The mesostructured nickel phosphates, NiPO-1 and NiPO-2, were synthesized with cetyltrimethylammonium bromide (CTAB) as a template via sol-gel method. The template was removed by solvent extraction in order to make their mesopores accessible. The influence of extractant, temperature, concentration and repetitions on the mesostructure and the removal efficiency were studied and optimized by XRD, FT-IR, CHN element analysis and N₂ adsorption techniques. The removal of the template in NiPO-1 and NiPO-2 exceeded 97% by using 0.1 mol/L CH₃COONa/EtOH as an extractant under 78 ℃ for 1 h and repeated for 4 times. The integrity and the ordering of the mesostructure were maintained. In the XRD patterns of the extracted samples, the diffraction intensity of (100) increased significantly, while the d₁₀₀ space also increased owing to the swelling behavior of the nanotubes in the extractant under elevating temperature. The results of N₂ adsorption showed that the surface areas of the extracted NiPO-1 and NiPO-2 reached 309.5 m²•g^－1 and 263.9 m²•g^－1 respectively.

Key words: mesoporous material, nickel phosphate, template removal, extraction, CTAB