Ce-Y-palygorskite catalysts were prepared by chemical blending method. The effect of preparation conditions on catalytic performance of Ce-Y-palygorskite catalyst for NO decomposition was investigated in a fixed bed flow reactor. The characteristics of the Ce-Y-palygorskite catalysts were studied by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The obtained results provided substantial evidence that the catalysts preparation conditions would have strong effect on the catalytic activity for NO decomposition. The Ce-Y-palygorskite catalyst prepared under the optimal conditions: rare earth content, Ce/Y, pH value of the chemical blending and calcination treatment temperature was 3%, CexY(1-x)(x=0.9), 7 and 350°C, respectively, was identified as the most active catalyst for the NO decomposition, and the denitration rate could be up to 67.3% under the experimental reaction conditions.