Abstract: A new type of high-efficiency and environmentally-friendly NCC was prepared by the catalytic hydrolysis of fiber raw material with p-toluenesulfonic acid. The effects of reaction time, reaction temperature and ultrasonication on the yield and properties of NCC were investigated. Fourier transform infrared spectroscopy(FT-IR), X-ray diffraction(XRD), transmission electron microscopy(TEM) and thermal gravimetric analysis(TGA) were used to characterize the spectral properties, crystal structure, morphology and thermal stability.The results showed that the NCC yield was the highest(51.66%) at the condition of reaction time of 45 min, reaction temperature of 80℃ and ultrasonic wave time 2 h. The TEM results indicated that the diameters of NCC were 10 to 40 nm and the lengths were 400 to 700 nm. XRD analysis showed that the crystallinity of NCC was 72.50%, which was higher than that of fiber raw material, and both of them maintained cellulose Ι structure.TGA displayed that the thermal properties of NCC were more stable than raw fiber.