Journal of Applied Polymer Science, Vol.66, No.7, 1325-1341, 1997
Synthesis of Uniform Microspheres with Higher Content of 2-Hydroxyethyl Methacrylate by Employing Spg (Shirasu Porous-Glass) Emulsification Technique Followed by Swelling Process of Droplets
Relatively uniform microspheres containing a hydrophilic monomer, 2-hydroxyethyl methacrylate (HEMA), were prepared by employing a swelling method of uniform seed droplets. A uniform seed emulsion composed mainly of styrene (St) was prepared by the Shirasu porous glass (SPG) membrane emulsification technique; this was mixed with a secondary emulsion composed mainly of HEMA/St or HEMA/MMA (methyl methacrylate) prepared by a homogenizer for swelling. The swollen droplets obtained were polymerized at 75 degrees C under a nitrogen atmosphere. The uniform microsphere with a higher content of HEMA was obtained successfully by the swelling method while it failed by a direct emulsification method. The effects of the composition of the oil phase and the inhibitor in the continuous phase on the incorporated fraction of HEMA, the morphology of particles, and monomer conversion were investigated. It was found that the incorporated fraction of HEMA increased with increasing its feed fraction, and more HEMA was incorporated into the microsphere when HEMA/MMA was used as the oil phase of the secondary emulsion rather than HEMA/St. Although the final conversion was very low when the feed fraction of HEMA was higher, it can be increased to more than 80% by using an adequate amount of ethylene glycol dimethacrylate (EGDMA) as a crosslinker and NaNO2 as an inhibitor in the aqueous phase. Various microspheres with different morphologies such as spherical, snowmanlike, and popcornlike were observed, depending on composition of the oil phase. Furthermore, the porous microsphere with a high content of HEMA was obtained by employing hexanol (HA) as a porogen.