Abstract: In view of the treatment/disposal problem of coal fly ash,which is a solid waste with large output,wet milling method to synthesize zeolite was used to explore the high value utilization of fly ash as resource. Through the design of four factors,three levels orthogonal synthesis experiments,combined with the evaluation of cation exchange capacity,the best condition of synthesis of zeolite from fly ash under wet milling method was determined. In order to test the adsorption and removal effect of cation heavy metals of the zeolite synthesized by this method,the adsorption and removal of heavy metal Pb( Ⅱ) under nine orthogonal conditions were carried out,and the adsorption and removal of anionic groups with less attention under the orthogonal conditions were also studied. According to the average value and range of cation exchange capacity of different factors under different orthogonal conditions,the optimal combination to synthesize zeolite is Na OH concentration of 4 mol/L,liquid-solid ratio of 4 m L/g,grinding time of 24 h and rotating speed of 350 r/min. The range of cation exchange capacity demonstrates that the most important factor for zeolite synthesis is grinding time,followed by liquid-solid ratio and alkali concentration,and the speed of planetary ball mill has the least influence. The results of adsorption and removal of Pb( Ⅱ) by zeolite synthesized under the experimental conditions show that the adsorption of Pb( Ⅱ) is mainly physical adsorption,and the removal rate is more than 70%,up to 92.5%,which mainly depends on the cation exchange capacity of synthetic zeolite. The results of adsorption and removal of heavy metal Cr on the zeolite synthesized under the experimental conditions show that the adsorption and removal of heavy metal Cr is both physical and chemical adsorption. The adsorption and removal rate of Cr( Ⅵ) on the synthesized zeolites is up to 35.7%. The zeolite synthesized by wet milling method has certain adsorption and removal effect on heavy metal cations and anions.