Three different novel sorbents were prepared by cross-linking polypropylene grafted styrene-divinylbenzene (PP-ST-DVB) fibre with monochloromethylether or p-xylylenedichloride or 1,4-bis-chloromethyldiphenyl according to Friedel- Crafts reaction. A series of synthesis tests were made and the effects of several important factors including reaction temperature, time, catalyst, and material ratio on the Friedel-Crafts reaction were investigated in detail. The optimal synthetic conditions of sorbents were obtained. Compared with PP-ST-DVB fibre, the sorbents have larger specific surface area, pore volume, pore radius and higher adsorption capacities for organic vapours. The adsorption capacities for organic vapours on the hypercrosslinked sorbents were increased about 10 times. The adsorption capacities on the sorbents were related with the molecular length of cross-linking agents. The amounts absorbed on the sorbent 1, sorbent 2 and sorbent 3 can be reached to 428.6 mg/g for methanol, 471.9 mg/g for benzene, and 491.1 mg/g for toluene, respectively.