Porous microwave irradiated activated carbon has been developed and its application for time efficient ultrasonic treatment of Congo‐red (CR) dye. The maximum removal efficiency of 97.73% was obtained using developed adsorbent with ultrasound treatment. The optimum parameters for maximum dye removal were obtained that is, contact time of 2 hr, adsorbent dose of 0.2 g, neutral pH, room temperature, and initial CR‐effluent concentration of 10 mg/l. Adsorption isotherms models, kinetics of the process, and thermodynamic analysis have been evaluated to investigate the adsorption performance. The pseudo second order rate kinetics (R2 = 0.99) and Langmuir equilibrium isotherm (R2 = 0.99) were well fitted to the experimental data. It has been found that microwave synthesized method was better technique in terms of energy savings, and ultrasonic treatment approach was efficient technique in terms of operational time. The combination of microwave‐ultrasonic reported to have an adsorptive capacity of 75.75 mg/g with least energy‐cost consuming approach.
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