Molecular Sieve Crystallization Endpoint via Viscosity Monitoring

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Solution Overview

Problem

Conventional methods for synthesizing molecular sieves are inefficient in monitoring crystallization progress, leading to prolonged reaction times, inconsistent product properties, and unnecessary resource consumption, as they rely on time-consuming and labor-intensive powder X-ray diffraction analysis for determining the endpoint of the synthesis reaction.

Innovation Solution

Monitoring viscometric parameters such as viscosity and shear rate index of the reaction mixture allows for the early detection of the endpoint, enabling timely termination of the synthesis process and production of molecular sieves with desirable characteristics, using methods like periodic sampling and rheological analysis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If powder X-ray diffraction analysis is used to determine the endpoint of synthesis, then measurement precision is improved, but loss of time and productivity deteriorate

Engineering Contradiction:
Improvecrystallinity measurement accuracyVSAvoidtime for endpoint determination
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent replaces the mechanical/X-ray based powder diffraction analysis with a rheological measurement system that monitors viscosity changes in real-time. This substitution enables continuous monitoring without the time-consuming sample preparation and analysis steps required by XRD, thereby resolving the contradiction between measurement precision and time loss.

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

Solution Approach 2:

The patent implements continuous monitoring of reaction progress through real-time viscosity measurements, eliminating the intermittent sampling approach required by conventional XRD analysis. This continuous action allows for immediate detection of the crystallization endpoint, significantly reducing the time required while maintaining measurement accuracy.

Inventive Principle:
Principle #20Continuity of useful action

2Quantity of substance

If reaction time is extended to maximize product yield, then quantity of substance is improved, but loss of time and energy consumption worsen

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

Solution Approach 1:

The patent employs feedback control by continuously monitoring viscosity changes and using this information to determine the optimal endpoint for crystallization. This feedback mechanism prevents both premature termination (which would reduce yield) and excessive extension (which would waste time and energy), thereby maximizing product yield within the minimum necessary time.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent monitors changes in rheological parameters (viscosity, shear rate index) to detect the crystallization endpoint. By tracking these parameter changes in real-time, the process can be terminated at the optimal point when maximum yield is achieved, avoiding unnecessary extension of reaction time and associated energy consumption.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If reaction time is extended to ensure complete crystallization, then manufacturing precision is improved, but loss of time and energy consumption worsen

Engineering Contradiction:
Improvecrystal size consistencyVSAvoidenergy consumption for heating
Core Design Contradiction:
Manufacturing precisionVSUse of energy by stationary object

Solution Approach 1:

The patent uses feedback from real-time viscosity monitoring to determine when crystallization is complete and uniform. This allows the process to be terminated at the precise moment when desired crystal size consistency is achieved, preventing unnecessary energy consumption from extended heating while ensuring manufacturing precision is met.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent replaces conventional endpoint determination methods with rheological monitoring that provides real-time feedback on crystallization progress. This substitution enables precise control of the crystallization process, ensuring consistent crystal properties while minimizing energy consumption by avoiding excessive reaction times.

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

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 enables the consistent and efficient production of molecular sieves by predicting the endpoint of the reaction, reducing crystallization time, and optimizing crystal size, thereby improving energy efficiency and product quality.

Implementation Method 1

maintaining the reaction mixture under crystallization conditions

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 2

monitoring at least one viscometric parameter of the reaction mixture

Methodology Applied
Scientific EffectViscometry: Viscometer

Data Source

PatentEP2635526B9Method for preparing molecular sieves
Publication Date: 2021.12.15 CHEVRON USA INC
  • EP2635526B9 patent drawingFigure 1
  • EP2635526B9 patent drawingFigure 2
  • EP2635526B9 patent drawingFigure 3

AI summary

A method for synthesizing a molecular sieve comprising providing a reaction mixture sufficient to synthesize the molecular sieve, maintaining the reaction mixture under crystallization conditions, monitoring at least one viscometric parameter of the reaction mixture, and determining an endpoint based on the monitoring of the at least one viscometric parameter.