Corn hulls were abundant and inexpensive byproducts of the corn dry or wet milling processes, but most of them were discarded as agro-wastes. The aim of this study was to extract the dietary fiber by hot-compressed water (HCW) from defatted corn hull and to determine the chemical properties. Results showed that temperature and time played critical roles in extraction efficiency; the maximal yield of dietary fiber A (DFA) extracted by HCW reached 33.0% at 150°C for 60 min. The yield of dietary fiber B (DFB) increased from 2.0% to 56.9% as the temperature increased from 110 to 180°C, while the yield of solid residue (SR) decreased from 88.7% to 27.7%. Fourier transform infrared spectroscopy (FT-IR) results demonstrated that C-H, O-H, C=O, COO- occurred in the DFA, SR and DFB. The dietary fiber polysaccharides consisted of arabinose, galactose, glucose, xylose and uronic acid.