Biochar, a carbon-rich and porous material, has numerous applications, including soil amendment, carbon sequestration, and environmental remediation. This study explored the prospects of employing activated sludge, a byproduct of organic matter-rich wastewater treatment, as a raw material for the synthesis of biochar. Biochar production from activated sludge resolves waste management issues and the demand for sustainable bio-based products. In order to produce biochar, the pyrolysis of activated sludge was investigated with an emphasis on using Design Expert software to optimize the process parameters. The important parameters, such as temperature and residence time, significantly impact the yield of the produced biochar. This study determined the ideal pyrolysis parameters to optimize biochar yield using a methodical experimental design technique. The data from the pyrolysis experiments were evaluated using response surface methodology (RSM) in Design Expert. The experiments were carried out at different temperatures and residence times. The maximum biochar yield (3.46%) is obtained with a pyrolysis temperature of 300 °C and a residence time of 2 h, according to the optimized results. The results showed that optimizing pyrolysis conditions is critical for effective biochar production, offering a feasible route for waste sludge assessment and supporting environmentally friendly waste management techniques.