific EffectMicelle templating:

Implementation Method 3

subjecting substantially solid metal oxide particles to pseudomorphic transformation in an aqueous solution with surfactants and swelling agents

Methodology Applied
Scientific EffectSurfactant action: Surfactant

Data Source

PatentUS9284456B2Superficially porous metal oxide particles, methods for making them, and separation devices using them
Publication Date: 2016.03.15 AGILENT TECHNOLOGIES INC
  • US9284456B2 patent drawing
  • US9284456B2 patent drawing
  • US9284456B2 patent drawing

AI summary

Superficially porous hybrid particles include hybrid solid cores that each contain an inorganic material and an organic material; and porous hybrid outer shells each include the inorganic and organic materials and having ordered pores, wherein the ordered pores have a median pore size ranges from about 15 to about 1000 Å with a pore size distribution (one standard deviation) of no more than 50% of the median pore size and produce at least one X-ray diffraction peak between 0.01° and 10° of a 2θ scan range; wherein the particles have a median size range from about 0.5 μm to about 100 μm with a particle size distribution (one standard deviation) of no more than 15% of the median particle size, wherein the inorganic material comprises a metal oxide selected from silica, alumina, titania or zirconia.