The toxic Cr(VI) contaminating water released from the metallurgical, dyeing, and electroplating industries is getting worse day by day and is extremely hazardous to human health. Thus, the development of a cost-effective, quick, and efficient adsorbent is highly essential for the Cr(VI) decontamination from wastewater. Herein, a microwave-assisted carbon-based composite called Mg-Fe LDH@OPAC was prepared by assembling Mg-Fe LDH onto orange peel-activated carbon (OAPC). Prior to investigating deeply into the adsorption behavior of the composite, the Mg-Fe LDH@OPAC formation was confirmed by using instrumental techniques like FESEM, EDS, Zeta potential, XRD, FTIR, Raman, XPS, and BET analyzer. The material had a high surface area of 143.9 m