The removal of cetylpyridinium chloride (CPC) (as a cationic surfactant) on nanoporous nickel phosphate (nano-NiPOx) particles is studied for the first time. The structure and morphology of the material are investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDAX), transmission electron microscopy (TEM) and BET surface area determination. Various operating parameters, such as the initial CPC concentration, amount of NiPOx, shaking speed, pH and temperature, are investigated. The point of zero charge (PZC) for NiPOx in 0.1 M KCl solution is found to be 6.5. The adsorption of the CPC on the NiPOx follows pseudo-first-order kinetics. Furthermore, the experimental data follow the modified Frumkin adsorption isotherm. Important thermodynamic parameters, such as the free energy of adsorption at different temperatures, are extracted by fitting the experimental data with the isotherm model. The parameters obtained above suggest that there is a strong extent of adsorption of the CPC on the NiPOx surface.