Adsorption of toluene by activated carbon fiber (ACF) coated with dielectric heating element and desorption by applying microwave were investigated. In order to prepare adsorbent so that VOC can be desorbed by microwave heating, fine dielectric heating element with nano size was coated on the surface of the ACF using hybrid binder. Eight adsorbents (ACF-DHE, Activated Carbon Fiber coated with Dielectric Heating Element) were prepared with different amount of dielectric heating element, kinds of hybrid binder, and solvent. In order to investigate adsorption characteristics, BET surface area, pore volume, and average pore size were measured for each adsorbent including ACF. Breakthrough experiments with toluene concentration, flow rate, bed length using fixed bed reactor were performed to investigate adsorbality of adsorbent, and results were compared with that of the ACF. Desorption reactor was constructed with modified microwave oven to investigate heating effect on ACF-DHE by applying microwave power. Each adsorbent saturated with toluene were put into desorption reactor. Composition of desorbed gas generated by applying controlled microwave power to reactor was measured. Up to now, hot air desorption method has been used. Experimental results showed that desorption method with new adsorbent prepared by coating dielectric heating element on ACF can be used for industrial application.