A greener process involving sol-gel method was adopted to prepare structurally controlled non-crystalline silica particles from rice husk collected from the local regions of Tamil Nadu. The experimental conditions were optimized and silica particles were characterized by BET with surface area of 320 ± 10 m²/gm and from the SEM measurements, the micro particles mean size range from 120 ± 10 nm respectively. The average pore size of the mesoporous powder obtained was measured to be 8 ± 2 nm. The mesoporous silica was surface modified hydrophobically utilizing phenyl triethoxysilane (PTEOS) and ultra-sonication. Using FTIR and SEM measurements the surface modifications were characterized. These silica sub micro particles with hydrophobic templates were used as sorbents for adsorption of PCB. Using the direct treatment of PCB sorbed chemically modified silica sub micro particles with fenton reagent, the degradation studies on PCB was performed. The degradation percentages dependence with sorbent feed loadings were measured by the analysis of the degraded products. The sub micro silica particles with surface chemical modifications have proved to be efficient solid matrix for the removal of PCB, in the aqueous phase at ambient conditions