In this article, a two-step activated carbon preparation technique from corncob has been elucidated. The derived catalysts AAC-CC has been characterized using various techniques for the determination of their structural properties and compared with AC-CC, already reported with another article. The conjugated boat structure of AAC-CC resulted in a very high surface area (779.8 m2/g) and high pore volume (0.428 cc/g). This unveils the suitability of AAC-CC as better among the two catalytic pathways for solketal production. The activated carbons so prepared have been used for the valorization of glycerol to produce 2,2-Dimethyl-1,3-dioxolane-4-methanol (solketal), oxygenated additives to fuel. The face-centered composite design (FCCD) of RSM was applied for the optimization of the reaction parameters for the ketalisation reaction using AAC-CC as a catalyst. From the optimized results, the acidic catalyst AAC-CC resulted in a glycerol conversion, i.e. 80.3% under the actual laboratory experiment. Moreover, the catalyst could be reused for three consecutive batch reactions without (< 5%) much reduction of activity and no distinctive structural deformity.