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 (FTIR)

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 μm

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.