Titanium Silicalite Zeolite Synthesis to Minimize TiO2 Formation

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Solution Overview

Problem

Existing zeolitic materials used for propylene oxide production, such as titanium silicalite-1 (TS-1), suffer from reduced catalytic performance and selectivity due to the formation of titanium dioxide (TiO2) during synthesis, which acts as a photosensitizer and interferes with the aldol condensation process, leading to decreased efficiency.

Innovation Solution

The synthesis of titanium silicalite-1 (TS-1) is optimized by using Ti-containing compounds with an APHA color number ≤ 300, minimizing the formation of TiO2 and aldol condensation products, thereby maintaining high selectivity and catalytic performance.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If Ti containing alcoholate is used as precursor for TS-1 synthesis, then Ti incorporation into zeolite framework is controlled, but TiO2 extra-framework formation occurs due to polymerization tendency

Engineering Contradiction:
ImproveTi incorporation controlVSAvoidTiO2 extra-framework formation
Core Design Contradiction:
Manufacturing precisionVSObject-generated harmful factors

Solution Approach 1:

Alcohols and ketones are introduced as intermediary substances that mediate between the Ti containing alcoholate precursor and the final zeolite structure. These intermediaries prevent direct polymerization of Ti species that would lead to TiO2 formation, while still allowing controlled Ti incorporation into the zeolite framework during synthesis.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The synthesis conditions are modified by changing chemical parameters - specifically adding alcohols and ketones to the reaction mixture. This alters the chemical environment during synthesis, suppressing the polymerization tendency of Ti species and reducing TiO2 formation while maintaining framework Ti incorporation.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If TiO2 is present in TS-1 catalyst, then photosensitization effect occurs, but catalytic performance and selectivity decrease

Engineering Contradiction:
Improvecatalytic performanceVSAvoidphotosensitization interference
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The invention addresses the harmful photosensitization effect of TiO2 by preventing its formation in the first place through controlled synthesis conditions. By using alcohols and ketones during synthesis, the harmful TiO2 extra-framework species are avoided, thereby eliminating their negative photosensitization interference while maintaining the desired catalytic framework structure.

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

3Productivity

If aldol condensation process is interfered with, then reaction efficiency decreases, but selectivity is maintained

Engineering Contradiction:
Improvereaction efficiencyVSAvoidselectivity
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The synthesis parameters are optimized by controlling the chemical environment with alcohols and ketones. This changes the physical-chemical parameters of the Ti species during synthesis, preventing premature condensation and TiO2 formation, thereby improving both reaction efficiency and selectivity of the final catalyst.

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

The optimized TS-1 catalyst achieves selectivity of ≥85% in propylene epoxidation with hydrogen peroxide, requiring lower reaction temperatures and maintaining efficiency over extended runtimes.

Implementation Method 1

TS-1 is usually hydrothermally synthesized, using a Ti containing alcoholate (alkoxide) precursor in order to get a controlled incorporation of Ti into the zeolite framework

Methodology Applied
Scientific EffectHydrolysis: Hydrolysis

Implementation Method 2

due to the strong polymerization tendency under aqueous conditions

Methodology Applied
Scientific EffectPolymerization:

Implementation Method 3

which acts as a photosensitizer and interferes with the aldol condensation process

Methodology Applied
Scientific EffectPhotosensitization:

Implementation Method 4

interferes with the aldol condensation process

Methodology Applied
Scientific EffectAldol condensation:

Data Source

PatentEP4126763B1Zeolitic material having a framework structure comprising si, o, and ti
Publication Date: 2026.01.28 BASF SE
  • EP4126763B1 patent drawingFigure 1
  • EP4126763B1 patent drawingFigure 2
  • EP4126763B1 patent drawingFigure 3

AI summary

The present invention relates to a zeolitic material having a framework structure comprising Si, O, and Ti, obtained or obtainable from a Ti containing compound, wherein the Ti containing compound has an APHA color number of ≤ 300. In a second aspect, the invention relates to the Ti containing compound having an APHA color number of ≤ 300. A third aspect of the present invention is related to the use of the Ti containing compound having an APHA color number of ≤ 300 of the second aspect for the preparation of a zeolitic material having framework structure comprising Si, O, and Ti, as well as to a process for preparation of a zeolitic material as in the first aspect having a framework structure comprising Si, O, and Ti, wherein the zeolitic material having a framework structure comprising Si, O, and Ti, is prepared from a Ti containing compound having an APHA color number of ≤ 300 as of the second aspect. A fourth aspect of the invention is directed to a molding comprising the zeolitic material having a framework structure comprising Si, O, and Ti as of the first aspect, as well as to the use of the molding as an adsorbent, an absorbent, a catalyst or a catalyst component. A fifth aspect of the invention relates to a process for oxidizing an organic compound comprising bringing an organic compound in contact with a catalyst comprising a molding as of the fourth aspect, wherein a sixth aspect relates to propylene oxide obtained or obtainable from the process according to the fifth aspect.