ChemInform Abstract: A Novel Method for the Preparation of Crystalline Silicic Acids

Schwieger, Wilhelm; Bergk, K.‐H.; Weise, M.; Porsch, Martin; Heidemann, D.

doi:10.1002/chin.198925032

Cited by 28 publications

(67 citation statements)

References 1 publication

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“…The gel obtained was transferred to the autoclave and treated at 423 K for 7 days. The synthesized Na-kenyaite (Na-Ken) was filtered, washed with deionized water to pH 7, and dried at 333 K for 48 h [10,22].…”

Section: Synthesis Of Na-kenyaitementioning

confidence: 99%

Organofunctionalized kenyaite for dye removal from aqueous solution

Royer

Cardoso

Lima

et al. 2009

Journal of Colloid and Interface Science

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Crystalline layered sodium kenyaite was exchanged to proton kenyaite when reacted with hydrochloric acid solution, providing a new surface with available silanol groups that are able to couple with N-3-trimethoxysilylpropylethylenediamine silylating agent, after prior expansion of the basal distance with the polar organic solvent dimethyl sulfoxide. The resulting organofunctionalized nanomaterial (2N-Ken) was characterized by elemental analysis, infrared spectroscopy, X-ray diffraction, carbon and silicon nuclear magnetic resonances in the solid state, surface analysis, porosity, thermogravimetry, and electron scanning microscopy. The quantity of silylating agent incorporated into the nanospace, calculated from the nitrogen elemental analysis, was determined as 0.48 mmol g(-1), after expanding of the acidic precursor basal distance from 1.62 to 1.99 nm. The presence of a covalent silicon-carbon bond of the organosilyl moiety on the inorganic layered structure was confirmed through nuclear magnetic resonance. This new nanomaterial has the ability to extract the Sumifix Brilliant Orange 3R textile dye from aqueous solution, using a batchwise process. The effects of stirring time, adsorbent dosage, and pH on the adsorption capacity demonstrated that 4 h is enough to reach equilibrium at 298+/-1 K under pH 4.0. Based on error function values (F(error)) the data were best fitted to fractional-order and chemisorption kinetic models when compared to pseudo-first-order and pseudo-second-order kinetic models. The equilibrium data were better fitted to the Sips isotherm model.

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Section: Synthesis Of Na-kenyaitementioning

confidence: 99%

Organofunctionalized kenyaite for dye removal from aqueous solution

Royer

Cardoso

Lima

et al. 2009

Journal of Colloid and Interface Science

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“…The gel was transferred to a stainless steel autoclave lined with Teflon for hydrothermal treatment during 9 days at 378 K. Then, the solid was filtered off and washed with doubly distilled water until neutral pH and air dried. 8,39 Synthesis of H-RUB-18…”

Section: Synthesis Of Na-rub-18mentioning

confidence: 99%

New inorganic–organic lamellar derivatives synthesized from H-RUB-18 and thermodynamics of cation sorption

Macedo

Airoldi

2009

New J. Chem.

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A synthesized crystalline lamellar sodium RUB-18 was reacted with hydrochloric acid solution to exchange the original hydrated sodium cation on the interlayer space to obtain the acidic form, H-RUB-18, whose silanol groups on the surface favour covalent bond formation with the silylating agents 3-aminopropyltriethoxysilane (N) and N-3-trimethoxysilylpropyldiethylenetriamine (3N). Both new organofunctionalized nanostructured materials were characterized by means of elemental analysis, IR spectroscopy, X-ray diffraction patterns, NMR, thermogravimetry and scanning electron microscopy. The determined maximum amount of coupling reagents incorporated were 2.28 and 1.03 mmol g À1 , for RUB-N and RUB-3N, respectively. The H-RUB-18 basal distance of 0.75 nm expands to 0.94 and 1.10 nm in two successive steps of reaction. Covalent bond formation between the organosilyl groups and the inorganic layered backbone was confirmed by 13 C and 29 Si NMR, as evidenced by carbon chemical shifts of the pendant organic chains and by the Q 3 and Q 4 sites, in addition to T 2 and T 3 species, that correspond to carbon-silicon bond formation from the pendant coupling reagents covalently attached to the H-RUB-18 structure. These two new synthesized materials have the ability to extract divalent cations from aqueous solution, using a batchwise process. The same interaction was also followed through calorimetric titration and the thermodynamic data, with high entropic contributions, indicated favourable cation/basic centre interactions at the solid/liquid interface.

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“…Herein we use a new approach that takes advantage of the joint effects of chemical shielding and dipolar interactions under slow magic‐angle‐spinning conditions to provide detailed information on the geometry of hydrogen‐bonded silanols in octosilicate10a (also known as ilerite10c or RUB‐1811), a prominent member of the layered hydrous sodium silicates 12. This class of material, available only in microcrystalline form, has a 2D layered structure in which the negative charge of the silicate layer is compensated by sodium ions coordinated by the oxygen atoms of the intercalated water molecules 10–17.…”

Section: Si and 1h Nmr Shift Tensor Parameters (In Ppm From Tms) Almentioning

confidence: 99%

Exploiting the Joint Action of Chemical Shielding and Heteronuclear Dipolar Interactions To Probe the Geometries of Strongly Hydrogen‐Bonded Silanols

et al. 2004

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Magic probes: The geometry of strongly hydrogen bonded silanols in octosilicate can be probed by exploiting the 1H NMR distance correlations together with the joint effects of 29Si chemical shielding and dipolar 1H–29Si interactions. Dipolar‐modulated, slow magic‐angle spinning 29Si NMR spectra allow the determination of Si⋅⋅⋅H distances, the magnitude of the 29Si chemical‐shielding tensor, and its orientation in the molecular frame.

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ChemInform Abstract: A Novel Method for the Preparation of Crystalline Silicic Acids

Abstract: ChemInform Abstract (protonization of sodium magadiite using hydrolyzable compounds such as e.g. chloro-dimethyl ether or by adsorption of organic compounds (methanol, methylal) and subsequent treatment with HCl).

Cited by 28 publications

References 1 publication

Organofunctionalized kenyaite for dye removal from aqueous solution

Organofunctionalized kenyaite for dye removal from aqueous solution

New inorganic–organic lamellar derivatives synthesized from H-RUB-18 and thermodynamics of cation sorption

Exploiting the Joint Action of Chemical Shielding and Heteronuclear Dipolar Interactions To Probe the Geometries of Strongly Hydrogen‐Bonded Silanols

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