Mesostructured organo-aluminophosphates were prepared by using surfactants with long alkyl chain lengths (C-16 and C-22) and by utilizing solubilization of triisopropylbenzene; calcination of the mesostructured materials yielded thermally stable mesoporous aluminophosphates with surface areas > 700 m(2) g(-1) and with pore diameters in the range 1.8-3.9 nm.