A porous coordination polymer, [Zn2(oba)2(4-bpdh)] 3DMF (TMU-5) upon silk yarn, has been synthe-sized under ultrasound irradiation. We here present a tex-tile for the adsorptive removal methyl orange from wastewater using three-dimensional porous Zn(II)-based metal–organic framework (TMU-5) and silk fibers. The effect of sequential dipping steps in growth of TMU-5 upon fiber has been studied. These systems depicted a decrease in the size accompanying a decrease in the sequential dipping steps. The samples were characterized with powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy spectra and scanning electron microscopy. XRD analyses indicated that the prepared TMU-5 on silk fibers were crystalline.