Hierarchically Ordered Crystalline Materials for Controlled Mesoporosity

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Solution Overview

Problem

Conventional methods for synthesizing hierarchically ordered crystalline materials, such as zeolites, often result in limited long-range ordering of mesophases, random mesopore sizes and locations, and lack control over the silica-to-alumina ratio (SAR), leading to poorly interconnected mesopores and inefficient diffusion of larger species.

Innovation Solution

A method involving the formation of an aqueous suspension with a parent crystalline microporous material, an alkaline reagent, a supramolecular template, and a silica or alumina source, followed by hydrothermal treatment, to induce controlled dissolution and self-assembly, resulting in hierarchically ordered crystalline materials with improved mesoporosity and SAR control.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional methods are used to form hierarchically ordered crystalline materials, then the microporous structure is maintained, but the long-range ordering of mesophase is limited and mesopores are random in size and location

Engineering Contradiction:
Improvemesopore orderingVSAvoidstructure complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent uses supramolecular templates as intermediary structures that self-assemble into ordered mesophases, which then guide the formation of hierarchically ordered crystalline materials. These templates act as mediators between the microporous parent material and the desired mesoporous structure, enabling long-range ordering without requiring complex external control mechanisms.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The method employs self-assembly of supramolecular templates and controlled dissolution of parent material to automatically generate the hierarchically ordered structure. The system uses thermodynamic driving forces and molecular recognition to spontaneously organize into the desired hierarchical architecture, eliminating the need for complex external directing agents or multi-step processing.

Inventive Principle:
Principle #25Self-service

2Manufacturing precision

If post-synthetic modification strategies are used, then hierarchically ordered structures can be formed, but control over silica-to-alumina ratio is lost and dissolution process is poorly controlled

Engineering Contradiction:
ImproveSAR controlVSAvoidprocess control
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent incorporates silica and alumina source materials into the aqueous suspension before hydrothermal treatment, allowing preliminary control of the silica-to-alumina ratio in the reaction mixture. This preliminary action ensures that the desired SAR is established before the dissolution and crystallization processes begin, maintaining precision throughout the transformation.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The method controls the dissolution process by adjusting parameters such as pH, temperature, and composition of the aqueous suspension. By carefully controlling these parameters during hydrothermal treatment, the patent achieves both controlled dissolution of parent material and precise control over the final silica-to-alumina ratio in the hierarchically ordered product.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If mesopores are introduced to improve diffusion of larger species, then accessibility to active sites improves, but mesopores become poorly interconnected

Engineering Contradiction:
Improvediffusion efficiencyVSAvoidmesopore interconnection
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent creates a nested hierarchical structure where ordered mesopores are embedded within the microporous crystalline framework. The supramolecular templates self-assemble to form mesoporous channels that are intimately connected to the microporous active sites, creating a nested architecture that ensures efficient mass transport from meso- to micropores while maintaining structural integrity.

Inventive Principle:
Principle #7Nested doll (Nesting)

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 method produces crystalline materials with enhanced mesoporosity and controlled SAR, enabling better diffusion of larger species and improved catalytic performance by maintaining the integrity of the microporous structure while achieving well-defined mesoporous symmetry.

Implementation Method 1

the inclusion of the alkaline reagent and the supramolecular template in the method may induce dissolution of the parent crystalline microporous material

Methodology Applied
Scientific EffectDissolution:

Implementation Method 2

induce dissolution of the parent crystalline microporous material and self-assembly to produce the hierarchically ordered crystalline material

Methodology Applied
Scientific EffectSelf-assembly: Self-Assembly

Implementation Method 3

hydrothermally treating the aqueous suspension to form the hierarchically ordered crystalline microporous material

Methodology Applied
Scientific EffectHydrothermal treatment:

Data Source

PatentUS20250223179A1Methods of making hierarchically ordered crystalline materials
Publication Date: 2025.07.10 SAUDI ARABIAN OIL CO
  • US20250223179A1 patent drawing
  • US20250223179A1 patent drawing
  • US20250223179A1 patent drawing

AI summary

Methods of making hierarchically ordered crystalline microporous materials are provided. The method may include forming an aqueous suspension comprising a parent crystalline microporous material, an alkaline reagent, a supramolecular template, and a silica source material, an alumina source material, or both. The method may further include hydrothermally treating the aqueous suspension to form the hierarchically ordered crystalline microporous material. The hierarchically ordered crystalline material may have a greater degree of mesoporosity than the parent crystalline microporous material and may have a silica-to-alumina ratio (SAR) that is at least 0.5 different than the parent crystalline microporous material.