Abstract
A two-step reaction sequence, dealumination via thionyl chloride followed by reaction with a Grignard reagent, has created a nanoscale morphology that appears as significantly roughened outer surfaces on zeolite 4A particles. X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) measurements revealed that such surface nanostructures are composed of Mg(OH)2 crystals. The formation mechanism of this specific surface morphology was explored. It was discovered by solid-state 29Si and 27Al NMR and XPS surface analysis that thionyl chloride partially removes aluminum from the zeolite 4A framework and yields NaCl and AlCl3. Precipitation of these extracted inorganic salts on the surfaces of zeolite particles occur. Subsequently, methylmagnesium bromide is reacted with 2-propanol in a quenching process and generates Mg(OH)2. The previously deposited NaCl and AlCl3 nanoparticles on zeolite surfaces are believed to function as heterogeneous nuclei for the growth of Mg(OH)2 crystals and thereby creates ...
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