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Elsevier, Microporous and Mesoporous Materials, 1-3(128), p. 136-143, 2010

DOI: 10.1016/j.micromeso.2009.08.014

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Controlled growth of thin and uniform TS-1 membranes by MW-assisted heating

Journal article published in 2010 by Julius Motuzas ORCID, Raminta Mikutaviciute, Emilie Gerardin, Anne Julbe
This paper is available in a repository.
This paper is available in a repository.

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Abstract

Thin and uniform Ti-containing silicalite-1 (TS-1) membranes were prepared for the first time by a microwave-assisted secondary growth method. The influence of synthesis temperature (150-200 °C), duration (90-150 min) and Ti concentration in the mother sol (molar ratio Si/Ti = 16-100) on the membrane formation were studied. The quantity of Ti species inserted in the silicalite-1 network was found to vary with these parameters, as well as the membrane quality and performance. TS-1 membranes with a Si/Ti molar ratio in the range 25-40 were successfully prepared from mother sols with compositions in the range Si/Ti = 16-100. An original parabolic evolution of membrane thickness vs. Si/Ti in the mother sol was evidenced, with a minimum thickness for Si/Ti around 50. In all cases Ti species were inserted within the zeolite network as far as no TiO2 clusters were detected after the thermal treatment at 550 °C. The membranes were typically 0.1-2 μm thick top-layers and crystal preferential orientation varied from oblique- to c-crystal preferential orientation (CPO) when the temperature was increased from 160 °C to 200 °C. The permeances of He, N2, O2, CO2 were high and lied in the range 1.9-7.48 × 10-6 mol m-2 s-1 Pa-1 when measured between 25 °C and 200 °C. The most selective membrane, prepared at 190 °C during 120 min with a molar ratio Si/Ti = 75 in the mother sol, had an ideal selectivity of 40 for n/i-C4H10 at 150 °C and 105 for CO2/SF6 at 25 °C.