Synthesis of mesoporous zeolite single crystals with cheap porogens

Journal Article · Fri Jul 15 04:00:00 EDT 2011 · Journal of Solid State Chemistry

OSTI ID:21580167

Haixiang, Tao; Changlin, Li; Jiawen, Ren ^[1]

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1. Key Laboratory for Advanced Materials, Research Institute of Industrial Catalysis, East China University of Science and Technology, Shanghai 200237 (China)

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, {sup 27}Al magic angle spinning nuclear magnetic resonance ({sup 27}Al MAS NMR), temperature-programmed desorption of ammonia (NH{sub 3}-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. {sup 27}Al 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. - Graphical abstract: Mesoporous zeolite single crystals were synthesized by using cheap porogens as template. Highlights: > 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.

• OSTI ID: 21580167
• Journal Information: Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Journal Issue: 7 Vol. 184; ISSN 0022-4596; ISSN JSSCBI
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
ALUMINIUM 27
ALUMINIUM ISOTOPES
AMMONIA
CARBOHYDRATES
CELLULOSE
COHERENT SCATTERING
CRYSTALS
DESORPTION
DIFFRACTION
ELECTRON MICROSCOPY
FOURIER TRANSFORM SPECTROMETERS
FOURIER TRANSFORMATION
HYDRIDES
HYDROGEN COMPOUNDS
INFRARED SPECTRA
INORGANIC ION EXCHANGERS
INTEGRAL TRANSFORMATIONS
ION EXCHANGE MATERIALS
ISOTOPES
LIGHT NUCLEI
MAGNETIC RESONANCE
MATERIALS
MEASURING INSTRUMENTS
MICROSCOPY
MINERALS
MONOCRYSTALS
NANOSTRUCTURES
NITROGEN COMPOUNDS
NITROGEN HYDRIDES
NMR SPECTRA
NUCLEAR MAGNETIC RESONANCE
NUCLEI
ODD-EVEN NUCLEI
ORGANIC COMPOUNDS
POLYSACCHARIDES
REAGENTS
RESONANCE
SACCHARIDES
SCANNING ELECTRON MICROSCOPY
SCATTERING
SILICATE MINERALS
SORPTION
SPECTRA
SPECTROMETERS
SPECTROSCOPY
STABLE ISOTOPES
STARCH
SYNTHESIS
TRANSFORMATIONS
TRANSMISSION ELECTRON MICROSCOPY
ULTRAVIOLET SPECTRA
VISIBLE SPECTRA
X-RAY DIFFRACTION
ZEOLITES