A new treatment technology of municipal solid waste incineration (MSWI) fly ash is presented in this paper. Feasibility of solidification/stabilization treatment of MSWI by successively adding trimercapto-s-triazine and cement, and the effect of addition, fly ash size and curing time were studied by batch tests. The results showed that MSWI posed a huge environmental risk, the partial distribution showed normal distribution approximately. Treatment of fly ash with trimercapto-s-triazine and cement showed a good effect, the leaching toxicity of treated fly ash solidified blocks with 2% trimercapto-s-triazine and 20% cement could meet the standard for pollution control on the landfill site of MSW in China after curing for 7 days, and the flexural strength of solidified blocks could reach 2.4 MPa. Ground fly ash had a positive effect on both leaching toxicity and strength.