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Synthesis and catalytic ammoxidation performance of hierarchical TS-1 prepared by steam-assisted dry gel conversion method: the effect of TPAOH amount

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Abstract

The hierarchical titanium silicalite-1 (TS-1) was synthesized by the steam-assisted dry gel conversion method in one step and characterized by XRD, SEM, N2 adsorption/desorption, UV–Vis, FT-IR, and Raman spectroscopies. And its catalytic activity was tested for ammoxidation of methyl ethyl ketone with hydrogen peroxide as oxidant. The results show that the amount of tetrapropylammonium hydroxide (TPAOH) as template has a major influence on the physicochemical and catalytic properties of the hierarchical TS-1 prepared. When lower amount of TPAOH (TPAOH/SiO2 = 0.08 mol) was used, hierarchical TS-1 can be successfully synthesized. With an increase in TPAOH amount in synthesis solution, the crystal size of TS-1 is decreased and mesoporous surface area is increased; if the excess template was used in the synthesis of TS-1, more extra-framework Ti would be formed in the TS-1 samples prepared. The hierarchical TS-1 exhibits higher catalytic activity than TS-1 prepared hydrothermally for ammoxidation of methyl ethyl ketone. Using hierarchical TS-1 synthesized under TPAOH/SiO2 = 0.18 as the catalyst, which has more tetrahedrally coordinated Ti species in the TS-1 framework, 94.2 % conversion of reactant and 100 % selectivity to methyl ethyl ketone oxime can be obtained after 2 h of reaction at 70 °C.

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Acknowledgements

We would like to acknowledge the financial support of the National Basic Research Program of China (2010CB732300).

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Authors and Affiliations

  1. Key Laboratory for Advanced Materials and Research Institute of Industrial Catalysis, East China University of Science and Technology, Shanghai, 200237, People’s Republic of China

    Mengjia Wu, Xiaohui Liu, Yanqin Wang, Yanglong Guo, Yun Guo & Guanzhong Lu

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  1. Mengjia Wu
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  2. Xiaohui Liu
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Correspondence to Xiaohui Liu or Guanzhong Lu.

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Wu, M., Liu, X., Wang, Y. et al. Synthesis and catalytic ammoxidation performance of hierarchical TS-1 prepared by steam-assisted dry gel conversion method: the effect of TPAOH amount. J Mater Sci 49, 4341–4348 (2014). https://doi.org/10.1007/s10853-014-8130-6

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