A new method was developed for preparing polystyrene-functionalized multiple-walled carbon nanotubes (MWNTs) through the termination of anionically synthesized living polystyryllithium with the acyl chloride functionalities on the MWNTs. The acyl chloride functionalities on the MWNTs were in turn obtained by the formation of carboxyls via chemical oxidation and their conversion into acyl chlorides. The polystyrene-functionalized MWNTs had good dispersion in common organic solvents, and this indicated good compatibility for the preparation of styrenic nanocomposite materials. The synthesis results and characterization data for the functionalized MWNTs collected via Fourier transform infrared, thermogravimetric analysis, solid-state NMR, and electron microscopy, are presented and discussed. (C) 2004 Wiley Periodicals, Inc.