The decomposition of hydrogen iodide in the thermochemical water splitting iodine–sulfur process at an intermediate temperature (400 °C) using a catalytic membrane reactor was reported here, for the first time. The performance of a catalytic membrane reactor based on a hexyltrimethoxysilane-derived silica membranes (H2 permeance of 9.4 × 10−7 mol Pa−1 m−2 s−1 and H2/N2 selectivity of over 80.0.) was evaluated at 400 °C by varying the HI flow rates of 2.6, 4.7, 6.9, 8.4, and 9.7 mL min−1. The silica membranes were prepared by counter-diffusion chemical vapor deposition method on γ-alumina-coated α-alumina tubes. Hydrogen was successfully extracted from the membrane reactor using the silica membrane at 400 °C. A significant increase in HI conversion was achieved. The conversion achieved at an HI flow rate of 2.6 mL min−1 was approximately 0.60, which was greater than the equilibrium conversion in HI decomposition (0.22).
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