Citation: YAO Xiao-Qiang, XU Xiang-Yu, LÜ Zhi, JIAO Kun, SONG Jia-Qing, LI Zhao-Fei, WANG Qian, YAN Li-Jun, HE Ming-Yuan. Synthesis of Plate Like Silicalite-1 with Controlled Thickness[J]. Acta Physico-Chimica Sinica, ;2013, 29(08): 1809-1813. doi: 10.3866/PKU.WHXB201305161 shu

Synthesis of Plate Like Silicalite-1 with Controlled Thickness

1.
1 State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, P. R. China;
2 Petrochemical Research Institute of Petrochina, Beijing 100195, P. R. China;
3 Shanghai Key Laboratory of Green Chemistry and Chemical Processes, East China Normal University, Shanghai 200062, P. R. China

Received Date: 11 April 2013
Available Online: 16 May 2013
Fund Project: 国家高技术研究发展计划(863) (2009AA064201) (863) (2009AA064201)国家科技支撑计划(2012BAE05B00)资助 (2012BAE05B00)

In this study, plate like Silicalite-1 samples with controlled thickness were synthesized using a SiO₂-TPAOH-H₂O-NH₄F (TPAOH: tetrapropylammonium hydroxide) system by careful tuning of the synthetic parameters. Samples were fully characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), and thermogravimetry-differential thermal analysis (TG-DTA). We confirmed that the concentration of NH₄F and pH of the initial gel played important roles in controlling sample morphology. The morphologies of the samples changed from ellipse to plate like shapes as the molar ratio of NH₄F to SiO₂ was increased from 0 to 0.18. In addition, the thickness of the plates was controlled by regulating the amount of NH₄F in the gel. The thickness of the sample decreased as the amount of NH₄F increased, and reached its minimum when the NH₄F/SiO₂ molar ratio reached 0.4. Further increase of the molar ratio of NH₄F/SiO₂ increased the thickness of the plates because of their improved crystallinity. In these plate like particles, the b axis was perpendicular to the plate, as confirmed by HRTEM, which implies that these materials could show od accessibility for guest molecules because the b axis is the straight channel in MFI structures. All of the plate like Silicalite-1 samples were highly stable and their morphologies were retained even after treatment at 1100℃.
- Silicalite-1,
- Morphology,
- Plate like material,
- NH₄F/SiO₂,
- HRTEM
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