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Issue 7, 2015
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Intercalation of triethylphosphine oxide bearing a phosphoryl group into Dion–Jacobson-type ion-exchangeable layered perovskites

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Abstract

Triethylphosphine oxide [(C2H5)3P[double bond, length as m-dash]O; TEPO] was intercalated into protonated Dion–Jacobson-type ion-exchangeable layered perovskites, HLaNb2O7·xH2O (HLaNb) and HCa2Nb3O10·xH2O (HCaNb), by hydrolysis of their n-decoxy derivatives (C10O-HLaNb or C10O-HCaNb) in the presence of TEPO. The interlayer distances of the products (TEPO/C10O-HLaNb and TEPO/C10O-HCaNb) were smaller than those of the corresponding n-decoxy derivatives, but still larger than those of anhydrous protonated forms of HLaNb and HCaNb. The solid-state 31P NMR signals of the products observed at 94 ppm (TEPO/C10O-HLaNb) and 93 ppm (TEPO/C10O-HCaNb) exhibited large downfield shifts from that of the physisorbed TEPO. IR spectroscopy also showed decreases in the ν(P[double bond, length as m-dash]O) band wavenumbers upon the reactions. These results clearly indicate that TEPO is intercalated and interacted with Brønsted acid sites, the surface hydroxyl groups generated via hydrolysis of n-decoxy groups. The difference in ν(P[double bond, length as m-dash]O) band wavenumbers as well as that in gallery heights suggests that TEPO exhibited different orientations with respect to the inorganic layers. The chemical shifts of solid-state 31P NMR signals suggested high Brønsted acidity of HLaNb and HCaNb.

Graphical abstract: Intercalation of triethylphosphine oxide bearing a phosphoryl group into Dion–Jacobson-type ion-exchangeable layered perovskites

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Publication details

The article was received on 23 Jul 2014, accepted on 23 Sep 2014 and first published on 16 Oct 2014


Article type: Paper
DOI: 10.1039/C4DT02230K
Citation: Dalton Trans., 2015,44, 3002-3008
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    Intercalation of triethylphosphine oxide bearing a phosphoryl group into Dion–Jacobson-type ion-exchangeable layered perovskites

    N. Toihara, Y. Yoneyama, A. Shimada, S. Tahara and Y. Sugahara, Dalton Trans., 2015, 44, 3002
    DOI: 10.1039/C4DT02230K

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