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In situ formation of the micro- and mesoporous structures of SBA-15 materials was investigated. It was found that the structure is significantly different from that for cylindrical or hexagonal pores, which suggests that the SBA-15 is more complex than an array of hexagonally ordered channels. Nitrogen adsorption isotherms at 77 K provided evidence that large (primary) mesopores are accompanied by a certain amount of significantly smaller pores with a broad distribution in the micropore/small-mesopore range within the mesoporous walls of main channels. It was found that the microporosity can be controlled by the time of heating as well as the synthesis temperature. The diffusion properties of n-heptane as a probe molecule in four selected SBA-15 samples with different micropore volumes were studied by the standard zero length column technique and related to their structural characteristics. The results have shown that the diffusion process involving n-heptane at a low concentration level takes place inside the walls of main mesoporous channels and depends on the relative content of micropores. In the samples that have a relatively high content of micropores, n-heptane diffusivities are relatively low, their activation energies are high, and the process is similar to diffusion in typical microporous adsorbents, like zeolites. As the micropore content is decreased, diffusion becomes more and more controlled by secondary mesopores of the intrawall pore structure, rendering diffusion faster and activation energies lower.

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In our recent studies (Vinh-Thang, H.; Huang, Q.; Eic, M.; Trong-On, D.; Kaliaguine, S. Langmuir 2005, 21, 2051-2057; Vinh-Thang, H.; Huang, Q.; Eic, M.; Trong-On, D.; Kaliaguine, S. Stud. Surf. Sci. Catal. 2005, in press), a series of synthesized SBA-15 materials were characterized using nitrogen adsorption/desorption isotherms at 77 K and SEM images. In the present paper, four of them (MMS-1-RT, MMS-1-60, MMS-1-80, and MMS-5-80) were further investigated with regard to their equilibrium characteristics using n-heptane and toluene as sorbates by the standard gravimetric technique. SBA-15 materials proved to have a broad pore size distribution within the micropore/small-mesopore range in the walls of their main mesoporous channels. The adsorption capacities for toluene were found to be higher than for n-heptane. The isosteric heats of adsorption, estimated by the Clausius-Clapeyron equation, are also higher for toluene compared to n-heptane. They were found to depend on framework microporosity of the relevant SBA-15 samples. The isosteric heats of adsorption for all sorbates decrease with increased loading and approach the heats of evaporation of the respective sorbate. The adsorption capacities of SBA-15 samples are significantly higher than those of silicalite, i.e., the MFI zeolite silica analogue. In contrast to that, the isosteric heats of adsorption in the mesopore channels of SBA-15 were found to be much smaller. This result also suggests that SBA-15 can potentially be a good candidate for separation of C(7) hydrocarbons.

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We present the first 13C magnetic resonance imaging study of CO2 transient adsorption/desorption processes in a zeolite 5A column. CO2 transient concentration profiles were measured with a centric scan spin-echo single point imaging technique. The adsorption wave profiles were determined under flow conditions, with the results analyzed by the Bohart-Adams model. The model adequately accounts for the spatial and the temporal behavior of CO2 in the column. CO2 adsorption rate constants were calculated from the fit. Desorption profiles were acquired by blowing a helium stream through a zeolite 5A column saturated with CO2. An asymmetry between the adsorption and desorption profiles is readily apparent. A linear relationship between the CO2 condensed phase concentration and square root of time was observed.