New stable polarization-sensitive materials are developed on the hydrophobic components basis which doesn't require an additional moisture protection. Bisazodye ortho-tolidinebisazophenol chromophoric component was synthesized which is liposoluble analogue of water-soluble azodye Mordant Pure Yellow M. This bisazodye were used to develop the hydrophobic materials films which can be applied as a protective layer themselves. To increase the thermal stability we have synthesized material by introducing bisazodye into the main-chain of macromolecule of thermally stable polymer. The different types of polarization-holographic gratings with high diffraction efficiency of 30-50% were recorded on the obtained materials by laser beams (441 - 488 nm).© (2011) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE). Downloading of the abstract is permitted for personal use only.