Characterization of a hybrid-smectite nanomaterial formed by immobilizing of N-pyridin-2-ylmethylsuccinamic acid onto (3-aminopropyl)triethoxysilane modified smectite and its potentiometric sensor application

Abstract

A novel N-pyridin-2-ylmethylsuccinamic acid-functionalized smectite nanomaterial was synthesized by immobilizing of N-pyridin-2-ylmethylsuccinamic acid through chemical bonding onto (3-aminopropyl)triethoxysilane modified smectite. The structural, thermal, morphological and surface properties of raw, silane-grafted and the N-pyridin-2-ylmethylsuccinamic acidfunctionalized smectites were investigated by various characterization techniques. The thermal analysis data showed the presence of peaks in the temperature range from 200 °C to 600 °C due to the presence of physically adsorbed silanes, intercalated silanes, surface grafted silanes and chemically grafted silane molecules between the smectite layers. The powder x-ray diffraction patterns clearly indicated that the aminopropyl molecules also intercalated into the smectite interlayers as bilayer arrangement whereas N-pyridin-2-ylmethylsuccinamic acid molecules were only attached to 3-aminopropyltriethoxysilane molecules on the external surface and edges of clay and they did not intercalate. Fourier transform infrared spectroscopy confirms N-pyridin-2ylmethylsuccinamic acid molecules bonding through the amide bond between the amine group of aminopropyltriethoxysilane molecules and a carboxylic acid functional group of N-pyridin-2ylmethylsuccinamic acid molecules. The guest molecules functionalized onto the smectite caused significant alterations in the textural and morphological parameters of the raw smectite.

Effect of Calcination Temperature on the Phase Composition, Morphology, and Thermal Properties of ZrO2 and Al2O3 Modified with APTES (3-aminopropyltriethoxysilane)

“…Most importantly, -NH2 groups were present, which can improve the adhesion of the ceramic to the polymer. Two peaks responsible for -NH2 deformation modes at 1562 cm −1 and 1484 cm −1 were identified, which strongly confirm hydrogen-bonded structures with silanol groups to the zirconia and alumina [29][30][31][32]. There were also peaks at 1143-1199 cm −1 , which were associated with the Si-O moieties of either polymerized or physisorbed The PSD measurements of the powders after calcination at different temperatures showed that for ZrO 2 , the main peak did not vary in a particular direction, but between 100 and 2000 µm, the powder agglomeration became worse upon increasing the temperature.…”

“…Most importantly, -NH 2 groups were present, which can improve the adhesion of the ceramic to the polymer. Two peaks responsible for -NH 2 deformation modes at 1562 cm −1 and 1484 cm −1 were identified, which strongly confirm hydrogen-bonded structures with silanol groups to the zirconia and alumina [29][30][31][32]. There were also peaks at 1143-1199 cm −1 , which were associated with the Si-O moieties of either polymerized or physisorbed APTES [31].…”

“…In the final range above 500 • C, the dehydroxylation of residual ZrOH groups occured. Loss (IV) is associated with the dehydroxylation of grafted APTES species [32][33][34]. For alumina, the curve has a similar shape, but the thermal decomposition is more linear without several stages.…”

Construction of a novel highly selective potentiometric perchlorate sensor based on neocuproine–Cu(II) complex formed in situ during the conditioning period

“…For the fabrication of the electrodes, the similar procedure given in our previous work was followed [23]. At the first stage, to obtain conductive and compatible surfaces for the adherence of the selective PVC-membranes, a mixture of 50% (w/w) graphite powder, 35% (w/w) epoxy and 15% (w/w) hardener was prepared by dissolving in adequate tetrahydrofurane (THF) and coated on the one open end of the shielded copper wires with a length of 5.0 cm and a radius of 0.5 mm when the appropriate viscosity was obtained.…”

“…In this context, earlier our research group has reported a number of cation and anion selective electrodes [19][20][21][22][23] and ongoing studies have been motivated on the development of novel ion selective electrodes for different species.…”