Abstract
The crystallization behavior of the initial mixture with the composition of Al2O3:4.0P2O5:3.0 diethylene-triamine(DETA):xHF:153H2O was investigated at 180 °C, where 0⩽x⩽3. If x⩽1.8, three-dimensional open-framework aluminophosphate AlPO-CJ31 was obtained. If 2⩽x⩽3, a chain-like aluminophosphate(1) was obtained. The crystallization process of both compounds was investigated by means of powder X-ray diffraction(XRD) and the concentrations of Al and P in the liquid product during the crystallization process were analysed by means of inductively coupled plasma atomic emission spectroscopy(ICP-AES). The evolution of the coordination state of Al, P and F during the crystallization was monitored with 27Al, 31P and 19F MAS NMR technique. The influence of the fluoride ions and the source of fluoride ions on the structure-directing effect of DETA was discussed. It was found that the fluoride ions changed the crystallization direction of the initial mixture, i.e., the structure-directing effect of DETA, via altering the distribution or micro-structure of the inorganic fragments.
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Supported by the National Natural Science Foundation of China(Nos.21571075, 21320102001, 21621001), the National Key Research and Development Program of China(No.2016YFB0701100) and the Programme of Introducing Talents of Discipline to Universities(the 111 Project), China(No.B17020).
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Tian, Y., Xu, J., Wang, Z. et al. Influence of fluoride ions on the structure-directing effect of organic amine in the synthesis of aluminophosphate open-frameworks. Chem. Res. Chin. Univ. 33, 853–859 (2017). https://doi.org/10.1007/s40242-017-7131-9
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DOI: https://doi.org/10.1007/s40242-017-7131-9