Porous zirconium phosphate was prepared by silylation with organic silanes. Octylamine was intercalated into alpha-Zr(HPO4)(2)center dot H2O for expanding interlayer spacing and 1,2-bis(dimethylchlorosilyl)ethane (BMCE) was used for silylation of inorganic layers in toluene. The number of octhylamine molecules intercalated was similar to the number of phosphorus in the inorganic layers. On the other hand, that of BMCE molecule after silylating treatment was much smaller than that of phosphorus. The interlayer spacing of silylated compound was confirmed to expand via high-temperature XRD patterns and was preserved on thermal treatment up to around 500 degrees C. The maximum specific surface area of the silylated compound heated at 300 degrees C was around 70 m(2)/g, though that was smaller for silylated compounds heated at higher and lower temperature. (c) 2007 Elsevier Ltd. All rights reserved.