In this research, Na[M(edta)(H 2 O) n ](M = Dy, Ho,Yb and Er),(n = 1-3) complexes were synthesized using lanthanide salts and Na 4 (edta). Then, the complexes were refluxed in the presence of a mixture of Al(OH) 3 and H 3 BO 3 for 24 h. The reaction mixture was then calcined at 400°C for 5 hours. The obtained powder as a new phosphorescent pigment was dispersed in water and acrylicpolyurethane resin to prepare a new phosphorescent paint. The precursors and pigments were characterized by elemental Analysis, XRD, XRF, FT-IR, UV-Vis and fluorescence spectroscopy. In addition, the prepared phosphorescent paint was characterized by solid state phosphorimetry