Abstract In this article, we report the green, simple and large-scale ultrasonic synthesis of nanocomposites of graphene oxide with three-dimensional two-fold interpenetration azine-functionalized MOF, TMU-16/GOn (n = the percentage of GO), at room temperature and atmospheric pressure. The materials were characterized by FT-IR, SEM, PXRD, Raman spectroscopy and nitrogen adsorption. The presence of GO significantly changes the morphologies of the composites and decreases their surface area. It is expected that TMU-16/GOn nanocomposites may find wide forthcoming industrial and technological applications in electrochemistry, gas adsorption and catalysts.