Isomorphously Substituted Silicate Synthesis via Two-Step Hydrothermal Crystallization

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Solution Overview

Problem

Current processes for preparing isomorphously substituted silicates, such as RUB-39 and RUB-36, face challenges in achieving high purity, crystallinity, and yield, particularly in industrial applications, where efficient and tailored materials are needed for catalysis and adsorption.

Innovation Solution

A two-step hydrothermal crystallization process is employed, starting with a mixture of silica, a structure directing agent, and water, followed by the addition of a source for isomorphous substitution, allowing for the incorporation of elements like aluminum into the silicate framework, enhancing the crystallization process and product quality.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If a one-step hydrothermal crystallization process is used to prepare isomorphously substituted silicates, then the process is simpler and faster, but the product purity and crystallinity are insufficient

Engineering Contradiction:
Improveprocess speedVSAvoidproduct purity and crystallinity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The synthesis process is divided into two distinct stages: (1) hydrothermal crystallization of the layered silicate framework without aluminum source, and (2) subsequent ion exchange or hydrothermal treatment to introduce aluminum into the framework. This segmentation allows each stage to optimize for its specific function, achieving both high crystallinity in the framework and controlled aluminum substitution, thereby resolving the contradiction between process simplicity and product quality.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The layered silicate framework is pre-formed through hydrothermal crystallization before introducing the aluminum source. This preliminary action ensures that the silicate framework achieves optimal crystallinity and structural order first, and then aluminum is incorporated through controlled substitution, preventing interference with framework formation and ensuring high product purity.

Inventive Principle:
Principle #10Preliminary action

2Quantity of substance

If aluminum source is added at the beginning of hydrothermal treatment, then aluminum incorporation occurs, but the crystallinity and purity of the silicate framework are compromised

Engineering Contradiction:
Improvealuminum incorporationVSAvoidframework crystallinity
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The silicate framework is crystallized in advance without aluminum present, allowing the framework to form with optimal structural order and crystallinity. Only after the framework is established does aluminum introduction occur through ion exchange or secondary hydrothermal treatment, ensuring that aluminum incorporation does not disrupt framework formation and both crystallinity and aluminum content requirements are met.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The synthesis is separated into framework formation stage (without aluminum) and aluminum incorporation stage (after framework formation). This temporal segmentation prevents aluminum from interfering with the delicate crystallization process while still achieving the desired aluminum substitution in the final product, resolving the contradiction between aluminum content and framework crystallinity.

Inventive Principle:
Principle #1Segmentation

3Productivity

If industrial-scale production requires high efficiency, then process time is reduced, but product quality (purity, crystallinity) deteriorates

Engineering Contradiction:
Improveindustrial efficiencyVSAvoidproduct quality consistency
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The two-stage process allows industrial production to optimize each stage independently: the first stage (framework crystallization) can be run at high temperature and pressure for rapid crystal growth, while the second stage (aluminum incorporation) can be performed under milder conditions to ensure complete substitution. This segmentation enables scalable industrial production while maintaining consistent high product quality across batches.

Inventive Principle:
Principle #1Segmentation

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 results in higher purity and crystallinity of isomorphously substituted layered silicates, improving their suitability for industrial applications, including catalysis and adsorption, by allowing for precise control of the silicate structure and elemental substitution.

Implementation Method 1

heating the mixture obtained according to (1) under hydrothermal conditions to give a precursor suspension

Methodology Applied
Scientific EffectHydrothermal crystallization: Crystallisation

Implementation Method 2

adding at least one source of at least one element suitable for isomorphous substitution of at least a portion of the Si atoms in the layered silicate

Methodology Applied
Scientific EffectIsomorphous substitution:

Data Source

PatentEP2403641B1Process for the preparation of an isomorphously substituted silicate
Publication Date: 2014.07.16 BASF SE
  • EP2403641B1 patent drawingFigure 1
  • EP2403641B1 patent drawingFigure 2
  • EP2403641B1 patent drawingFigure 3

AI summary

A process for the preparation of an isomorphously substituted layered silicate comprising (1) providing a mixture containing silica or a precursor thereof, at least one structure directing agent (SDA) allowing for the crystallization of the layered silicate, and water; (2) heating the mixture obtained according to (1) under hydrothermal conditions; (3) adding at least one source at least one element suitable for isomorphous substitution; (4) heating the mixture obtained according to (3) under hydrothermal conditions.