Ga-Zn Silicate Crystallization via Si-RUB-39 Seeding

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Solution Overview

Problem

Current methods for preparing microporous framework silicates, such as those described in WO 2005/100242 A1, require lengthy crystallization times, often exceeding 15 days, especially when using the RUB-39 structure without a crystallization assistant, which hinders their practical application in chemical production and purification processes.

Innovation Solution

A process involving the preparation of a colloidal aqueous solution with silicon dioxide, tetraalkylammonium compounds, a base, and a heteroatom source, followed by hydrothermal crystallization using a silicate with the Si-RUB-39 structure as a crystallization assistant, significantly reduces crystallization time to less than 10 days by incorporating Ga and/or Zn into the silicate lattice.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If no crystallization assistant is used in the hydrothermal synthesis of microporous framework silicates, then the synthesis process is simpler, but the crystallization time becomes excessively long (15 to 45 days)

Engineering Contradiction:
Improvesynthesis process simplicityVSAvoidcrystallization time
Core Design Contradiction:
Ease of manufactureVSLoss of time

Solution Approach 1:

A silicate with the Si-RUB-39 structure is introduced as a crystallization assistant (seeding agent) to mediate the hydrothermal synthesis process. This intermediary substance provides nucleation sites that accelerate the crystallization of Ga- and Zn-comprising silicates, reducing the crystallization time from 15-45 days to a much shorter period without complicating the overall synthesis procedure.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Adaptability or versatility

If Ga and Zn are incorporated into the silicate lattice, then the catalytic and adsorptive properties are enhanced, but the crystallization process becomes more complex

Engineering Contradiction:
Improvecatalytic and adsorptive propertiesVSAvoidcrystallization process complexity
Core Design Contradiction:
Adaptability or versatilityVSDevice complexity

Solution Approach 1:

The crystallization process parameters (temperature, pressure, time, and composition) are optimized to enable the incorporation of Ga and Zn heteroatoms into the silicate lattice. By carefully controlling these parameters and using the Si-RUB-39 structure as a crystallization assistant, the process achieves the desired heteroatom incorporation for enhanced catalytic and adsorptive properties while maintaining manageable process complexity.

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 efficiently shortens the hydrothermal crystallization time for Ga- and Zn-comprising silicates, enabling their use as molecular sieves, adsorbents, and catalysts, thereby enhancing their applicability in chemical production and purification processes.

Implementation Method 1

hydrothermally crystallizing by heating the colloidal aqueous solution obtained in (1) to a temperature in the range from greater than the boiling temperature of the colloidal aqueous solution under the selected pressure to 180° C. at standard pressure to obtain a suspension comprising at least one silicate

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 2

hydrothermally crystallizing by heating the colloidal aqueous solution obtained in (1) to a temperature in the range from greater than the boiling temperature of the colloidal aqueous solution under the selected pressure to 180° C. at standard pressure

Methodology Applied
Scientific EffectHydrothermal synthesis:

Data Source

PatentUS10226763B2Process for preparing a heteroatom-comprising silicate
Publication Date: 2019.03.12 BASF SE
  • US10226763B2 patent drawing
  • US10226763B2 patent drawing
  • US10226763B2 patent drawing

AI summary

The present invention relates to a process for preparing at least one sheet silicate comprising Ga and/or Zn, and based thereon, a framework silicate, preferably of the RRO structure type, to the sheet silicate and framework silicate themselves and to the uses of the silicates, especially of the framework silicate, preferably as catalysts.