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On the fluoride-mediated synthesis and amine intercalation of large lamellar crystals of layered titanosilicate Na/K-JDF-L1

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Abstract

Fluoride-mediated synthesis in the inorganic hydrothermal system has been proposed for preparing large crystals of layered Na/K-JDF-L1 with lamellar morphology. The protonated JDF-L1 crystals derived from their layered precursors are structurally modified by 1,6-hexanediamine intercalation under mild hydrothermal conditions. All the materials mentioned are characterized by XRD, FESEM, EDX/ICP-AES, and TGA–DSC. It is concluded that the combination of fluorides with low alkalinity (pH ca.10.0) and crystallization temperature (200 °C) facilitates the oriented growth of metastable layered phase Na/K-JDF-L1, yielding regular lamellar crystals with square-sheet structure in two-dimensions of ca. 15 × 15 μm. Data on Na/K-JDF-L1 structure are presented for identification of the most probable tetragonal space group, P4212, corresponding to the highest crystallographic symmetry. It is also revealed that amine intercalation of relevant H-JDF-L1 by the hydrothermal process leads to the formation of layered titanosilicate materials with an ordered redistribution of the dominant interlayer space (d001) shifting from 10.674 to 15.620 Å.

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Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 21171083).

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Correspondence to Yingjie Jin.

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Zhang, L., Jin, Y., Li, P. et al. On the fluoride-mediated synthesis and amine intercalation of large lamellar crystals of layered titanosilicate Na/K-JDF-L1. J Porous Mater 27, 1389–1397 (2020). https://doi.org/10.1007/s10934-020-00915-y

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