A method for preparing a fine particulate AlPO.sub.4 which comprises reacting an aqueous phosphoric acid solution with an aluminum compound selected from the group consisting of an aluminum hydroxide and an aluminum oxide, wherein the molar ratio of phosphoric acid to the aluminum compound is in the range of 0.8 to 1.8 in terms of P.sub.2 O.sub.5 /Al.sub.2 O.sub.3, said reaction being performed under stirring at an elevated temperature in an organic solvent capable of forming two phases with water, said solvent having a boiling point not lower than 60.degree. C. under atmospheric pressure, and being present in at least two times the weight ratio, based on the amount of Al.sub.2 O.sub.3, of the aluminum compound.