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- Author or Editor: Y. Grillet x
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Abstract
Then-alkanes of different lengths were preadsorbed to selectively block part of the micropores of a MFI-type zeolite, Silicalite-I. The porosity available to argon and nitrogen was then studied by quasi-equilibrium adsorption microcalorimetry and volumetry at 77K and compared to what was found for the bare zeolite. Indeed, although partial adsorption ofn-alkanes does not alter the value of the differential enthalpies of adsorption for both argon and nitrogen, then-butane preadsorption diminishes the adsorption capacity by inducing inaccessible volumes in the micropore network. Moreover, the microcalorimetric experiments clearly show thatn-butane is not evenly distributed in the zeolite channel network while the longern-alkanes used are.
Abstract
Thermodesorption is here considered for its possibility of giving access to the microporosity of adsorbents. The requirements of this application (good separation of successive desorption steps, good control of the desorption pressure and temperature throughout the sample, possibility of a safe kinetic analysis of each step) are here fulfilled by carrying out the thermodesorption in the Controlled transformation Rate Thermal Analysis (CRTA) mode. The method is applied to 4 zeolites (3A, 4A, 5A and 13X) and a well characterized charcoal, from −25 to 325°C, after pre-adsorption of water.
Abstract
Water adsorption at temperatures of 286 and 296 K on silicalite-I, ZSM-5 (Si/Al=16), ZSM-48 (Si/Al=50) and AlPO4-5 is followed by gravimetry with a quasi-equilibrium continuous adsorptive introduction. The results show that all of these samples are characterized by a continuous distribution of strongly energetic water adsorption sites (from 60 to 120 kJ·mol−1) for which the adsorption is irreversible at the experimental temperature. This probably justifies the presence of hysteresis on desorption at very low relative pressure values. Adsorption of water in these systems firstly occurs by site. This is then followed by cluster formation and it is suggested that it is the ability of the adsorbent to build up these clusters within the microporous structure which determines intracrystalline uptake. It is put forward that the zeolites, silicalite-I and ZSM-5, do not accommodate cluster formation within its microporous network. However, an external flexible microporous structure, containing Lewis sites, may be present for large crystals. This flexible secondary structure may then be able to opened (swelled) at high relative pressures. On the other hand, for the aluminophosphate AlPO4-5, it is believed that a change in the aluminium coordination on the formation of a crystal hydrate together with capillary condensation results in a large step in the adsorption isotherm, which is itself preceded by a smaller step, revealing a brutal densification of the adsorbed phase.
The adsorption of argon, oxygen, nitrogen and carbon monoxide at 77 K on crystalline zirconia and microporous zirconia gels has been studied by adsorption volumetry and isothermal microcalorimetry.
The adsorption of argon and nitrogen on a series of MFI-type zeolites (silicalite-I (Si/Al>1000) and HZSM-5 (16<Si/Al<120)) was studied by isothermal microcalorimetry, volumetry and neutron diffraction.
