On the fluoride-mediated synthesis and amine intercalation of large lamellar crystals of layered titanosilicate Na/K-JDF
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On the fluoride‑mediated synthesis and amine intercalation of large lamellar crystals of layered titanosilicate Na/K‑JDF‑L1 Li Zhang1,2 · Yingjie Jin1 · Ping Li1 · Feixue Liang1 · Ruijiang Feng1
© Springer Science+Business Media, LLC, part of Springer Nature 2020
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. Keywords Microporous titanosilicate · Lamellar phase · Oriented growth · Intercalation materials · Interlayer space
1 Introduction JDF-L1 (Na4Ti2Si8O22·4H2O) [1], as a typical layered zeotype with defined ultra-micropore (0.3 nm) system [2], is still the most notable one of only a few of naturally occurring and synthetic microporous titanosilicates to date [3–5]. Classical JDF-L1 contains five-coordinated Ti (IV) ions in the form of T iO5 square pyramids where each of the vertices of the base is linked to SiO4 tetrahedra to form continuous sheets with interlamellar Na+ ions residing in the interlayer space [6]. It is certain that such a characteristic structure Electronic supplementary material The online version of this article (doi:https://doi.org/10.1007/s10934-020-00915-y) contains supplementary material, which is available to authorized users. * Yingjie Jin [email protected] 1
Faculty of Chemistry and Chemical‑Environmental Engineering, Liaoning Shihua University, Fushun 113001, Liaoning, People’s Republic of China
Institute of Unconventional Hydrocarbon and New Energy Sources, University of Petroleum (East China), Qingdao 266580, People’s Republic of China
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individuates JDF-L1 from the others, so that it has been expected to have particular applications in heterogeneous catalysis [7], radioactive cation adsorption [8, 9], highcapacity lithium ion battery anodes [10], and also fabrication of mixed matrix membranes for small gas molecular sieving [11–13]. More recently, considerable effort has been expended in establishing reliable and reproducible synthetic routes to the layered JDF-L1 and the i
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