Synthesis of mesoporous zeolite single crystals with cheap porogens

Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals have been successfully synthesized by adding soluble starch or sodium carboxymethyl cellulose (CMC) to a conventional zeolite synthesis system. The obtained samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen sorption analysis, 27Al magic angle spinning nuclear magnetic resonance (27Al MAS NMR), temperature-programmed desorption of ammonia (NH3-TPD) and ultraviolet–visible spectroscopy (UV–vis). The SEM images clearly show that all zeolite crystals possess the similar morphology with particle size of about 300 nm, the TEM images reveal that irregular intracrystal pores are randomly distributed in the whole crystal. 27Al MAS NMR spectra indicate that nearly all of the Al atoms are in tetrahedral co-ordination in ZSM-5, UV–vis spectra confirm that nearly all of titanium atoms are incorporated into the framework of TS-1. The catalytic activity of meso-ZSM-5 in acetalization of cyclohexanone and meso-TS-1 in hydroxylation of phenol was also studied. The synthesis method reported in this paper is cost-effective and environmental friendly, can be easily expended to prepare other hierarchical structured zeolites.

Mesoporous zeolite single crystals were synthesized by using cheap porogens as template.Figure optionsDownload as PowerPoint slideHighlights
► Mesoporous zeolite (silicalite-1, ZSM-5, TS-1) single crystals were synthesized.
► Soluble starch or sodium carboxymethyl cellulose (CMC) was used as porogens.
► The mesoporous zeolites had connected mesopores although closed pores existed.
► Higher catalytic activities were obtained.