Phosphor and nitrogen co-doped titania were prepared by hydrothermal method with phosphorous acid and ammonia as the P and N sources, respectively. The resulting materials were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS). Phosphor and nitrogen co-doped titania give a higher photocatalytic activity in the degradation of methylene blue (MB) under solar light irradiation. It was evidenced that the incorporation of P and N in the anatase titania lattice in the form of O–Ti–N, O–P–N, and Ti–O–P linkages. After photocatalytic properties studies, we can conclude that N, P codoped titania exhibit the further enhanced photocatalytic activity.