ETS-10 Synthesis Using Titanium Oxide Hydrosol

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Solution Overview

Problem

Conventional synthesis methods for ETS-10 titanosilicate molecular sieves face challenges with unstable titanium sources, poor repeatability, and the presence of stray crystals due to the properties of titanium sources like TiCl3, TiCl4, TiOSO4, and TiO2, which affect the purity and crystallinity of the product.

Innovation Solution

The method involves using titanium oxide hydrosol as a titanium source, which is more stable and easily dispersible, allowing for the synthesis of ETS-10 titanosilicate molecular sieves by mixing titanium oxide hydrosol with a silicon source, sodium hydroxide, a fluorine-containing mineralizer, and water, and adjusting the pH before hydrothermal crystallization.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional titanium sources (TiCl3, TiCl4, TiOSO4, TiO2) are used for synthesis, then the synthesis process can be carried out, but the product purity and crystallinity deteriorate due to stray crystal formation and poor repeatability

Engineering Contradiction:
Improveproduct purity and crystallinityVSAvoidsynthesis repeatability
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent changes the chemical state of titanium from solid or gaseous forms to a colloidal sol form, which fundamentally alters the reactivity and dispersion characteristics. This parameter change enables uniform distribution of titanium species throughout the gel matrix, preventing localized precipitation and stray crystal formation, thereby improving both product purity and synthesis repeatability

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The titanium sol acts as an intermediary form between conventional titanium sources and the final molecular sieve structure. This intermediate colloidal state provides controlled reactivity and uniform nucleation, eliminating the harmful effects of direct precipitation from solid or gaseous titanium sources while maintaining the desired crystallization process

Inventive Principle:
Principle #24Intermediary (Mediator)

2Productivity

If trivalent titanium sources (TiCl3) are used, then synthesis can proceed, but synthesis efficiency deteriorates due to indirect hydrolysis requirements and operational complexity increases

Engineering Contradiction:
Improvesynthesis efficiencyVSAvoidoperational complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent extracts the problematic hydrolysis step from the synthesis pathway by using tetravalent titanium sources that do not require indirect hydrolysis conversion. This eliminates the need for complex operational controls and intermediate conversion steps, directly improving synthesis efficiency and reducing operational complexity

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The titanium sol is prepared in advance with controlled hydrolysis characteristics, so that when mixed with the gel precursors, the titanium species are already in the appropriate state for direct incorporation into the molecular sieve structure. This preliminary preparation eliminates subsequent complex processing steps

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If nanoscale TiO2 (P25) is used as titanium source, then synthesis effect is improved, but cost increases making it unsuitable for industrial application

Engineering Contradiction:
Improvesynthesis effectVSAvoidsynthesis cost
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The patent replaces expensive nanoscale TiO2 with a cost-effective titanium sol that can be prepared from conventional titanium sources. The sol provides comparable or superior performance to nanoscale TiO2 while being significantly cheaper and suitable for large-scale industrial production

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

Solution Approach 2:

The invention creates a composite colloidal system where titanium oxide species are dispersed in a liquid medium with controlled rheological and chemical properties. This composite form combines the advantages of nanoscale dispersion with the cost benefits of conventional titanium sources, achieving both high synthesis effect and cost-effectiveness

Inventive Principle:
Principle #40Composite materials

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 results in high-purity, high-crystallinity ETS-10 titanosilicate molecular sieves with improved synthesis efficiency and reduced stray crystal formation, simplifying the operational process.

Implementation Method 1

mixing a titanium oxide hydrosol, a silicon source, a sodium hydroxide, a fluorine-containing mineralizer and a water to give a gel

Methodology Applied
Scientific EffectSol-gel process: Gel

Implementation Method 2

hydrothermal crystallizing the gel at 170 to 250° C. for 10 to 100 hours to obtain the ETS-10 titanosilicate molecular sieve

Methodology Applied
Scientific EffectHydrothermal crystallization: Crystallisation

Data Source

PatentUS9382124B2Synthesis method for ETS-10 titanosilicate molecular sieve
Publication Date: 2016.07.05 CHINA NAT PETROLEUM CORP
  • US9382124B2 patent drawing
  • US9382124B2 patent drawing
  • US9382124B2 patent drawing

AI summary

The present invention relates to a synthesis method for ETS-10 titanosilicate molecular sieves. The method comprises the steps of mixing a titanium oxide hydrosol, a silicon source, a sodium hydroxide, a fluorine-containing mineralizer and a water to give a gel and adjusting the pH thereof to 10.4 to 10.8; and hydrothermal crystallizing the gel at 170 to 250° C. for 10 to 100 hours to obtain the ETS-10 titanosilicate molecular sieves. In the synthesis method for ETS-10 titanosilicate molecular sieves provided by the present invention, a titanium oxide hydrosol is used as the titanium source to synthesize the ETS-10 titanosilicate molecular sieves, and the problem that conventional soluble titanium salt-based titanium sources tend to hydrolyze and the problem of poor dispersibility for the titanium source system of insoluble titanium oxide are therefore prevented. The ETS-10 titanosilicate molecular sieves synthesized has high purity and high crystallinity.