The copolymerization process of oil-soluble monomer (styrene) and water-soluble functional monomers (methacrylic acid and acrylic acid) has been studied. The polymerization process is tracked by use of TEM transparent Electronic Microscope and IR spectrometry. It is found that the difference of hydrophilicity between methacrylic acid and acrylic acid leads to their different copolymerization procedure with styrene