Rotational State Change of Acetonitrile Vapor on MCM-41 upon Capillary Condensation with the aid of Time-Correlation Function Analysis of IR Spectroscopy

The infrared spectra of adsorbed acetonitrile on MCM-41 (porewidth = 3.2 nm) were measured at 303 K. In the CN stretching ν2 region, two bands were observed at 2265 cm− 1 and 2254 cm− 1, assigned to hydrogen-bonded molecules on surface hydroxyls of MCM-41, and physisorbed molecules in mesopores, respectively. We designate here the 2265 cm− 1 band as the ν2α band and the 2254 cm− 1 band as the ν2β band. The bandwidth of the fundamental transition ν2fβ, was obtained by removing the overlap with hot band transitions of the same mode, ν2α band, and other modes by least-squares fitting. Before capillary condensation, the relaxation time τ obtained from the bandwidth of the ν2fβ band was smaller …

Novel pathways for the preparation of mesoporous MCM-41 materials: control of porosity and morphology

Two novel synthesis routes for the preparation of mesoporous MCM-41 materials are introduced. Both methods use tetra-n-alkoxysilanes such as tetraethoxysilane (TEOS) or tetra-n-propoxysilane (TPS) as a silica source which are added to an aqueous solution of a cationic surfactant in the presence of ammonia as catalyst. In this study, n-alkyltrimethylammonium bromides and n-alkylpyridinium chlorides were employed as templates. The addition of an alcohol (e.g. ethanol or isopropanol) leads to a homogeneous system which allows the formation of spherical MCM-41 particles. The main advantages of these methods are short reaction times, excellent reproducibility and easy preparation of large batche…

Molecular mechanism of capillary condensation of acetonitrile vapor on MCM-41 with the aid of a time-correlation function analysis of IR spectroscopy

Abstract The adsorption isotherm and IR spectra of acetonitrile adsorbed on MCM-41 (pore-width=3.2 nm) were measured at 303 K. The adsorption isotherm had a sharp jump at P / P 0 =0.3 without adsorption hysteresis. The CN stretching ν 2 -band of adsorbed acetonitrile had two-component α- and β-bands at 2263 and 2254 cm −1 , respectively, assigned to hydrogen-bonded molecules on surface hydroxyls of MCM-41 and physisorbed molecules in mesopores whose walls are coated with hydrogen-bonded molecules, respectively. The β-band was analyzed with a time correlation function, giving a reorientation time τ . The τ value of the adsorbed molecule before capillary condensation was smaller than that of …

A Novel Pathway for Synthesis of Submicrometer-Size Solid Core/Mesoporous Shell Silica Spheres

Tailored syntheses of nanostructured silicas: Control of particle morphology, particle size and pore size

Ordered mesoporous silicas with spherical morphology and average particle size in the range between 100 nm and 2 μm were synthesised according to two novel routes. Both synthesis routes used tetraethoxysilane, water, alcohol and aqueous ammonia for producing spherical silica beads. The porosity was created by adding two different kinds of pore structure directing agents to the starting solution: one was an n-alkyltrialkoxysilane which was covalently bonded to the silica framework, the other was an n-alkylamine which acted as a nonionic template. After calcination and post treatment the resulting particles showed a specific surface area up to 1000 m2 g-1, a specific pore volume of up to 0.8 …

Novel route in the synthesis of MCM-41 containing framework aluminum and its characterization

Abstract Mesoporous molecular sieve MCM-41 with incorporated structural aluminum (Al-MCM-41) was prepared by hydrolysis of a solution of tetraethoxysilane and aluminum isopropoxide in the presence of ammonia as a catalyst. This method provides Al-MCM-41 of different Si/Al ratios from 13 to 297 corresponding to 0.3–7 mol% Al within an hour. X-ray diffraction and nitrogen adsorption measurements showed that the Al-MCM-41 prepared by this method had a highly ordered structure of pore arrays. Most Al atoms in these samples were incorporated tetrahedrally in the MCM-41 structure, which gave rise to cationic sites in the framework.