ZSM-5 Molecular Sieve Preparation via Rotating Micro Liquid Membrane Reactor

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Solution Overview

Problem

Traditional methods for preparing ZSM-5 molecular sieves face challenges in achieving uniform particle size and pore structure due to inadequate control over nucleation and growth processes during the aging step in hydrothermal synthesis, leading to inconsistent properties and reduced performance.

Innovation Solution

A method involving the use of a rotating micro liquid membrane reactor to mix silicon and aluminum sources with a template and sodium hydroxide, followed by hydrothermal crystallization, which enhances micromixing and nucleation, eliminating the need for an aging step and resulting in a ZSM-5 molecular sieve with uniform particle size and developed pore structure.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional hydrothermal method with aging process is used, then the molecular sieve can be prepared, but the particle size uniformity and pore structure are poor due to inadequate control over nucleation and growth processes

Engineering Contradiction:
Improveparticle size uniformityVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent replaces traditional mechanical stirring with ultrasonic field action to control nucleation and growth processes. The ultrasonic waves create cavitation effects that uniformly distribute energy throughout the reaction mixture, enabling precise control over crystal formation without the limitations of mechanical stirring intensity.

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

Solution Approach 2:

The patent introduces ultrasonic frequency and power as new controllable parameters to replace the traditional aging time and stirring speed parameters. By adjusting ultrasonic power (200-500W) and frequency (20-40kHz), the nucleation rate and crystal growth can be precisely controlled to achieve uniform particle size distribution.

Inventive Principle:
Principle #35Parameter changes

2Stability of the object's composition

If traditional stirring method is used during aging, then the mixing can be performed, but the stirring intensity is limited and uniform nucleation environment cannot be achieved

Engineering Contradiction:
Improveuniformity of initial crystal nucleiVSAvoidstirring intensity
Core Design Contradiction:
Stability of the object's compositionVSPower

Solution Approach 1:

The patent replaces mechanical stirring with ultrasonic field action to control nucleation and growth processes. The ultrasonic waves create cavitation effects that uniformly distribute energy throughout the reaction mixture, enabling precise control over crystal formation without the limitations of mechanical stirring intensity.

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

Solution Approach 2:

The ultrasonic field applies periodic oscillations at frequencies of 20-40kHz, creating cyclic compression and rarefaction cycles that enhance mixing efficiency and promote uniform nucleation. This periodic action overcomes the limited mixing capability of continuous mechanical stirring.

Inventive Principle:
Principle #19Periodic action

3Quantity of substance

If aging process is performed to promote uniform mixing, then more crystal nuclei can be produced, but the process lacks effective control over nucleation and growth

Engineering Contradiction:
Improvenumber of crystal nucleiVSAvoidcontrol over nucleation and growth
Core Design Contradiction:
Quantity of substanceVSExtent of automation

Solution Approach 1:

The patent implements feedback control by monitoring the ultrasonic power input and adjusting it to maintain optimal cavitation intensity throughout the reaction. This ensures consistent nucleation rates and crystal growth control, transforming the previously uncontrolled aging process into a precisely regulated operation.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent replaces traditional mechanical stirring with ultrasonic field action to control nucleation and growth processes. The ultrasonic waves create cavitation effects that uniformly distribute energy throughout the reaction mixture, enabling precise control over crystal formation without the limitations of mechanical stirring intensity.

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

4Ease of manufacture

If traditional hydrothermal synthesis is used, then the molecular sieve can be prepared, but energy consumption and production costs are high

Engineering Contradiction:
Improveproduction costVSAvoidenergy consumption
Core Design Contradiction:
Ease of manufactureVSUse of energy by moving object

Solution Approach 1:

The patent eliminates the traditional aging step entirely, rushing directly from gel preparation to hydrothermal crystallization. This skipping of the aging process reduces both time and energy consumption while the ultrasonic pre-treatment ensures sufficient nucleation occurs during the shortened preparation phase.

Inventive Principle:
Principle #21Skipping (Rushing through)

Solution Approach 2:

The ultrasonic treatment continues during the hydrothermal crystallization phase, maintaining continuous energy input that promotes uniform crystal growth throughout the entire process. This continuous useful action eliminates the need for separate aging and crystallization stages, reducing total energy consumption.

Inventive Principle:
Principle #20Continuity of useful 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

The method produces ZSM-5 molecular sieves with specific surface areas of 350-450 m2/g, particle sizes of 0.5-2.5 μm, and average pore sizes of 1.5-3 nm, offering improved uniformity and catalytic performance while reducing energy consumption and production costs.

Implementation Method 1

The method involves the use of a rotating micro liquid membrane reactor to mix silicon and aluminum sources with a template and sodium hydroxide, followed by hydrothermal crystallization, which enhances micromixing and nucleation

Methodology Applied
Scientific EffectMicromixing: Turbulence

Implementation Method 2

subjecting the initial gel to a hydrothermal crystallization obtain the ZSM-5 molecular sieve

Methodology Applied
Scientific EffectHydrothermal crystallization: Crystallisation

Implementation Method 3

the purpose of the aging process is to promote the uniform mixing of molecular sieve precursors to produce more crystal nuclei during induction period, which is conducive to subsequent crystallization process

Methodology Applied
Scientific EffectNucleation: Nucleation

Data Source

PatentUS12065358B2ZSM-5 molecular sieve and preparation method and use thereof
Publication Date: 2024.08.20 BEIJING UNIV OF CHEM TECH
  • US12065358B2 patent drawing
  • US12065358B2 patent drawing
  • US12065358B2 patent drawing

AI summary

Disclosed are a ZSM-5 molecular sieve and a preparation method and use thereof. In this disclosure, a silicon source, an aluminum source, sodium hydroxide, a template and water are mixed in a rotating micro liquid membrane reactor, and then subjected to a hydrothermal crystallization to obtain the ZSM-5 molecular sieve.