Three kinds of activated coke powders (ACPs) were prepared from different coal by a one-step rapid pyrolysis activation method. Detailed pore structure and surface characteristics of the ACPs were characterized by BET specific surface area test, scanning electron microscope (SEM), and Fourier transform infrared spectrometer (FTIR). Adsorption capacity of ethyl acetate, benzene, and p-xylene onto the ACPs was tested. Results demonstrated that the ACPs had well-developed pore structures, with considerable specific surface area and pore volume. Volatile contents in the feed coal had promotion effect on the fast formation and development of the pore structure. Shengli lignite (SLC) showed the largest specific surface area and pore volume, which reached 351.07 m 2 /g and 0.1698 m 3 /g, separately. Surfaces of ACPs were rich of functional groups as carboxyl, lactone, phenolic hydroxyl (or ether), and carbonyl, the types of which kept relatively constant regardless of the change of the feed coal. ACPs presented good VOCs adsorption performance. With the most micropore structures, SLC sample presented the best adsorption capacity for ethyl acetate, benzene, and p-xylene, which is 222.23, 149.87, and 217.63 mg/g, respectively. All ACPs presented preferential VOC adsorption order of ethyl acetate > pxylene > benzene, which suggested that ACPs presented favorable adsorption ability to VOC species of polar and large molecules. K E Y W O R D S activated coke powders, adsorption capacity, breakthrough curve, pore structure characteristics, VOCs adsorption 1 | INTRODUCTION Nowadays, with the growing trend of industrialization, air pollution has become one of the main challenges of humans, which can unprecedentedly threaten their health and environment. Volatile organic compounds (VOCs) such as formaldehyde, benzene, toluene, and xylene are recognized as the major contributors to regional air pollution, and most of them are precursors of PM 2.5 and photochemical smog. 1 Due to the hypertoxicity