Simultaneously ultrasonic wave and microwave assisted technique (SUMAT), as a method of process intensification, was first applied to the preparation of nanocellulose whiskers (NCWs) from filter paper by sulfuric acid hydrolysis. The effects of temperature, sulfuric acid concentration, and mass of raw material and time on the yield of NCWs were investigated by single-factor experiments, and the preparation conditions were optimized with response surface methodology. The obtained NCWs were characterized by transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction and thermal gravimetry. The results showed NCWs were facilely prepared by using SUMAT. However, some harsh reaction conditions such as high temperature, strong acidity and long time treatment easily induced the reduction of the yield of NCWs. Under the optimal conditions, the yield and the crystallinity of NCWs with the crystal form of cellulose Ice is 85.75% and 80%, respectively. (c) 2013 Elsevier Ltd. All rights reserved.