Interpenetrating polymer network (IPN) based on poly (Methylhydrosiloxane) and poly (Acrylonitrile) have been synthesized using benzyl peroxide as initiator and divinyl benzene as crosslinker in toluene under an inert atmosphere of nitrogen. The scanning electron microscopy reveals dual phase morphology of the synthesized polymer network. The properties like percentage swelling, average molecular weight between crosslink?s (Mc), are the direct function of [copolymer] and initiator [benzoylperoxide] whereas inverse function of concentration of monomer (acrylonitrile) and crosslinker (divinyl benzene). A fluorescence spectrum of the material is observed in the visual range near 457 nm. FTIR spectrum confirmed the presence of PMHS and acrylonitrile and DVB in the synthesized IPN. The differential scanning calorimeter (DSC) curve showed glass transition temperature at 340oC. Thermogravimetric analysis (TGA) depicted thermal stability of IPN upto 400oC. The synthesized IPN is thermally stable upto 400oC.