A series of mixed zinc-aluminum phosphate (ZnAlP) catalysts containing 40-90 aluminum molar % were synthesized by a coprecipitation method and characterized by nitrogen adsorption-desorption, X-ray diffraction, FTIR spectroscopy, thermogravimetric analysis (TGA), differential thermal analysis (DTA), diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and temperature programmed desorption (TPD) of ammonia. The presence of aluminum greatly affected the surface properties of Zn-3(PO4)(2) by delaying the crystallization process of Zn-3(PO4)(2). All amorphous samples were shown to be mesoporous and they contained two types of aluminum surface hydroxyl groups and one type of phosphorus hydroxyl group, as shown by DRIFT spectra. The specific surface area and the acidity of ZnAlP increased on increasing the aluminum content. On the other hand, a great difference in the texture and the concentration of surface acid sites was found by changing the precipitating agent and calcination temperature. Thus these factors also play an important role in the final properties of these catalysts.