Two types of novel hypercross-linked fiber adsorbents, ZH-01 and ZH-02, were prepared by cross-linking PP-ST-DVB fibers in solution with p-xylylenedichloride and monochloromethylether according to the Friedel-Crafts reaction. A series of static adsorption tests were performed. The results showed that the adsorbents have excellent adsorption capacities for 2-methylpyridine and the adsorption equilibrium data can be fitted well by the Freundlich model. The thermodynamic studies supported the conclusion that the mechanism of adsorption for 2-methyl-pyridine on the adsorbents is physical adsorption and a lower temperature is favorable to the exothermic physisorption process. In addition, kinetic studies were also carried out. The hypercross-linked fiber adsorbents showed a faster adsorption rate than the base PP-ST-DVB fiber. The faster attainment of adsorption equilibrium for 2-methylpyridine on the adsorbents (within 2 h), is advantageous for practical use. A first-order reaction rate equation was assumed for the adsorption system and was suitable to describe the process. The equilibrium rate constants of the adsorbents correlated well with their adsorption capacities.