In this work, nickel promoted sulfated zirconia (Ni/SZ) as catalyst was prepared by either by reflux (Ni/SZ-R) or hydrothermal Ni impregnation (Ni/SZ-H) routes. The aim of this study was to evaluate the influences of two preparative methods on the physico-chemical properties of prepared catalysts. Both the catalysts were characterized by XRD, FTIR, ammonia adsorption, SEM-EDX, TEM-SAED, AAS and BET. It was found that the presence of sulfate and nickel could enhance the Brønsted and Lewis active acid sites. In relation to the effect of Ni impregnation method, acidity, amount of sulfate and Ni found in Ni/SZ-R were higher than those in Ni/SZ-H. Unfortunately, higher impregnated sulfate and nickel on zirconia support led to a decrease in surface area and pore volume and an increase
in crystallite size of grainy aggregated mesoporous nickel promoted sulfated zirconia (Ni/SZ).