The synthesis of mesoporous materials, such as the M41S type, initiated intense research into the synthesis and properties of novel mesoporous materials. This research has led to the discovery that compositions other than silicates or aluminosilicates, particularly oxides and phosphates, can be organized into three-dimensional porous or layered compounds. In this paper we report on the synthesis of a mesoporous and a layered aluminophosphate. The starting solutions were prepared by dissolution of a hydrated aluminophosphate in HF, followed by treatment with solutions of cetyltrimethylammonium bromide in tetramethylammonium hydroxide. The products were characterized by X-ray powder difrfraction, thermal analysis, NMR and surface area measurements. Because of the presence of significant quantities of HF the synthetic pathway was most likely S +F −I +.
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