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Title: Synthesis of mesoporous zeolite single crystals with cheap porogens

Abstract

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: >more » 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.« less

Authors:
; ;  [1];  [1];  [1]
  1. Key Laboratory for Advanced Materials, Research Institute of Industrial Catalysis, East China University of Science and Technology, Shanghai 200237 (China)
Publication Date:
OSTI Identifier:
21580167
Resource Type:
Journal Article
Journal Name:
Journal of Solid State Chemistry
Additional Journal Information:
Journal Volume: 184; Journal Issue: 7; Other Information: DOI: 10.1016/j.jssc.2011.05.023; PII: S0022-4596(11)00272-6; Copyright (c) 2011 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Journal ID: ISSN 0022-4596
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; ALUMINIUM 27; AMMONIA; CELLULOSE; DESORPTION; FOURIER TRANSFORM SPECTROMETERS; FOURIER TRANSFORMATION; INFRARED SPECTRA; MONOCRYSTALS; NANOSTRUCTURES; NMR SPECTRA; NUCLEAR MAGNETIC RESONANCE; SCANNING ELECTRON MICROSCOPY; SPECTROSCOPY; STARCH; SYNTHESIS; TRANSMISSION ELECTRON MICROSCOPY; ULTRAVIOLET SPECTRA; VISIBLE SPECTRA; X-RAY DIFFRACTION; ZEOLITES; ALUMINIUM ISOTOPES; CARBOHYDRATES; COHERENT SCATTERING; CRYSTALS; DIFFRACTION; ELECTRON MICROSCOPY; HYDRIDES; HYDROGEN COMPOUNDS; INORGANIC ION EXCHANGERS; INTEGRAL TRANSFORMATIONS; ION EXCHANGE MATERIALS; ISOTOPES; LIGHT NUCLEI; MAGNETIC RESONANCE; MATERIALS; MEASURING INSTRUMENTS; MICROSCOPY; MINERALS; NITROGEN COMPOUNDS; NITROGEN HYDRIDES; NUCLEI; ODD-EVEN NUCLEI; ORGANIC COMPOUNDS; POLYSACCHARIDES; REAGENTS; RESONANCE; SACCHARIDES; SCATTERING; SILICATE MINERALS; SORPTION; SPECTRA; SPECTROMETERS; STABLE ISOTOPES; TRANSFORMATIONS

Citation Formats

Tao Haixiang, Li Changlin, Ren Jiawen, Wang Yanqin, E-mail: wangyanqin@ecust.edu.cn, and Lu Guanzhong, E-mail: gzhlu@ecust.edu.cn. Synthesis of mesoporous zeolite single crystals with cheap porogens. United States: N. p., 2011. Web.
Tao Haixiang, Li Changlin, Ren Jiawen, Wang Yanqin, E-mail: wangyanqin@ecust.edu.cn, & Lu Guanzhong, E-mail: gzhlu@ecust.edu.cn. Synthesis of mesoporous zeolite single crystals with cheap porogens. United States.
Tao Haixiang, Li Changlin, Ren Jiawen, Wang Yanqin, E-mail: wangyanqin@ecust.edu.cn, and Lu Guanzhong, E-mail: gzhlu@ecust.edu.cn. Fri . "Synthesis of mesoporous zeolite single crystals with cheap porogens". United States.
@article{osti_21580167,
title = {Synthesis of mesoporous zeolite single crystals with cheap porogens},
author = {Tao Haixiang and Li Changlin and Ren Jiawen and Wang Yanqin, E-mail: wangyanqin@ecust.edu.cn and Lu Guanzhong, E-mail: gzhlu@ecust.edu.cn},
abstractNote = {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.},
doi = {},
journal = {Journal of Solid State Chemistry},
issn = {0022-4596},
number = 7,
volume = 184,
place = {United States},
year = {2011},
month = {7}
}