A highly absorptive resin was prepared by glow-discharge electrolysis plasma initiated suspension copolymerization, in which methyl methacrylate and butyl acrylate were used as monomers, N,N'-methylenebis(acrylamide) as crosslinking agent, polyvinyl alcohol as dispersant, and Na(2)SO(4) solution as supporting electrolyte. To optimize the synthesis conditions, the discharge voltage, discharge time, polymerization temperature, the ratio of monomers, the amounts of crosslinking agent and supporting electrolyte, as well as the ratio of water to oil, were examined in detail. The structure and properties of the obtained resin were characterized by means of attenuated total reflectance Fourier transform infrared spectroscopy (ATR FT-IR), thermogravimetric analysis (TG), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM), respectively. The oil absorbency, absorption rate, absorption selectivity, and network parameters of the resin were also examined. Results showed that under the optimal conditions, the oil absorbency was about 28.5 g/g for benzene, 25.4 g/g for toluene, 28.0 g/g for xylene, 38.1 g/g for chloroform, and 37.0 g/g for carbon tetrachloride.