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Hydrothermal synthesis of an ITH-type germanosilicate zeolite in a non-concentrated gel system

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Abstract

A germanosilicate zeolite with the ITH framework type (designated JLG-18) has been hydrothermally synthesized. Compared with other ITH-type materials synthesized in concentrated systems, JLG-18 was the first one synthesized in a non-concentrated system. In addition, the organic structure-directing agent (OSDA) for the synthesis of JLG-18 was N,N,N′,N′-tetramethyl-1,6-hexanediamine (TMHDA), which was less expensive than those used for the synthesis of other ITH-type materials. The optimal molar ratio of the initial gel was 0.5 SiO2: 0.5 GeO2: 7 TMHDA: 1.4 HF: 42 H2O. The effects of various synthetic parameters on the formation of final products, such as source materials, GeO2:SiO2 ratio, H2O:(SiO2 + GeO2) ratio, TMHDA:(SiO2 + GeO2) ratio, crystallization temperature, and reaction time, were investigated. The as-synthesized samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), inductively coupled plasma (ICP), elemental analysis, thermogravimetric analysis (TG), and N2 adsorption. JLG-18 with a Si:Ge ratio of 2:1 exhibited excellent thermal stability, even after calcination at 700 °C in air. The microporous surface area of JLG-18 was 317.07 m2/g.

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Acknowledgments

The authors thank the National Natural Science Foundation of China and the State Basic Research Projects of China (2011CB808703) for financial supports.

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Authors and Affiliations

  1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun, 130012, People’s Republic of China

    Xiaoyan Ren, Jiancong Liu, Yi Li, Jihong Yu & Ruren Xu

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  1. Xiaoyan Ren
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  2. Jiancong Liu
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  3. Yi Li
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  4. Jihong Yu
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Correspondence to Yi Li.

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Ren, X., Liu, J., Li, Y. et al. Hydrothermal synthesis of an ITH-type germanosilicate zeolite in a non-concentrated gel system. J Porous Mater 20, 975–981 (2013). https://doi.org/10.1007/s10934-013-9676-4

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