Nanoscale lignin was successfully prepared with a supercritical antisolvent (SAS) apparatus using acetone as a solvent and superciritical carbon dioxide as an antisolvent. Four factors were studied and optimized by a four-level orthogonal array design (OAD). According to analysis of variance, precipitation pressure had a significant effect on mean particle size. The optimal conditions are as follows: precipitation temperature 35 °C, precipitation pressure 30 MPa, temperature difference +10 °C and concentration of lignin solution 0.5 mg/mL. The micronized lignin under the optimal conditions was characterized by Scanning Electron Microscopy (SEM), Fourier-transform Infrared Spectroscopy (FTIR), Dynamic Light Scattering (DLS) and X-Ray Diffraction (XRD) analyses. The results showed the mean particle size of micronized lignin was 0.144 ± 0.03 μm and had no degradation. The solubility of micronized lignin was improved significantly in distilled water.