Continuous Zeolite Synthesis via LHSV and Temperature Control

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Solution Overview

Problem

Current continuous processes for synthesizing zeolitic materials face limitations in achieving efficient and prolonged operation due to clogging issues and limited reduction of reaction times, especially on an industrial scale, despite advancements in reactor geometries and flow methodologies.

Innovation Solution

A continuous process involving a specific range of liquid hourly space velocities in continuous flow reactors, with a mixture of YO2, optionally X2O3, and a liquid solvent system, is used to crystallize zeolitic materials at temperatures between 100 to 300°C, allowing for extended operation periods and improved properties such as purity and crystallinity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If continuous flow reactors are used for synthesizing zeolitic materials, then reaction time is reduced and productivity is improved, but clogging occurs limiting extended operation

Engineering Contradiction:

Improvereaction timeVSAvoidcontinuous operation

Core Design Contradiction:

ProductivityVSReliability

Solution Approach 1:

The patent applies dynamic control of reaction parameters including liquid hourly space velocity (LHSV) adjustments and temperature modulation (100-300°C) to maintain optimal crystallization conditions while preventing clogging. The system dynamically adapts operating conditions to sustain continuous operation without interruption.

Inventive Principle:

Principle #15Dynamics

Solution Approach 2:

The invention utilizes parameter changes by optimizing LHSV ranges and temperature profiles to control zeolite crystallization kinetics. By adjusting these parameters, the process achieves both reduced reaction time and prevention of reactor clogging, enabling reliable continuous operation.

Inventive Principle:

Principle #35Parameter changes

2Reliability

If batch synthesis is used for zeolitic materials, then reaction conditions can be maintained, but space-time-yield is low and operation is discontinuous

Engineering Contradiction:

Improvereaction condition stabilityVSAvoidspace-time-yield

Core Design Contradiction:

ReliabilityVSProductivity

Solution Approach 1:

The patent implements continuous flow processing where reactants continuously flow through the reactor system, maintaining steady-state crystallization conditions. This continuous action eliminates batch interruptions while sustaining optimal reaction conditions, achieving both high space-time-yield and reliable operation.

Inventive Principle:

Principle #20Continuity of useful action

Solution Approach 2:

The invention replaces mechanical batch processing (loading, heating, stirring, unloading cycles) with a continuous flow system where reactants are pumped through the reactor. This substitution eliminates the discontinuous mechanical operations of batch processing while maintaining controlled reaction conditions.

Inventive Principle:

Principle #28Mechanics substitution (Replace mechanical system)

3Productivity

If multiple stage reactors are employed to increase efficiency, then productivity improves, but device complexity increases

Engineering Contradiction:

Improvereaction efficiencyVSAvoidreactor configuration

Core Design Contradiction:

ProductivityVSDevice complexity

Solution Approach 1:

The patent segments the continuous flow reactor into multiple zones or stages within a single reactor vessel, each optimized for specific crystallization requirements. This segmentation achieves high reaction efficiency while avoiding the complexity of multiple separate reactor units.

Inventive Principle:

Principle #1Segmentation

Solution Approach 2:

The invention merges multiple reaction stages into a single continuous flow reactor system, combining crystallization, growth, and maturation zones in one integrated apparatus. This merging achieves high productivity while simplifying the overall device configuration compared to multiple separate reactors.

Inventive Principle:

Principle #5Merging (Combining)

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 uninterrupted operation on an industrial scale, enhancing space-time-yield levels and resulting in zeolitic materials with improved purity and crystallinity, surpassing conventional methods in efficiency and product quality.

Implementation Method 1

crystallizing the zeolitic material from the mixture in the continuous flow reactor

Methodology Applied

Scientific EffectCrystallization: Crystallisation

Implementation Method 2

wherein the mixture is heated to a temperature in the range of from 100 to 300°C

Methodology Applied

Scientific EffectHeating: Heating

Data Source

PatentUS11046587B2Process for a continuous synthesis of zeolitic materials

Publication Date: 2021.06.29 BASF MOBILE EMISSIONS CATALYSTS LLC

AI summary

A continuous process for preparing a zeolitic material comprising (i) preparing a mixture comprising a source of YO2, optionally a source of X2O3, and a liquid solvent system; (ii) continuously feeding the mixture prepared in (i) into a continuous flow reactor at a liquid hourly space velocity in the range of from 0.3 to 20 h−1 for a duration of at least 1 h; and (iii) crystallizing the zeolitic material from the mixture in the continuous flow reactor, wherein the mixture is heated to a temperature in the range of from 100 to 300° C.; wherein the volume of the continuous flow reactor is in the range of from 150 cm3 to 75 m3, as well as to zeolitic materials which may be obtained according to the inventive process and to their use.