The waste coal fly ash was utilized to synthesize zeolite by alkaline fusion method through orthogonal test. The copper oxide was loaded on the zeolite by dipping method. The optimal ratio of coal fly ash to sodium hydroxide, ratio of liquid to solid, calcining temperature and crystallization time were determined to be 1.2, 9, 700°C and 10 h, respectively. The CuO dipped zeolite was applied to treat the acid red GR wastewater and the obtained color and COD removal rates were 83.80% and 99.88%, respectively. The XRD pattern showed that the NaA type zeolite phase was formed in the experiment.