ChemInform Abstract: Analysis of Active Site Distribution in ZSM-5 Crystals by IR Microscopy.

Controlling the spatial distribution of aluminum in ZSM-5 crystals

Abstract The spatial distribution of aluminum over ZSM-5 crystals was systematically studied using electron microprobing on polished crystals. Crystals synthesized with TPABr as template exhibit a pronounced enrichment of aluminum in the crystal rim, essentially irrespective of the aluminum source employed, although aluminum sources with organic anions are favoring less inhomogeneous profiles. With 1,6-hexanediol or from totally inorganic reaction gels, crystals with completely homogeneous aluminum profiles are obtained, even if the crystals grow larger than 50 μm. In the 1,6-hexanediol system the homogeneous profiles could be changed to profiles similar to the TPABr system by addition of K…

Analysis of Active-Site Distribution in ZSM-5 Crystals by Infrared Microscopy

Abstract The acid Site distribution over large ZSM-5 crystals was analyzed using FTIR microscopy. Results of the analysis of the OH-stretching vibrations and of vibrations of pyridine adsorbed on Bronsted and Lewis acid sites were found to be in good agreement. The resolution which can be obtained using this novel technique is about 10-20 μm. This limits the application to large crystals as analyzed in this study. Comparison of the results of IR microscopy with aluminum distributions obtained by electron microprobe analysis revealed that IR microscopy cannot resolve inhomogeneities on a scale smaller than the above-stated limits. The results of both methods on a larger scale, however. are i…

Is the formation of a zeolite from a dry powder via a gas phase transport process possible?

Abstract ZSM-5 was synthesized by four methods with a gradually decreasing water content ending in a reaction mixture with absolutely dry reagents in the form of a powder in the complete absence of a solution phase. Amorphous precursors obtained by drying SiO2·A2O3 gels at 650°C were transformed into zeolites in the presence of dried NH4F and TPABr. Some water is probably formed as a reaction product, but the maximum water pressure is appreciably below the saturation pressure under the given reaction conditions. To explain the formation of a zeolite, we suggest a vapor phase mass transfer process with SiF4 as the mobile species between the solid phase, which contains the amorphous Si/Al pre…

The synthesis of zeolites from dry powders

Summary ZSM-5 was synthesized by different methods with a gradually decreasing water content ending in a reaction mixture with absolutely dry reagents in form of a powder in the complete absence of a solution phase. Amorphous precursors obtained by drying SiO 2 * Al 2 O 3 gels at 650°C were transformed into zeolites in the presence of dried NH 4 F and TPABr. The reaction products were characterized by XRD, REM, TG/DTA, MAS NMR and Electron Micropobe. Pure ZSM-5 or Silicalite-1 was obtained in all cases. Some water is probably formed as a reaction product, but the maximum water pressure is appreciably below the saturation pressure at the given reaction conditions. To explain the formation of…