Chromium based metal organic framework (MIL-101)/activated carbon composite materials were synthesized using hydrothermal method and the catalytic effect was investigated for the acetylation of glycerol with acetic acid. Activated carbon and chromium based metal organic framework hybrid material was fabricated with two different weight ratio of chromium ion to activated carbon, materials were labelled as AC@MIL-10110, AC@MIL-1015. The characterization of synthesized catalysts was performed using XRD, N2 adsorption, TGA, FTIR, SEM/EDS, XPS, n-butylamine titration, contact angle measurement and TEM in order to explore the relation between the structure and catalytic performance. The effect of addition of the activated carbon on the catalytic activity of materials was determined by considering conversion of glycerol and selectivity of glycerol monoacetate, glycerol 1,3 diacetate and glycerol triacetate. Taguchi orthogonal L9 matrix has been applied to understand the effect of temperature, molar ratio and catalyst loading on the conversion of glycerol and selectivity of acetates. Signal to noise ratio (S/N) and analysis of variance (ANOVA) results revealed that the temperature was the dominant factor affecting the conversion and selectivity. 100% of glycerol was converted to acetates and 5.2% of glycerol triacetate selectivity was achieved at 110 ?C, acetic acid/glycerol molar ratio of 9 and catalyst loading of 4 g/L.