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In situ assembly of ZSM-5 nanocrystals into micro-sized single-crystal-like aggregates via acid-catalyzed hydrolysis of tetraethylorthosilicate

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Abstract

ZSM-5 aggregates were synthesized with the silica source tetraethylorthosilicate (TEOS) being hydrolyzed at acidic conditions to produce siliceous precursors, followed by the addition of aluminum sulfate and tetrapropyl ammonium bromide (TPABr), and with the resulting gel mixture being hydrothermally crystallized at basic conditions. The obtained products were characterized by XRD, SEM, and N2 adsorption. Well crystallized ZSM-5 can be successfully synthesized through the sulfuric acid-catalyzed hydrolysis of TEOS within a short crystallization time 35 h. The thus produced micro-sized single-crystal-like zeolite ZSM-5 aggregates (10 μm) are made of uniformly distributed nanocrystals with sizes of about 200 nm. Moreover, by adjusting the hydrothermal reaction parameters, such as increasing the crystallization temperature, the TPABr/SiO2 ratio and the pH value of reaction solution, the crystallization is accelerated substantially. Also, the moderate H2O/SiO2 molar ratio of 20–60 in the synthesis mixture can lead to pure ZSM-5, and yet the optimal ratio is 40.

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Acknowledgements

This study is supported by the Key Natural Science Foundation for Universities of Jiangsu Province (06KJA53012), National Natural Science Foundation of China (No. 20776069) and Program for Changjiang Scholars and Innovative Research Team in University (PCSIRT 0732).

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Authors and Affiliations

  1. State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing University of Technology, No 5 Xinmofan Road, Nanjing, 210009, China

    Jing Gu, Yajing Wu, Jun Wang, Youdong Lu & Xiaoqian Ren

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  1. Jing Gu
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  2. Yajing Wu
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  3. Jun Wang
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  4. Youdong Lu
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  5. Xiaoqian Ren
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Correspondence to Jun Wang.

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Gu, J., Wu, Y., Wang, J. et al. In situ assembly of ZSM-5 nanocrystals into micro-sized single-crystal-like aggregates via acid-catalyzed hydrolysis of tetraethylorthosilicate. J Mater Sci 44, 3777–3783 (2009). https://doi.org/10.1007/s10853-009-3508-6

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