0000000000131809
AUTHOR
H. Reichert
Investigation of the porosity of silica and alumina with chemically bonded polystyrene
The effect of modification of porous silica and alumina with a copolymer of styrene and vinylsilane on the porosity of oxides have been investigated by means of low temperature nitrogen sorption. Only small changes of the specific surface area and of the specific pore volume were observed on modification of oxides with non-cross-linked copolymer. The specific surface area significantly increased after the cross-linking of the deposited polymeric layer while the specific pore volume remains almost unaffected. A broad hysteresis loop appears in the nitrogen sorption isotherm for the alumina modified with the cross-linked polymer. The porosity of oxides modified by chemisorption method differe…
Confinement in micropores and enthalpies of physisorption
Abstract The use of quasi-equilibrium volumetry associated with isothermal microcalorimetry at 77 K allows direct measurement of the interactions on adsorption of simple probe molecules within well crystallised aluminophosphate and zeolite molecular sieves. Four particular cases are presented which show: the effect of varying micropore diameter, the effect of adsorbing molecules with a favourable geometric compatibility with a given micropore system, the effect of varying the field potential within a given micropore system and finally, the effect of variable selective blocking of the micropore system.
A microcalorimetric study of the different states of argon and nitrogen adsorbed AT 77 K on silicalite-I and ZSM-5
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.
Synthesis And Sorptive Properties Of Dodecasil 1 H With An Acessible Pore System
Abstract The synthesis of Dodecasil 1H was studied in the system SiO2/1-adamantylamine/NH3/water with the objective of controlling the particle size and the morphology of the crystals. Since nucleation occurs in a very early stage of the synthesis, the heating rate to the final temperature have a strong influence on both parameters. Using seed crystals and such a heating programme, the expensive template 1-adamantylamine can be reduced to so small amounts, that a nearly template free pore system is achieved. The emptiness of the pore system was demonstrated from adsorption measurement using He and H2.
High-resolution physisorption techniques for the characterization of adsorbents and catalysts
Abstract High-resolution physisorption techniques performed in the continuous volumetric mode have been developed to investigate the surface and pore structure properties of porous solids. Physisorption data on well-defined microporous solids (zeolites and aluminophosphates) provide novel information on the mechanism of micropore filling, the behavior of the adsorbed phase and the pore structure of the adsorbent. The combination of physisorption with high-resolution analytical techniques such as calorimetry and neutron diffraction further expands our knowledge and understanding of physisorption processes. The results are not only important for fundamental research but can be applied in the …
Investigation on the Adsorption of N2 Ar, CO and CH4 on Aluminophosphates
Abstract Adsorption isotherms at different temperatures and isothermal micro-calorimetric curves were measured for N2 Ar, CO, and CH4 on various molecular sieves as VPI-5, MCM-9, AlPO4-8, AlPO4-H, AlPO4-5, SAPO-5, AlPO4-39, AlPO4-C. It was shown that the isosteric heats of adsorption correlated with the pore-sizes of the studied molecular sieves.
High-resolution sorption studies of argon and nitrogen on large crystals of microporous zeolite ZSM-5
High resolution adsorption (HRADS) with argon and nitrogen at 77 K were performed on large crystals of zeolite ZSM-5 using a novel volumetric device. Multi-step isotherms for both adsorptives could be observed for the first time. The micropore filling was followed by low temperature microcalorimetry. Exothermic heats of adsorption were found to be correlated with steps in the adsorption isotherms. Based on results from atom-atom potential energy calculations (AAP) as well as from independent model building it is shown that 24 kinetic adsorbate molecules can be situated in a ZSM-5 unit cell. Localized adsorption is presented as possible filling mechanisms. Experimental results are reasonably…
Sorption of argon and nitrogen on network types of zeolites and aluminophosphates
Abstract Synthetic zeolites and aluminophosphates comprising 10- and 12- membered ring openings, unidimensional and network type of pore systems (MFI, MEL, ERI, LTA, AEL, AFI and FAU) were used as model adsorbents to examine the impact of micropore structure on the sorption properties. Argon and nitrogen were employed as adsorptives. Adsorption measurements were carried out on gravimetric and volumetric sorption devices and also monitored by microcalorimetry. From the low coverage regime of the isotherm Henry's constants and isosteric heats of adsorption were derived. Both quantities allowed the discrimination between 10- and 12- membered ring systems. Unidimensional 10- and 12- membered ri…