A novel hypercross-linked fiber which has an excellent adsorption capacity for cyclohexane vapor was prepared by cross-linking PP-ST-DVB fibers with p-xylylenedichloride according to the Friedel-Crafts reaction. The effects of several important factors on the Friedel-Crafts reaction, including reaction temperature, reaction time, catalyst type, and material ratio were investigated in detail and the optimal synthesis conditions of hypercross-linked fiber were obtained. The adsorption equilibrium for cyclohexane vapor on hypercross-linked fiber was measured by a static volumetric technique. The equilibrium measurements were performed at 298, 323 and 348 K and pressures of up to 6.04 kPa. The results can be well fitted by the Freundlich model. The isosteric heat curve was derived from the equilibrium data, and indicates that the hypercross-linked fiber has an energetically heterogeneous surface.