Coal fly ash (CFA), a solid waste from power plants, was selected as the support of Ni-based catalysts used for steam reforming of toluene in a fixedbed reactor. The CFA support was thermally pretreatment first, followed by chemical activation with different treatment time (6 h to 4 days) in 2-mol/L HNO 3 solution. Then, series low-cost catalysts were prepared by wet impregnation. The prepared catalysts were characterized suitably by X-ray diffraction (XRD), Brunauere-Emmette-Teller (BET), temperature programmed reduction (TPR), temperature programmed desorption (TPD), and Raman techniques. According to the catalyst characterization, the chemical pretreatment could improve the support property by adjusting the chemical composition. The Fe-rich Fe-Ni and Ni-Co alloy was formed by H 2 reduction on the Ni/CFA-6h and Co-Ni/CFA-6h catalysts, respectively. In the catalytic steam reforming of toluene, the Ni/CFA-6h had the best catalytic active among all monometallic catalysts, which could be attributed to the existence of Fe 0.94 Ni 0.06 particles, and its performance could be further improved after partly replacing Ni by Co. The Co-Ni/CFA-6h catalyst exhibited the best ability of carbon deposit resistance, implying that its catalytic performance slightly lower than Ni/SiO 2 was due to the too large S BET surface area gap. K E Y W O R D S carbon deposit, catalyst, coal fly ash, steam reforming, toluene 1 | INTRODUCTION Recently, the depletion of fossil fuel is increasingly becoming a global concern. So along with the shortage of fossil fuels, biomass has drawn considerable attention owing to its high availability, low emission, and renewability. 1,2 Of all biomass thermochemical conversion technologies, gasification, in particular, enables the transformation of biomass into syngas, which include hydrogen and carbon monoxide. 3 Syngas can be converted into many kinds of chemical substances through the Fischer-Tropsch method and can be used for power generation. 4-6 However, the formation of tar in the syngas is the primary challenge and urgently facing the gasification process. 7 Biomass tars mainly are largely aromatic hydrocarbons, such as benzene, toluene, and naphthalene, and they constitute condensable fractions of the organic gasification product. 8 The presence of tar in syngas contributes to end-use problems such as blockages and corrosion in downstream filters, fuel line, engine nozzles, and turbines. 9 Therefore, the removal of biomass tar is an urgent problem to be solved at present.