Zeolite X Synthesis via Seeding and High Temperature

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Solution Overview

Problem

Current industrial synthesis methods for FAU X-type zeolite crystals are limited by long synthesis times and the formation of impurities like zeolite P and A at higher temperatures, making it challenging to achieve high-purity crystals efficiently.

Innovation Solution

Incorporating a seeding agent into the synthesis gel and conducting the crystallization at temperatures greater than 120°C, allowing for the elimination of the low-temperature maturing phase and enabling the use of hotter reagents to significantly reduce synthesis time while maintaining high crystallinity and purity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If zeolite X is synthesized at higher temperatures to reduce synthesis time, then productivity is improved, but impurity phases (zeolite P and A) form reducing manufacturing precision

Engineering Contradiction:
Improvesynthesis timeVSAvoidcrystal purity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent applies preliminary action by adding seeding agents (zeolite X crystals or nuclei) before the crystallization phase. This pre-introduction of crystalline templates guides the reaction to form only the desired zeolite X phase even at high temperatures, preventing impurity formation from the outset and enabling faster synthesis without sacrificing purity.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent changes the temperature parameter from conventional low temperatures (25-40°C) to high temperatures (120-200°C) while maintaining product purity through the combined effect of seeding agents and optimized alkalinity. This parameter change dramatically reduces synthesis time while the seeding mechanism ensures selective formation of zeolite X phase.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If conventional low-temperature synthesis is used to ensure high crystal purity, then manufacturing precision is improved, but synthesis duration increases reducing productivity

Engineering Contradiction:
Improvecrystal purityVSAvoidsynthesis time
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent fundamentally changes the temperature parameter from conventional low temperatures (25-40°C) to high temperatures (120-200°C). This parameter change accelerates the crystallization kinetics dramatically, reducing synthesis time from days to hours or minutes, while the seeding mechanism maintains high purity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent enables continuous synthesis processes by eliminating the separate low-temperature maturing phase. The high-temperature crystallization with seeding agents produces mature, high-purity crystals directly in a single continuous operation, maximizing productivity without compromising purity.

Inventive Principle:
Principle #20Continuity of useful action

3Productivity

If high temperature synthesis is attempted without seeding agents, then productivity is improved through faster reaction kinetics, but the metastable zeolite X phase cannot form selectively and impurity phases dominate reducing manufacturing precision

Engineering Contradiction:
Improvereaction rateVSAvoidphase selectivity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The seeding agents act as intermediaries that mediate between the high-temperature reaction conditions and the selective formation of zeolite X phase. These pre-formed crystal templates or nuclei provide a pathway for selective crystallization, guiding the reaction to form only the desired phase even under conditions that would otherwise produce impurities.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent applies preliminary action by pre-introducing zeolite X seeding agents before the high-temperature crystallization. This preliminary presence of the target phase template ensures that crystallization proceeds selectively toward zeolite X formation, overcoming the thermodynamic tendency toward impurity phases at high temperatures.

Inventive Principle:
Principle #10Preliminary 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

This approach enables the production of high-purity zeolite X crystals with crystallinity greater than 98% and reduced synthesis duration, achieving faster and more energy-efficient continuous synthesis.

Implementation Method 1

by carrying out seeding by adding seeding agent(s) into the synthesis gel, it is possible to form zeolite X crystals at a temperature greater than 120° C.

Methodology Applied
Scientific EffectNucleation: Nucleation

Implementation Method 2

forming zeolite X crystals after the crystallization phase carried out at higher temperature

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentUS10850988B2Process for synthesizing zeolite crystals with seeding agent
Publication Date: 2020.12.01 ARKEMA FRANCE SA

AI summary

The present invention relates to process for synthesizing zeolite X crystals comprising at least one step of adding seeding agent(s) into a synthesis gel and at least one step of forming zeolite X crystals at a temperature strictly greater than 120° C., preferably equal to or greater than 130° C.