: Using bagasse as raw material, the xylose-rich pre-hydrolyzed sugar solution was obtained by pre-hydrolysis under high temperature and low acid concentration (0.176% H2SO4), and then furfural was obtained by further deep acidolysis, and the separation of furfural was realized by the highly efficient extraction from the aqueous phase with a mixture of organic solvents. The pre-hydrolysis of bagasse, the deep acid hydrolysis and the organic solvent extraction of furfural were investigated; morphology and structure of bagasse and pre-hydrolysis residue were characterized by FT-IR, XRD, SEM and TGA; and quantitatively detection of the xylose in the pre-hydrolysis process and the furfural in the deep acid hydrolysis process was conducted by an UV spectrophotometer. The results showed that the highest xylose concentration (41.72 g/L) was obtained in the pre-hydrolyzed solution at 160 °C, liquid-solid ratio of 6:1, and mass percentage of concentrated sulfuric acid to bagasse (oven dry) as 0.176%. The pre-hydrolyzed solution was directly deep acidified at 170 °C for 90 min, the concentration of furfural in the solution could reach up to 15.91 g/L, with the highest molar yield of furfural as 59.60%. Extraction of furfural from aqueous solution was carried out by mixing organic solvents in the ratio of v(1,2-dichloroethane):v(n-butanol) = 9:1, and the extraction rate of furfural was up to 93.53% when the volume ratio of the extracting phase was v(organic phase):v(aqueous phase) = 2:1.