Different catalytic materials of mixed oxide of zinc and vanadium Zn3V2O8 were synthesized using co-precipitation, combustion, alginate gelation and mechanosynthesis methods. The synthesized mixed oxide Zn3V2O8 were characterized by several techniques including XRD, SEM, EDX, XPS and BET. Structural measurement revealed the influence of the synthesis method on the physical and catalytic proprieties of Zn3V2O8 materials. Catalytic performance of Zn3V2O8 has been studied by oxidation of xylose to organic acids in water at 150 degrees C for 1 h. Significantly, this is the first time that the Zn3V2O8 nano-oxide was used as catalyst for xylose oxidation in water. Zn3V2O8 can efficiently catalyze the synthesis of glycolic acid (70% selectivity and 60% yield) from xylose with excellent stability and reusability. The ability to regenerate the Zn3V2O8 was also assessed by determining the change in the reaction indices in successive reaction-regeneration cycles.