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Issue 36, 2017
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A crystalline AlPO4-5 intermediate: designed synthesis, structure, and phase transformation

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Abstract

AlPO4-5 is the most extensively studied material in exploring the crystallization mechanism of aluminophosphate molecular sieves, and it can be synthesized using 4-dimethylaminopyridine (DMAP) as an organic structure-directing agent (OSDA). Achieving the AlPO4-5 intermediate in the crystalline form would be of great importance and significance for this purpose. In this study, we proposed a concept that by carefully regulating the synthesis conditions, crystalline alumimophosphate intermediates could be rationally prepared. A crystalline AlPO4-5 intermediate, (C7H11N2)2(H3O)(Al3P4O16)·(H2O)2.5 (1), was, therefore, synthesized by significantly increasing the amounts of orthophosphoric acid and DMAP. The intermediate 1 consists of alternating organic DMAP and inorganic [Al3P4O16]3− layers with abundant hydrogen bonds and can transform to the AlPO4-5 framework upon heating in air or through a steam-assisted conversion (SAC) method. To unravel the role of DMAP in the transformation, pure AlPO4-5 (2) was also synthesized by altering the synthesis conditions. The supramolecular assembly templating (SAT) effects of DMAP in 1 and 2 were verified via fluorescence spectra. Thus, the π–π stacking interactions between the DMAP molecules and the abundant hydrogen bonds between the adjacent layers are considered to be important for the phase transformation of 1. This crystalline intermediate would promote the understanding of the crystallization mechanism in the system of aluminophosphate molecular sieves.

Graphical abstract: A crystalline AlPO4-5 intermediate: designed synthesis, structure, and phase transformation

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Supplementary files

Article information


Submitted
29 Jul 2017
Accepted
20 Aug 2017
First published
21 Aug 2017

Dalton Trans., 2017,46, 12209-12216
Article type
Paper

A crystalline AlPO4-5 intermediate: designed synthesis, structure, and phase transformation

C. Lin, J. Li, F. Pan, Y. Zhao, L. Xu, Y. Yang, X. Du, X. Lin, F. Liao, J. Lin, T. Yang and J. Sun, Dalton Trans., 2017, 46, 12209 DOI: 10.1039/C7DT02772A

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