NiCr2O4 normal spinel nanostructures were prepared via hydrothermal treatment at 180oC for 12 h in the presence of cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulphate (SDS) and poly vinylpyrrolidone-25000 (PVP-25000) as capping agents and subsequent calcination process at 500°C for 3 h.In this method, [Ni (en)2 (H2O) 2] (NO3) 2 and [Cr (en) 3] Cl3.3H2O used as precursors and not utilized any alkaline or precipitating agent.Detailed characterization of the as-prepared nanostructures were carried out by Fourier transform infrared (FTIR), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), UVVis diffuse reflectance spectroscopy (DRS). XRD revealed the formation of pure nickel chromite spinel phase and SEM showed the formation of uniform sphere-like nanoparticles. Furthermore, the photocatalytic degradation of acid black 1 as diazo dye used in textile and dyeing water pollutants was Investigated.