The objective of this study was to prepare carbonaceous catalysts. Taking cellulose as the starting material, functionalization with sulphuric acid was done using 1:10 w / v ratio under one pot hydrothermal treatment at 80 °C. The catalyst was extensively characterized with BET, XPS, TGA, SEM, FT-IR, XRD etc. The synthesized C-SO 3 H catalyst had a surface area of 447 m 2 g −1 , pore radius of 30.020 Å and pore volume of 0.157 cc g −1 . The total acidity of the catalyst was 4.56 mmol g −1 and sulphonic acid density was 1.31 mmol g −1 . It was used in acetalization of glycerol under microwave irradiation. Under the optimized reaction conditions of 1:5 M ratio of glycerol and acetone, catalyst loading of 7 wt% at 70 °C in 10 min, the glycerol to solketal conversion was found to be 97.1%. The product was characterized with FT-IR, NMR, GC–MS that confirmed the successful synthesis of solketal. The catalyst showed excellent reusability giving 82.1% conversion at the 5th reaction cycle.