We have studied the effect of synthesis conditions on formation of thermally stable mesoporous zirconium phosphate. We have used X-ray diffraction, temperature-programmed desorption of ammonia, IR spectroscopy, NMR, and DTA to establish that formation of hexagonally ordered materials which are stable during detemplating is possible only when using cationic and nonionic surfactants, a temperature of 20 °C, and post-synthesis treatment with a solution of orthophosphoric acid. We have established that, depending on the ordering, there is a change in both the adsorption characteristics of the zirconium phosphate as well as the concentration of acid sites and their strength distribution.