Hydroxyalkylation/alkylation of biomass-derived 2-methylfuran with cyclic ketones (cyclopentanone and cyclohexanone) has great potential in synthesizing high-density biofuel. But the conversion and selectivity are still unsatisfactory because the in-situ formed water decreases the acidity of catalyst and induces side reaction. Herein, hydrophobic mesoporous resins with sulfonic acid group (PS) and fluoride sulfonic acid group (PCS) were synthesized by a simple solvothermal reaction and ion exchange treatment, which have good mesoporous structure with surface area of 300-700 m(2)/g. Notably, PS and PCS have better hydrophobicity and oleophilicity as compared to widely used sulfonic acid functional amberlyst-15 and fluoride sulfonic acid functional nafion-212. In the hydroxyalkylation/alkylation reaction, PS shows higher activity and selectivity than amberlyst-15 while PCS surpasses nafion-212. Furthermore, both PS and PCS have good recycling stability in consecutive 5 runs. After hydrodeoxygenation, two high-density biofuels with density of 0.819 and 0.825 g/mL were obtained. (c) 2016 American Institute of Chemical Engineers AIChE J, 63: 680-688, 2017