Abstract
Activation of natural sepiolite by means of grinding in a planetary mill followed by wet NaOH activation was studied for the purpose of endowing the product with enhanced basicity for potential catalytic/sorptive applications. Synthesized solids were characterized with X-ray powder diffraction (XRD), N2 adsorption/desorption, scanning electron microscopy (SEM), energy dispersive (EDX), atomic absorption (AAS), Fourier-transform infrared (FTIR) and 29Si magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopies. Surface basicity was determined by titration with benzoic acid. Grinding changed the pathway of sepiolite phase transformation upon NaOH treatment. The as-received sepiolite evolved to Na-sepiolite (loughlinite) with a micropore system blocked by nanocrystalline Mg(OH)2, while ground samples yielded magnesium silicate hydrate phase (MSH), with well-developed microporous texture. In unmilled sepiolite desilication involved preferential leaching of Si from the center of the structural ribbons, while in ground samples additional loss of Si from ribbon-ribbon corner linkages was observed. In all cases treatment with NaOH led to enhancement of surface basicity. Synthesized materials were tested as catalysts in a base-catalyzed aldol self-condensation of acetone and oxidation of cyclohexanone to ε-caprolactone, as well as CO2 sorbents. Catalytic trends depended not only on samples’ basicity, but also on texture and phase composition of the catalysts. Grinding combined with alkali activation proved a simple and effective method for boosting CO2-sorption capacity of sepiolite to the level comparable to amine-functionalized, acid-activated sepiolite sorbents.
Highlights
Grinding of clay minerals is a very common treatment used both at the industrial scale and in research laboratories
The results indicated that the magnesium silicate hydrate (MSH) phase, developed in alkali-treated ground sepiolite, was catalytically less active than the nanocrystalline Mg(OH)2 particles formed in the NaOH-activated parent sepiolite
The study revealed that grinding pretreatment of natural sepiolite changed the pathway of phase transformation of this mineral upon treatment with NaOH solution
Summary
Grinding of clay minerals is a very common treatment used both at the industrial scale and in research laboratories. Catalysis, of mineral mineralfillers, fillers,ceramic ceramicindustry, industry,agriculture, agriculture, pharmacology, cosmetology, Another type of modification of clay mineral is activation with acid or base, in order to selectively etc. Another type of modification of clay mineral is activation with acid or base, in order to selectively leach basic basic or oracidic acidicelements, elements,respectively respectively[3,4]. Such treatment modifies mineral porosity leach treatment modifies the the mineral porosity by by creating voids within the clay lattice, and endows the material with enhanced acid or base creating voids within the clay lattice, and endows the material with enhanced acid or base properties, properties, factors of crucialfor importance forinapplications catalysisAsand sorption.
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