The suspension polymerization with two organic phases was adopted to prepare spherical hypercrosslinked resin by self-polycondensation of 4,4 '-bis-(chloromethyl)-1,1 '-biphenyl (CMB). The chemical structure, morphology and pore characteristics of the novel spherical resin were characterized with Fourier transform infrared spectroscopy (FM), micrograph and Brunauer-Emmett-Teller (BET). It is found that the suspension system and stirring speed impose a great influence upon the regularity and size distribution of hypercrosslinked beads. To prepare CMB resin beads with diameter of about 300 mu m, the optimal condition is as follows: stirring speed 300 r.min(-1), and the volume ratio of the two organic phases (nitrobenzene/dimethyl silicon oil) 1 : 5. After the self-polycondensation and succedent post-crosslinking of CMB monomer, the spherical adsorbent presents high special surface area (1190 m(2). g(-1)) and abundant pore volume (0.714 cm(3). g(-1)), and could be potentially applied in the adsorption of various organic molecules and synthesis of porous ion exchanger.