<p>Nancomposite of Al<sub>2</sub>O<sub>3</sub>/activated carbon was prepared from the mixture of alumina oxide (Al<sub>2</sub>O<sub>3</sub>) and activated carbon from palm oil shell under the mixture of aquabidest and ethanol (1:1). The mixture was treated by hydrothermal process at 250 <sup>o</sup>C for 3 h. Resulted Al<sub>2</sub>O<sub>3</sub>/ activated carbon was characterized using SEM/EDX for studying the morphology structure of activated carbon and composite showing a like flower structure attached on the surface. The chemical compositions were 73.18%, oxygen 23.72%, aluminium 2.30%, dan silica 2.00%. The efficiency of composite was investigated for removal of phenol in aqueous solution. The maximum adsorption of phenol was obtained at pH 2, adsorbent weight 2 g, contact time 60 min and phenol concentration 100 ppm.</p>