Given the fact that the literature describing the intercalation of organic molecules in monometallic LDH systems is scarce, the present investigation is aimed at the generation of ethylene glycol intercalated Fe-Fe LDH with the objective of enhancing the surface area for further catalytic applications of industrially important and environmentally harmful organics. The solvothermal reaction of FeCl with urea in an ethylene glycol medium yielded a brown colored powder which was characterized employing a wide range of analytical techniques including high resolution powder X-ray diffraction (PXRD), scanning electron microscopy, thermal analysis, X-ray photo electron spectroscopy (XPS), elemental (C, H, N and S) analysis, UV-visible, photoluminescence spectroscopy measurements, BET surface area and pore-size analysis. The observed reflections in the PXRD pattern were indexed in a rhombohedral symmetry with a = 3.175 and c = 31.9 Å. Combining the results from the Fe 2p core level analysis and anion contents from elemental and thermogravimetric analysis, a formula of Fe Fe (OCH) (OH) was deduced for the sample. The intercalation of EG in the interlayer was confirmed from FTIR and Raman spectroscopy measurements. The d-d transitions of the Fe-ion and the charge transfer transition of the Fe(ii)-Fe(iii) lattice were evident in the UV-visible spectrum. Blue indigoid emission bands arising from the transitions present in the Fe-ion were noticed in the photoluminescence spectrum. The measured BET surface area and pore diameter of the sample were 144 m g and 12.5 nm, respectively. Almost instant decolourisation of the Xylenol Orange (XO) dye occurred in the presence of HO and the LDH sample as catalyst. Similar observations were encountered for Methyl Orange (MO) and Methylene Blue (MB) dyes. All these reactions followed pseudo first-order kinetics. The industrially important reductive conversion of nitro aromatics was catalyzed by the sample. The selective reduction of 2,4-dinitrophenol to 2-amino-4-nitrophenol was effected almost instantaneously by this catalyst. Both the reusability and possible mechanism of catalytic action have been discussed. The EG intercalated Fe-Fe LDH influenced the relaxivity value of protons as determined from NMR spectroscopy experiments.
Polyaniline was synthesized by the chemical oxidative polymerization procedure at room temperature employing hydrogen peroxide (H 2 O 2 ) as oxidant and ferrous chloride (FeCl 2 Á2H 2 O) and vanadyl sulphate (VOSO 4 ÁH 2 O) as co-catalysts, respectively. The obtained polymers were characterized by high resolution powder X-ray diffraction, Fourier transform infrared spectroscopy, Raman, UV-Visible, photoluminescence spectroscopy, thermogravimetric Field Emission Scanning Electron Microscopy (FESEM) and Transmission Electron Microscopy (TEM) techniques. Ordered arrangement indicative of semi-crystalline nature of polyaniline was evidenced from the presence of intense reflection at d ¼ 13.72 Å in the powder X-ray diffraction pattern followed by two lesser intense peaks at 4.61 and 3.47 Å . Fourier transform infrared spectroscopy and Raman spectroscopic results indicated the polyaniline to be emeraldine salt form. Fibrous morphology was observed in scanning electron microscope images. Nearly 93% of Methyl Orange dye was adsorbed in 30 min by the ordered polyaniline at room temperature. No significant difference in the crystallinity and/or ordering was noticed in the powder X-ray diffraction pattern after dye adsorption. The correlation between the ordered structure of polyaniline and its higher adsorption property derived in the current study has the potential to fabricate devices consisting polyaniline to detect dye molecules.
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