The reuse study of niobium phosphate catalyst (NbOPO4.nH2O, abbreviated as NbP) in furfural production from sugarcane bagasse (SCB) in an aqueous medium is the aim of this project. The heterogeneous NbP catalyst was exploited to hydrolize the SCB biopolymers and dehydrate the major released carbohydrate, i.e., xylose, into furfural. The compounds were separated and quantified by high-performance liquid chromatography (HPLC). At the end of each reaction, the catalyst was separated from the SBA by sieving and pre-treated with water (A), 5 ml of acetone (B), 10 ml of acetone (C) or calcined at 550 °C (D). After pretreatment, the catalyst was reused for another cycle. An analysis of variance was performed to compare the difference in productivity between cycles statistically. The catalyst was analyzed for its morphology by SEM images and XEDS. For the release of xylose, at a significance level of 0.01, the pretreatments A, B, and D in the reactions at 150 °C were efficient to reactivate the catalyst’s active sites. Cycles 1 and 2 produced about 15 g kg-1 xylose at 110 °C and 80 g kg-1 furfural at 150 °C. The results with pretreatment A at 150 °C are promising from an economic and environmental point of view since the other pretreatments either use a toxic, more costly solvent or consume electricity.