Buffered Room-Temperature Synthesis of Mesoporous Silica

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Solution Overview

Problem

Current methods for producing surface-functionalized ordered mesoporous silica (SF-OMS) face challenges in large-scale, cost-effective, and environmentally friendly production due to harsh synthesis conditions, high energy consumption, and inefficiencies in metal scavenging and catalysis applications.

Innovation Solution

A method involving the mixing of alkali silicate, non-ionic polymeric pore structure directing agents, and functionalizing agents in a buffered solution at room temperature, allowing for immediate solid formation and continuous synthesis without the need for high temperatures or organic solvents, followed by ultrasonication for template removal.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional co-condensation method with TEOS and strong acid is used, then surface-functionalized ordered mesoporous silica can be obtained, but high energy consumption and long synthesis time occur due to high temperature aging

Engineering Contradiction:
Improvesurface functionalisation qualityVSAvoidenergy consumption
Core Design Contradiction:
ReliabilityVSUse of energy by stationary object

Solution Approach 1:

The patent changes the pH parameter from strongly acidic (conventional method) to buffered solution with pH 2-8, and changes the temperature parameter from high temperature aging (80-130°C) to room temperature or mild heating, thereby reducing energy consumption while maintaining functionalisation quality

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent replaces expensive TEOS precursor with inexpensive alkali silicate solution, and uses buffer solutions that can be easily prepared and disposed of, reducing both material cost and energy input requirements

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Reliability

If conventional co-condensation method with TEOS and strong acid is used, then surface-functionalized ordered mesoporous silica can be obtained, but long synthesis time is required due to extended aging periods

Engineering Contradiction:
Improvesurface functionalisation qualityVSAvoidsynthesis time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent changes the pH parameter from strongly acidic to buffered solution, which accelerates the condensation reaction and eliminates the need for extended aging periods, reducing synthesis time from days to hours or even minutes

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent performs surface functionalisation during the initial synthesis stage rather than requiring separate post-synthesis treatment, combining multiple steps into one efficient process

Inventive Principle:
Principle #10Preliminary action

3Reliability

If conventional method with toxic organic solvents and multiple steps is used, then surface-functionalized ordered mesoporous silica can be obtained, but environmental friendliness and process simplicity deteriorate

Engineering Contradiction:
Improvesurface functionalisation qualityVSAvoidenvironmental impact
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The patent removes toxic organic solvents from the synthesis system entirely, replacing them with aqueous buffered solutions, thereby eliminating harmful environmental factors while maintaining functionalisation effectiveness

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent combines pore formation, silica condensation, and surface functionalisation into a single one-pot synthesis process, eliminating multiple separate steps and associated solvents, thereby improving environmental friendliness and process simplicity

Inventive Principle:
Principle #5Merging (Combining)

4Ease of manufacture

If disordered silica gel is used instead of ordered mesoporous silica, then production cost and complexity are reduced, but metal scavenging activity and catalytic performance deteriorate

Engineering Contradiction:
Improveproduction simplicityVSAvoidmetal scavenging activity
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent incorporates pore-forming agents during synthesis to pre-establish the ordered mesoporous structure, eliminating the need for subsequent complex ordering treatments while maintaining high metal scavenging activity and catalytic performance

Inventive Principle:
Principle #10Preliminary action

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 cost- and time-efficient production of SF-OMS with improved uniformity and accessibility, enhancing metal scavenging and catalytic performance while reducing environmental impact and operational costs.

Implementation Method 1

Mesoporous silica materials possess attractive characteristics such as large surface areas and well-defined ordered pores of controlled size that are the result of templating with organic molecules.

Methodology Applied
Scientific EffectTemplating:

Implementation Method 2

The mixture is then ultrasonicated to remove the template.

Methodology Applied
Scientific EffectUltrasonic vibration: Ultrasonic Vibration

Data Source

PatentEP3743376B1A method for obtaining mesoporous silica particles with surface functionalisation
Publication Date: 2024.03.06 TECH UNIV BERLIN
  • EP3743376B1 patent drawingFigure 1(A)
  • EP3743376B1 patent drawingFigure 1(B)
  • EP3743376B1 patent drawingFigure 2(A)

AI summary

The present invention relates to a method for obtaining mesoporous silica particles with surface functionalisation comprising the steps of a) providing solutions of at least three precursors, wherein the at least three precursor agents are selected from a group containing: at least one alkali silicate solution, at least one solution containing at least one pore structure directing agent (SDA), and at least one agent for surface functionalisation; wherein the pH of the mixture is adjusted to a range between 2 and 8 in a buffered system; b) Mixing the precursor solutions thereby allowing a reaction to take place at a temperature between 20 and 60 °C, preferably between 20 °C and 25 °C, whereby surface functionalized mesoporous silica particles as solid reaction product are formed; c) Separating the surface functionalized mesoporous silica particles from the reaction mixture by centrifugation or filtration and optionally washing the surface functionalized mesoporous silica; d) Removing any pore structure directing agent present in the pores of the formed surface functionalized mesoporous silica particles by ultrasonication at a temperature between 20 °C and 30 °C, preferably between 20 °C and 35°C; e) followed by separation by centrifugation or filtration, washing and drying of the surface functionalized mesoporous silica particles.