Composite of Al2O3/activated carbon (Al2O3/AC) has been successfully synthesized by hydrothermal method. It was synthesized from activated carbon from oil palm shell waste by mixing with Al2O3 powder in ethanol. The mixer was placed in a hydrothermal reactor and heated up to 250°C for 3 hours. Comparison study of surface area between activated carbon and composite of Al2O3/AC indicate that surface area decreased from 67.6 to 65.3 m2/g. However, XRD analysis shows that there was a slight different hkl phase. Characterization using FTIR showed that the composite have more oxygen functional groups compared with activated carbon. SEM-EDX of composite of Al2O3/AC showed an increasing of crystalline structure on the surface.