Porous cuprous oxide (Cu2O) nanospheres composed of small nanoparticles with diameters at 10~20 nm were successfully synthesized without surfactant at room temperature within 5 min. The products were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), N2adsorption-desorption, and Fourier transform infrared (FT-IR) spectrum. The adsorption ability of the as-prepared products towards methyl orange (MO) as the pollutant was investigated and FT-IR spectrum was employed to identify the adsorbed species. In addition, the reusability of the as-prepared products was studied as well.