Amphiphilic microspheres, ranging in size from 3 to 35 mum, were prepared by suspension copolymerization of styrene with poly(ethylene oxide) vinylbenzyl (PEO-VB) macromonomer by changing polymerization conditions. It was found that an increase in the amount of dispersant and the PEO-VB concentration resulted in decreases of the size and size distribution of amphiphilic microspheres. The morphology, size, and size distribution of amphiphilic microspheres were characterized by scanning electron microscopy. The structure of copolymer was confirmed by infrared spectroscopy, differential scanning calorimetry, elemental analysis, and X-ray photoelectron spectroscopy. The content of the hydroxyl groups localized in the microspheres ranged from 0.05 to 0.2 mmol/g.