Abstract: Multiwalled carbon nanotubes (MWCNTs) were synthesized by catalytic chemical vapor deposition and functionalized by oxidation with potassium permanganate at room temperature using a phase transfer catalyst, methyl trioctyl ammonium chloride as a dispersion agent. The functionalized nanotubes were characterized by Fourier transform infrared spectroscopy and thermogravimetry. Sonication was used to assist their dispersion in dichloromethane and the resulting suspension was added dropwise to a stirred polyvinyl alcohol aqueous solution and spongy microspheres were formed. SEM showed that the microspheres consisted of loosely entangled MWCNTs that had diameters in the range 50-150μm. The microspheres may be useful for lightweight energy absorbing coatings, catalyst and electronics applications.