Sustainable material research has benefited greatly by inventing two-dimensional (2D) materials, graphene oxide (GO), and Ti3C2 MXenes using carbon sources from industrial waste. This method provides a cost-effective way to obtain high-value nanomaterials and solves the environmental issues related to waste disposal. Carbon-rich industrial wastes are converted into GO during the synthesis process by oxidation-reduction pathways, with effective purification and exfoliation achieved through the Improved Hummer’s method. Simultaneously, MXenes are produced through the selective etching of transition metal carbides, with industrial waste serving as a precursor for the carbide phase. The resulting GO and Ti3C2 MXenes sheets display distinctive physicochemical properties and have distinctive Raman spectra. The structural characteristics of prepared graphene oxide and MXene nanosheets using industrial waste carbon are confirmed by XRD (X-ray diffraction method) and scanning electron Microscopy (SEM).