Abstract: A highly selective tubular silicon based pyrolysis membrane has been prepared and its preparation method has also been given in the paper. The membrane was made by pyrolyzing a silicon resin material with regular molecular arrangement The permeability of the membrane for H₂ is about 10⁴ Barrer and the selectivity for H₂/N₂ 16.8. The membrane shows much better Permselectivity comparing with polymeric membranes, ordinary inorganic membranes and the pyrolysis membrane prepared from silicon resin with random molecular arrangement Furthermore, the preparation process of the membrane is simple, inexpensive and highly reproducible.