AbstractIn the present work, the V2O5/S‐doped graphitic carbon nitride nanocomposite was constructed using the in‐situ growth method. The properties of this interesting material were improved by S‐doping as well as addition of V2O5. The nanocomposite was characterized using FT‐IR, XRD, SEM, EDX, BET, TEM, PL, XPS and UV‐DRS techniques. In continuation, the constructed nanocomposite was applied for adsorption and degradation of methylene blue and phenol as organic pollutants. The effect of certain factors such as pH, doses of adsorbent and adsorbate (methylene blue and phenol), time, and temperature was evaluated through performing of adsorption under different conditions. Then, degradation of the pollutants was performed under various conditions such as sunlight, light‐emitting diode, and ultraviolet irradiations and also in dark. The results showed a significant increase in the adsorption and photocatalytic activities of V2O5/S‐doped graphitic carbon nitride in comparison with pristine graphitic carbon nitride. The performance of V2O5/S‐doped graphitic carbon nitride remained after treatment for five times.