Photocatalytic degradation of different organic dyes under simulated sun light irradiation found an increasing attention in the recent years. To development of high-efficient photocatalyst, in this work, we prepared NiFe 2 O 4 nanoparticles by the chitosan-assisted route and characterized by FT -IR, XRD, UV-Vis, SEM and TEM analysis. In addition, the photodegradation of methylene blue (MB) as a model wastewater has been studied and the effect of important parameters such as initial pH solution, catalyst dose, initial MB concentration and irradiation time was investigated. The highest degradation of 98.99 % was reported at optimal conditions, initial pH of 10, photocatalyst dose of 0.04 g, initial MB concentration of 50 mg/L and irradiation time of 150 min. The kinetics of the experimental data analysis using the Langmuir-Hinshelwood model, result predicted that the process obeyed from pseudo -first -order with a strong correlation value (R 2 ) of 0.9936, k = 0.03082 min -1 and t 1/2 = 22.49 min. Reusability of NiFe 2 O 4 nanoparticles revealed that the degradation efficiency was change from 98.99 % (initially) to 95.68 % (five cycles). The results predicted that the as-prepared NiFe 2 O 4 nanoparticles showing great photodegradation efficiency towards MB dye, ease of use, good stability and potential to be used as catalyst for photodegradation of other organic dyes.