Carbonization of PAN grafted uniform crosslinked polystyrene microspheres

Micrometer-sized polystyrene/poly(styrene-divinylbenzene) and polystyrene/polydivinylbenzene composite particles of narrow size distribution were formed by a single-step swelling process of uniform polystyrene template particles with emulsion droplets of dibutyl phthalate containing benzoyl peroxide and divinylbenzene in the presence or absence of styrene, followed by polymerization of the monomer(s) within the swollen template particles at 70 °C. Porous poly(styrene-divinylbenzene) and polydivinylbenzene uniform microspheres were formed by dissolution of the polystyrene part of the former composite particles. Hydroperoxide conjugated microspheres were formed by ozonolysis of the former porous microspheres. Uniform poly(styrene-divinylbenzene)/PAN and polydivinylbenzene/PAN core/shell microspheres were prepared by room temperature redox graft polymerization of AN onto the hydroperoxide conjugated particles. Uniform carbon microspheres were prepared by carbonization of the core/shell particles at 800 and 1100 °C under dynamic N₂ atmosphere. On the other hand, a similar treatment of the core particles only resulted in destruction of the particle shape. Carbon microspheres of increasing surface area (up to ca. 1000 m²/g) were prepared by activation of the former carbon microspheres with CO₂ at 850 °C. The influence of the carbonization temperature of the core/shell particles and the activation time of the carbon particles on the carbon yield and surface area has been elucidated.