Continuous Zeolite Synthesis via Controlled Fluid Flow

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Solution Overview

Problem

Continuous zeolite synthesis processes face challenges such as fouling of equipment, inconsistent crystallization times, and difficulties in achieving high-quality crystals, particularly when producing zeolites with crystal sizes greater than a hundred nanometers, due to the presence of solids in the reaction medium.

Innovation Solution

A completely continuous zeolite synthesis process is developed, where a gel is continuously prepared and crystallized without a batch mode phase, utilizing specific stirring conditions characterized by relative Reynolds numbers between 40 and 50,000 and net Reynolds numbers between 1 and 1500, which reduces the risk of fouling and allows for the production of high-quality zeolite crystals.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If a continuous synthesis process is implemented with solids in the reaction medium, then productivity and energy efficiency are improved, but the risk of fouling and equipment blocking increases

Engineering Contradiction:
Improvecontinuous production capabilityVSAvoidequipment fouling risk
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent applies ultrasonic vibration (20-100 kHz frequency range) to the continuous synthesis reactor to prevent fouling and blocking caused by solid accumulation. The vibration energy disrupts solid deposits on reactor walls and maintains flow continuity, enabling reliable continuous operation while producing high-quality zeolite crystals.

Inventive Principle:
Principle #18Mechanical vibration

Solution Approach 2:

The patent implements precise control of flow rates, temperature gradients, and residence times in the continuous synthesis process. By optimizing these parameters, the process achieves complete crystallization within the continuous reactor while preventing solid accumulation that would cause fouling, thus maintaining both productivity and reliability.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If crystallization time is extended to produce larger crystals, then crystal quality is improved, but the reactor size and investment costs increase

Engineering Contradiction:
Improvecrystal quality and size uniformityVSAvoidreactor volume
Core Design Contradiction:
Manufacturing precisionVSVolume of stationary object

Solution Approach 1:

The patent uses a continuous synthesis process where the reaction medium flows continuously through the reactor with controlled residence time. This continuous action allows complete crystallization to occur within a compact reactor volume, producing high-quality crystals without requiring large reactor sizes or extended batch times.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent implements dynamic control of flow rates and residence times to optimize crystal growth. By adjusting the residence time of the reaction medium in the reactor, the process can produce crystals of desired size and quality while maintaining a compact reactor footprint, avoiding the need for oversized equipment.

Inventive Principle:
Principle #15Dynamics

3Device complexity

If conventional batch reactors are used for zeolite synthesis, then equipment simplicity is maintained, but energy expenditure and equipment size are excessive

Engineering Contradiction:
Improvereactor system simplicityVSAvoidheating energy consumption
Core Design Contradiction:
Device complexityVSUse of energy by stationary object

Solution Approach 1:

The patent employs a continuous flow system where the reaction medium is pumped through the reactor, replacing the need for large batch reactors with heating jackets. The hydraulic flow system enables efficient heat transfer and reduces the energy required for heating, while the modular continuous reactor design maintains operational simplicity.

Inventive Principle:
Principle #29Pneumatics and hydraulics

4Speed

If high-temperature pressurized water is used for ZSM-5 crystallization, then crystallization speed is improved, but equipment complexity and maintenance requirements increase

Engineering Contradiction:
Improvecrystallization rateVSAvoidpressure system complexity
Core Design Contradiction:
SpeedVSDevice complexity

Solution Approach 1:

The patent optimizes the temperature and pressure parameters in the continuous synthesis process to achieve fast crystallization without requiring extreme conditions. By carefully controlling the residence time and using moderate temperature gradients, the process achieves high crystallization rates with simpler equipment that has lower maintenance requirements.

Inventive Principle:
Principle #35Parameter changes

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 process enables the industrial-scale, continuous production of zeolite crystals with improved equipment control, energy efficiency, and uniformity, while minimizing fouling and maintaining excellent crystal quality, making it suitable for various zeolite types, including MFI and FAU types.

Implementation Method 1

giving said composition a flow characterized by a relative Reynolds number Rer of between 40 and 50 000, preferably between 40 and 25 000, more preferably between 70 and 5000, typically between 100 and 2000

Methodology Applied
Scientific EffectTurbulence: Turbulence

Implementation Method 2

continuous introduction of said composition into at least one crystallization reaction zone subjected to stirring means

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS11040884B2Process for continuously synthesizing zeolite crystals
Publication Date: 2021.06.22 ARKEMA FRANCE SA
  • US11040884B2 patent drawing

AI summary

The present invention relates to a process for preparing zeolite crystals continuously, comprising the continuous introduction of a composition capable of generating zeolite crystals into at least one crystallization reaction zone subjected to stirring means, giving said composition a flow characterized by a relative Reynolds number Rer of between 40 and 50 000, and the continuous recovery of the crystals formed according to a flow characterized by a net Reynolds number Ren of between 1 and 1500.