Methyl methacrylate/nitrile butadiene rubber/graphene oxide (MMA/NBR/GO) composite materials were prepared by ball-milling based on the mechanochemical principle. The effects of some key process parameters, such as graphene oxide (GO) content, ball-to-powder ratio (BPR), and ball-milling time on textures and structures of MMA/NBR/GO composite materials were studied systematically by Zeta potentials, Raman spectroscopy, Thermogravimetric analysis, Fourier transform infrared spectrometry, and the derivation mechanism was examined. The results indicated composite materials with excellent dispersion stability at GO content of 0.3%, BPR of 3.87, and ball-milling time of 5 h, the value of sedimentation rate is only 1.0%, the Zeta potential is À41.5 mV, and the mass loss ratio is 40.36%. FT-IR result shows that the intensity of the characteristic peak all decreases after ball milling, and carboxyl group of GO and hydroxyl group connected to the benzene ring is broken. The graft position is CN and CH 2 of NBR, and CH 3 of MMA. Under these conditions, the oxygen-containing functional groups of GO were successfully grafted onto the MMA and NBR.