To enhance adsorption and desorption efficiency of volatile organic compounds from gas streams, we synthesized a series of well-developed micro-mesoporous hypercrosslinked polymeric adsorbents (MM-1, MM-2, and MM-3). The adsorption and desorption performance of dichloromethane and 2-butanone on newly synthesized adsorbents was investigated and compared with commercial micropore-dominated hypercrosslinked polymeric adsorbent UT-001). The contributions of micropore and mesopore to adsorption and desorption of dichloromethane and 2-butanone on polymeric adsorbents were well elucidated. Consequently, the adsorbent MM-3 had been sorted out with high BET surface area (1606 m(2)/g), large micropore and mesopore volumes (0.562 mL/g and 1.046 mL/g, respectively). The MM-3 exhibited the similar adsorption capacities with JT-001 for dichloromethane and 2-butanone at regions of p/p(0) < 0.2, but had higher adsorption capacities than JT-001 at high relative pressures. The largest adsorption capacities of MM-3 for dichloromethane and 2-butanone at 308 K were 13453 mg/g and 853.5 mg/g, respectively, which are about 1.78 and 1.88 times those of JT-001 under the same condition. Furthermore, the MM-3 exhibited higher desorption efficiencies than JT-001, especially for 2-butanone with a higher boiling point. (C) 2014 Elsevier Inc. All rights reserved.