A dialysis-based method was developed to remove Na ions in fullerol preparation by a conventional synthetic route. Fullerol was synthesized using a typical two-phase reaction in the presence of tetrabutylammonium hydroxide. Its structure was confirmed by UV spectra, Fourier transform infrared spectroscopy spectra, H-1 nuclear magnetic resonance, and matrix-assisted laser desorption/ionization time of flight mass spectra. The content of Na element was determined by inductive coupled plasma atomic emission spectroscopy. The mass content of Na in the product obtained from the conventional route was about 10%, and it could be almost completely eliminated by dialysis with a membrane of molecular weight cut-off (MWCO) 8-15 kDa. The yield of fullerol by the dialysis method was slightly higher than by the conventional route. These results indicate that dialysis may have a potential application for fullerol preparation.