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C3+ hydrocarbons fraction is a valuable raw material for the petrochemical industry. Membrane gas separation is an attractive technique for the separation of C3+¬ hydrocarbons from natural gas1. However, the existing membrane materials cannot provide the required combination of membrane properties. Highly permeable glassy polymers such as PTMSP, PIM-1, despite the good separation properties, do not exhibit stability of the membrane performance with time. Whereas traditional gas separation membranes based on poly(dimethylsiloxane) (PDMS) exhibit good stability, but show lower selectivity in comparison with glassy polymers. In this research new membrane polymers were synthesized based on poly(methylhydrosiloxane) modified hydrocarbons substituents in the side chain for gas separation applications, including gas separation of n-C4H10/CH4. Technique was developed for the preparation of membranes based on poly(octylmethylsiloxane), poly(decylmethylsiloxane) and poly(hexylmethylsiloxane). Results will be presented on the synthesis and characterization of the obtained membrane materials and their gas permeation properties.