Mesoporous Zeolite Preparation Without Organic Templates

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Solution Overview

Problem

Conventional methods for preparing mesoporous zeolites are complex and costly, often requiring organic amine templates or surfactants, which hinder their commercial application.

Innovation Solution

A method involving the mixing of silica and aluminum precursors with pH adjustment and aging to form a synthetic zeolite gel, followed by hydrothermal synthesis, cooling, and treatment with a basic solution to create mesopores, then washing, drying, and firing to produce mesoporous zeolites without the need for expensive templates or surfactants.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional methods using organic amine templates or surfactants are employed to prepare mesoporous zeolites, then mesopore formation and catalytic performance are improved, but production cost and process complexity increase significantly

Engineering Contradiction:
Improvecatalytic performanceVSAvoidprocess complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The invention extracts and removes the expensive organic amine templates and surfactants from the conventional preparation process. Instead of using these complex additives, the method relies on a simplified hydrothermal synthesis process that directly forms mesoporous zeolites with improved catalytic performance, eliminating the need for template removal steps and reducing overall process complexity

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention changes the synthesis parameters by adjusting pH, temperature, and composition ratios during hydrothermal treatment to naturally form mesoporous structures. This parameter optimization allows mesopore formation without requiring organic templates or surfactants, thereby reducing production cost and simplifying the process while maintaining catalytic performance

Inventive Principle:
Principle #35Parameter changes

2Reliability

If conventional methods using organic amine templates or surfactants are employed to prepare mesoporous zeolites, then mesopore formation and catalytic performance are improved, but production cost increases

Engineering Contradiction:
Improvecatalytic performanceVSAvoidproduction cost
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The invention replaces expensive organic amine templates and surfactants with inexpensive, readily available inorganic precursors and water. The simplified process uses low-cost reagents that can be easily disposed of or recycled, dramatically reducing production cost while still achieving mesoporous zeolite formation with good catalytic performance

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

Solution Approach 2:

By optimizing hydrothermal synthesis parameters such as temperature, time, pH, and composition ratios, the invention achieves effective mesopore formation using cheap inorganic materials instead of expensive organic templates. This parameter control enables cost-effective production of high-performance mesoporous zeolites

Inventive Principle:
Principle #35Parameter changes

3Adaptability or versatility

If only microspores are present in zeolite, then catalyst selectivity is limited, but molecular transfer distance is long leading to slow diffusion and reduced catalyst life

Engineering Contradiction:
Improvecatalyst selectivityVSAvoidcatalyst life
Core Design Contradiction:
Adaptability or versatilityVSDuration of action of moving object

Solution Approach 1:

The invention segments the pore structure into two distinct systems: microspores for selective catalytic reactions and mesopores for rapid molecular transport. This dual-pore segmentation allows reactants to quickly access active sites through mesopores, undergo selective reactions in microspores, and exit rapidly via mesopores, thereby improving both catalyst selectivity and extending catalyst life by reducing coke accumulation

Inventive Principle:
Principle #1Segmentation

4Speed

If zeolite crystal size is reduced to increase exterior surface area, then molecular transfer distance is reduced, but catalyst utility is limited to surface reactions only

Engineering Contradiction:
Improvemolecular transfer rateVSAvoidcatalyst utility
Core Design Contradiction:
SpeedVSAdaptability or versatility

Solution Approach 1:

The invention creates an interconnected porous network combining microspores and mesopores throughout the zeolite crystal structure. This porous architecture allows molecules to diffuse rapidly through mesopores to reach internal active sites, enabling the entire crystal volume to participate in catalysis rather than just the surface, thereby maintaining high molecular transfer rates while significantly increasing catalyst utility

Inventive Principle:
Principle #31Porous materials

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 approach results in mesoporous zeolites with improved molecular transfer properties and catalytic performance, offering a cost-effective solution for commercial use as catalysts or adsorbents with enhanced selectivity and catalyst life.

Implementation Method 1

adding a basic solution thereto so as to form mesopores

Methodology Applied
Scientific EffectChemical etching/dissolution:

Implementation Method 2

subjecting the synthetic zeolite gel to a hydrothermal reaction to synthesize a zeolite

Methodology Applied
Scientific EffectHydrothermal synthesis:

Implementation Method 3

subjecting the mesoporous inner wall to hydrothermal synthesis for zeolite crystallization

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 4

mixing compounds which contain elements (such as Si, Al, Na) required to zeolite synthesis, adjusting pH with the addition of an acid and aging the resulted product so as to form a synthetic zeolite gel

Methodology Applied
Scientific EffectSol-gel transformation:

Data Source

PatentUS9403690B2Method for preparation of mesoporous zeolites
Publication Date: 2016.08.02 HANWHA TOTALENERGIES PETROCHEMICAL CO LTD
  • US9403690B2 patent drawing
  • US9403690B2 patent drawing

AI summary

Provided is a preparation method for a mesoporous zeolite, particularly a method for preparing mesoporous zeolite through a simple process without using costly materials such as an organic amine template or a surfactant. The method includes 1) forming a synthetic zeolite gel by mixing a silica precursor, an aluminum precursor and water and aging the resulted mixture; 2) carrying out zeolite synthesis by subjecting the synthetic zeolite gel to a hydrothermal reaction; 3) cooling the synthesized zeolite from the above step 2), then adding a basic solution thereto and allowing them to react, thereby obtaining a mesoporous zeolite slurry; and 4) washing the mesoporous zeolite slurry with water, drying and firing it, thereby obtaining a mesoporous zeolite.