Zeolite Nanoparticle Synthesis via Microfluidic Micromixer

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current methods for synthesizing zeolites, particularly nanozeolites, face challenges such as low synthesis yield, long crystallization times, difficulty in controlling particle size and distribution, and inefficient mass transfer, which hinder their application in catalytic processes like fluidized catalytic cracking in oil refining.

Innovation Solution

A continuous flow synthesis system comprising a microfluidics mixer, a buffer system, and a tubular hydrothermal system is developed, utilizing a microfluidic micromixer for efficient mixing and eliminating the aging step, allowing for controlled crystallization of Y-type zeolite nanoparticles with improved accessibility and surface area.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If conventional zeolite synthesis methods are used, then shape selectivity is maintained, but mass transfer rate is reduced due to steric restriction

Engineering Contradiction:
Improveshape selectivityVSAvoidmass transfer rate
Core Design Contradiction:
Stability of the object's compositionVSSpeed

Solution Approach 1:

The invention changes the size parameter of zeolite particles from conventional micrometer scale to nanometer scale (1-100 nm). This parameter change increases the surface area to volume ratio, improving mass transfer rate while preserving the crystalline structure that provides shape selectivity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention transitions from zero-dimensional bulk zeolite particles to low-dimensional nanoparticle structures. This dimensional change enables molecules to access active sites more easily while the internal pore structure maintains shape selectivity through steric restriction.

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

2Quantity of substance

If batch synthesis method is used, then zeolite particles are produced, but synthesis yield is low and crystallization time is long

Engineering Contradiction:
Improvesynthesis yieldVSAvoidcrystallization time
Core Design Contradiction:
Quantity of substanceVSLoss of time

Solution Approach 1:

The invention replaces batch synthesis with continuous flow synthesis using microfluidic technology. Reactants continuously flow through the system, enabling continuous nucleation and crystallization processes. This eliminates idle time between batches and maintains optimal reaction conditions continuously, significantly increasing synthesis yield and reducing crystallization time.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The continuous flow system segments the synthesis process into distinct zones within the microfluidic device: mixing zone, nucleation zone, and crystallization zone. This segmentation allows each process step to occur under optimized conditions simultaneously, improving overall efficiency and reducing total crystallization time.

Inventive Principle:
Principle #1Segmentation

3Manufacturing precision

If conventional synthesis routes are used, then zeolite particles are formed, but particle size and granulometric distribution are difficult to control

Engineering Contradiction:
Improveparticle size controlVSAvoidprocess control complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention utilizes precise control of flow rate parameters in the microfluidic system to control particle size. By adjusting the flow rates of reactants and residence time in the crystallization zone, particle size and distribution are precisely controlled at the nanometer scale without complex additional equipment.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The system incorporates real-time monitoring of synthesis conditions (temperature, pressure, flow rates) with feedback control mechanisms. This ensures consistent particle size and distribution by automatically adjusting parameters to maintain optimal conditions throughout the continuous synthesis process.

Inventive Principle:
Principle #23Feedback

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 system enables the rapid synthesis of zeolite nanoparticles with controlled particle size and distribution, enhancing catalytic performance by reducing mass transfer limitations while maintaining shape selectivity, thus increasing conversion capacity and refining efficiency.

Implementation Method 1

The need of improving analytical methods, making them capable of delivering reliable results quickly, gave rise to microfluidics, which since then has contributed significantly to technological innovations with miniaturized processes, precisely controlled and carried out in one operating time reduced when compared to other processes carried out in conventional ways.

Methodology Applied
Scientific EffectLaminar flow: Laminar Flow

Implementation Method 2

Another advantage of microfluidics lies in the operating conditions, such as the flow rate used in a miniaturized process and the reduced size of the cross-section of the microchannels, which induce a laminar flow, given the low Reynolds number (Re<1000). The interest in using microfluidic technology for both scientific and industrial applications has resulted in different configurations of microfluidic systems

Methodology Applied
Scientific EffectDiffusion: Diffusion

Implementation Method 3

a tubular hydrothermal system for carrying out a hydrothermal process

Methodology Applied
Scientific EffectHydrothermal process:

Implementation Method 4

tubular system heated to a temperature of 170° C. and pressurized at up to 15 bar (1.5 MPa), for carrying out a hydrothermal process

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS20230191355A1System and method for synthesis of zeolite nanoparticles in continuous flow with microfluidic micromixer
Publication Date: 2023.06.22 PETROLEO BRASILEIRO SA PETROBRAS
  • US20230191355A1 patent drawing
  • US20230191355A1 patent drawing
  • US20230191355A1 patent drawing

AI summary

The present invention refers to a system for the process of synthesis of zeolite nanoparticles in continuous flow wherein the processes of mixing, aging and crystallization are integrated, to reduce the synthesis time. The system has a microfluidic device of the 3D crossing channels micromixer type, consisting of microchannels built in series, used to generate the reaction mixture; buffer system with addition of seeds; and a heated tubular reactor which, in turn, is used for crystallization, which takes place through a continuous hydrothermal process.