Organotemplate-Free LEV Zeolite Synthesis via Seed Crystallization

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Solution Overview

Problem

The production of LEV-type zeolites is cost-intensive and environmentally harmful due to the need for high-temperature calcination to remove organotemplates, which limits the types of architectures that can be produced and results in energy consumption and waste products.

Innovation Solution

A process for synthesizing organotemplate-free zeolitic materials with an LEV-type framework structure using seed crystals, eliminating the need for calcination and reducing costs by avoiding the use of expensive organotemplates and minimizing waste, while maintaining the zeolite's architecture and enhancing its properties for catalytic and adsorption applications.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If organotemplates are used as structure directing agents in LEV-type zeolite synthesis, then the zeolite framework structure can be formed, but the synthesis becomes cost-intensive and requires subsequent removal of the organotemplate through calcination

Engineering Contradiction:
Improvezeolite framework structure formationVSAvoidsynthesis cost
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The invention extracts and eliminates the organotemplate component from the synthesis system entirely. By using diethyldimethylammonium hydroxide as a simple, inexpensive alternative to complex organotemplates like quinuclidine derivatives, the patent removes the need for costly template materials while still achieving LEV-type framework formation through alternative structure-directing mechanisms

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent replaces expensive, complex organotemplates with a cheap, simple ammonium compound (diethyldimethylammonium hydroxide) that can be easily discarded after synthesis without requiring removal. This disposable approach eliminates both the cost of expensive templates and the energy-intensive calcination process needed to remove them

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Loss of substance

If calcination is performed to remove organotemplates from the zeolite structure, then the organotemplate can be eliminated, but energy consumption increases and harmful waste products are generated

Engineering Contradiction:
Improveorganotemplate removalVSAvoidcalcination energy consumption
Core Design Contradiction:
Loss of substanceVSLoss of energy

Solution Approach 1:

The patent converts the potential harm of organotemplate presence into a benefit by selecting a template (diethyldimethylammonium hydroxide) that decomposes cleanly and completely under mild drying conditions, leaving no residual carbonaceous material. The 'harm' of having an organic template is transformed into the benefit of complete decomposition without requiring energy-intensive calcination

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The invention extracts the problematic calcination step from the synthesis protocol. By using a simple ammonium compound instead of complex organotemplates, the patent removes the need for high-temperature treatment, eliminating both energy consumption and harmful waste generation while still achieving complete template removal

Inventive Principle:
Principle #2Taking out (Extraction)

3Loss of substance

If high-temperature calcination is used to remove organotemplates, then complete removal is achieved, but the zeolite architecture may be damaged and recycling of materials is prevented

Engineering Contradiction:
Improvecomplete organotemplate removalVSAvoidzeolite architecture integrity
Core Design Contradiction:
Loss of substanceVSStability of the object's composition

Solution Approach 1:

The patent changes the thermal parameters from high-temperature calcination (450-930°C) to mild drying conditions. By selecting a template with appropriate chemical properties (diethyldimethylammonium hydroxide) that decomposes at low temperatures, the patent achieves complete template removal while preserving the zeolite framework through gentle thermal treatment

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The use of a simple, disposable ammonium compound template that decomposes completely under mild conditions allows for template removal without harsh treatment. The template is designed to be transient and completely removable through simple drying, preserving the zeolite structure while achieving complete template elimination

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

4Loss of substance

If decomposition of organic template material occurs during hydrothermal synthesis, then the template can be broken down, but reaction vessels must display high pressure resistance and material recycling is limited

Engineering Contradiction:
Improvetemplate decompositionVSAvoidreaction vessel pressure resistance
Core Design Contradiction:
Loss of substanceVSDevice complexity

Solution Approach 1:

The patent changes the decomposition conditions from high-pressure hydrothermal decomposition to low-pressure atmospheric drying. By selecting a template that decomposes at low temperatures, the patent eliminates the need for pressure-resistant equipment while still achieving complete template breakdown and removal

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 allows for the production of zeolites with novel properties and high Al content, achieving shorter reaction times, reduced energy consumption, and lower costs, with the ability to recycle materials and avoid harsh thermal treatments, resulting in a more efficient and environmentally friendly synthesis method.

Implementation Method 1

crystallizing the mixture obtained in step (1)

Methodology Applied
Scientific EffectCrystallisation: Crystallisation

Data Source

PatentEP2582625B1Organotemplate-free synthetic process for the production of a zeolitic material of the LEV-type structure, zeolitic material thus obtained and use thereof
Publication Date: 2017.03.22 BASF SE
  • EP2582625B1 patent drawingFigure 1A
  • EP2582625B1 patent drawingFigure 1B
  • EP2582625B1 patent drawingFigure 2A

AI summary

The present invention relates to an organotemplate-free synthetic process for the production of a zeolitic material having an LEV-type framework structure comprising YO2 and optionally comprising X2O3, wherein said process comprises the steps of (1) preparing a mixture comprising seed crystals and one or more sources for YO2; and (2) crystallizing the mixture obtained in step (1); wherein Y is a tetravalent element, and X is a trivalent element, wherein the zeolitic material optionally comprises one or more alkali metals M, and wherein the seed crystals comprise zeolitic material having an LEV-type framework structure, and to a zeolitic material having an LEV-type framework structure obtainable by said process, as well as to an organotemplate-free zeolitic material having an LEV-type framework structure comprising YO2 and optionally comprising X2O3, wherein Y is a tetravalent element, and X is a trivalent element, wherein the zeolitic material optionally comprises one or more alkali metals M, wherein said zeolitic material is non-calcined.