Abstract
The preparation and performance of membranes for application to hydrogen separation from coal-derived gas is described. The membrane material investigated was dense amorphous silica deposited on a suitable support by chemical vapor deposition (CVD). Two types of support materials were pursued. One type consisted of a two-layer composite, zeolite silicalite/{alpha}-Al{sub 2}O{sub 3}, in the form of tubes approximately 0.7 cm in diameter. The other type was porous glass tubes of diameter below 0.2 cm. The first type of support was prepared starting from {alpha}-Al{sub 2}O{sub 3} tubes of 1{micro}m mean pore diameter and growing by hydrothermal reaction a zeolite silicalite layer inside the pores of the alumina at the OD side. After calcination to remove the organic template used in the hydrothermal reaction, CVD was carried out to deposit the final silica layer. CVD was carried out by alternating exposure of the surface with silicon tetrachloride and water vapor. SEM and N2 adsorption measurements were employed to characterize the membranes at several stages during their preparation. Permeation measurements of several gases yielded H{sub 2}:N{sub 2} ideal selectivity of 150-200 at room temperature declining to 110 at 250 C. The second type of support pursued was porous glass tubes prepared by a novel extrusion technique. A thick suspension of borosilicate glass powder in a polyethersulfone solution was extruded through a spinneret and after gelation the glass-polymer tube was heat treated to obtain a gas-tight glass tube. Leaching of the glass tube in hot water yielded connected pores with diameter on the order of 100 nm. CVD of the final silica layer was not carried out on these tubes on account of their large pore size.
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