Abstract: Silica-supported titanic sulfate and zirconium sulfate solid acid catalyst (Ti(SO4)2-Zr(SO4)2/SiO2) was prepared by impregnation method. The supported catalyst was characterized by TG, acidimetric analysis, FT-IR and XRD. The effects of calcination and loading amount on the catalyst activity were investigated. The results indicate that the catalyst prepared has a esterification rate of 95.6% at the conditions of m(catalyst)2.0g/0.1mol oleic acid, ratio of methanol to oleic acid 4, reaction temperature 85℃ and reaction time 5h. It is found after the catalyst was continuously used for 5 times, the esterification rate drops to below 80% because of coking，proved by infrared analysis of deactivated catalyst, but the activity of the catalyst can successfully recovered after activation by roasting and/or supplementing certain amount of active components needed.