Photocatalytic degradation of nonylphenol(NP) using the Mirco/mesoporous Composite La/13X/MCM-41, which was synthesized by hydrothermal method as reported in this article, was carried out to test the catalytic activity of the composite material. The synthesized materials were characterized by powder X-ray diffraction patterns (XRD), transmission electron microscopy (TEM), N2sorption isotherms, fourier-transform infrared (FT-IR). The influencing factors of the NP photodegradation were also evaluated.The NP removal efficiency can reach above 93% when the optimum conditions are as follows catalyst dosage is 0.1g/L, reaction time is 120min, initial pH is 6and initial concentration is 1mg/L. The NP photodegradation process obeys first-order reaction. The Mirco/mesoporous Composite La/13X/MCM-41 exhibited higher catalytic activity.