The reaction of 4-iodobenzenesulfonamide or 4-fluorobenzenesulfonamide with CS 2 and KOH in dimethylformamide yielded the potassium N-R-sulfonyldithiocarbimates, K 2 (RSO 2 N@CS 2) [R = 4-IC 6 H 4 (1) and 4-FC 6 H 4 (2)]. These salts reacted with K 2 [PtCl 4 ] in water/methanol to yield complex anions bis(N-R-sulfonyldithiocarbimato)platinate(II), which were isolated as their tetrabutylammonium salts, (Bu 4 N) 2 [Pt(RSO 2 N@CS 2) 2 ] [R = 4-IC 6 H 4 (3) and 4-FC 6 H 4 (4)]. The structures of 2-4 were determined by X-ray crystallography. The Pt 2+ in both complexes 3 and 4 lies at the inversion centre and the PtS 4 moiety has a distorted square-planar configuration. The compounds were also characterized by IR, 1 H NMR and 13 C NMR spectroscopies, and elemental analyses. The molar conductance data are consistent with the fact that 3 and 4 are dianionic complexes.
Highlight► The catalysts composite TiO 2 /MgZnAl-5, was more efficient than TiO 2 P25.► The effects of different molar ratios zinc on the photocatalysts were investigated.► Synergistic effect between constituents of TiO 2 /MgZnAl-5 increases the photocatalysis.► TiO 2 /MgZnAl-5 exhibited the adsorption of light displacing the greater wavelength.► The catalyst composite TiO 2 /MgZnAl-5 can be reused for five consecutive cycles.
AbstractPage 2 of 34 A c c e p t e d M a n u s c r i p t 2 A series of TiO 2 /MgZnAl photocatalysts, were successfully synthesized from ternary (Mg, Zn and Al) layered double hydroxides impregnated with TiO 2 nanoparticles by the co-precipitation method at variable pH with different Zn 2+ /Mg 2+ molar ratios . The composite photocatalysts were calcined at 500 °C resulting in the incorporation of oxide zinc, in the calcined MgZnAl LDH structure. Synergistic effect between ZnO and TiO 2 lead to significant enhancement of TiO 2 /MgZnAl photocatalytic activity. Composite photocatalysts were characterized by ICP-MS, N 2 adsorption/desorption, XRD, SEM, EDS, IR and UV-Vis DRS. Phenol in aqueous solution (50 mg/L) was used as a model compound for evoluation of UV-Vis (filter cutoff for λ > 300 nm) photocatalytic activity . The most efficient phocatalyst composite was obtained at a 5% Zn 2+ /Mg 2+ molar ratio , in the catalyst identified as TiO 2 /MgZnAl-5. This composite catalyst had high photocatalytic activity, completely destroying phenol and removing 80% of total organic carbon in solution after 360 min.The TiO 2 /MgZnAl-5 catalyst remained relatively stable, presenting a 15% decrease in phenol degradation efficiency after five consecutive photocatalytic cycles.
The new magnetic photocatalysts HT/TiO2/Fe and HT-DS/TiO2/Fe, modified with the anionic surfactant sodium dodecylsulfate (DS) were successfully synthesized in this work. Titanium dioxide (anatase) followed by iron oxide were deposited on the hydrotalcite support. Several catalyst samples were prepared with different amounts of titanium and iron. The photocatalysts were characterized by infrared and Raman spectroscopy, X-ray diffraction, scanning electron microscopy. Photocatalytic performance was analyzed by UV-visible radiation (filter cutoff, λ > 300 nm) of an aqueous solution (24 mg/L) of methylene blue (MB). The most efficient catalyst was obtained at an iron oxide:TiO2 molar ratio of 2:3. This catalyst showed high photocatalytic activity, removing 96% of the color and 61% of total organic carbon from the MB solution after 120 min. It was easily removed from solution after use because of its magnetic properties. The reuse of the HT-DS/TiO2/Fe23 catalyst was viable and the catalyst was structurally stable for at least four consecutive photocatalytic cycles.
Five new compounds with the general formula of (Bu(4)N)(2)[M(RSO(2)NCS(2))(2)], where Bu(4)N=tetrabutylammonium cation, (M=Ni, R=4-FC(6)H(4)) (1), (M=Zn, R=4-FC(6)H(4), 4-ClC(6)H(4), 4-BrC(6)H(4), 4-IC(6)H(4)), (2), (3), (4) and (5), respectively, were obtained by the reaction of the appropriate potassium N-R-sulfonyldithiocarbimate (RSO(2)N=CS(2)K(2)) with nickel(II) chloride hexahydrate or zinc(II) acetate dihydrate in metanol:water 1:1. The elemental analyses and the IR data are consistent with the formation of the expected bis(dithiocarbimato)metal(II) complexes. The (1)H and (13)C NMR spectra showed the signals for the tetrabutylammonium cation and the dithiocarbimate moieties. The compounds 1, 2 and 5 were also characterized by X-ray diffraction techniques. The nickel(II) is coordinated by two N-4-fluorophenylsulphonyldithiocarbimato(2-) ligands forming a planar coordination. The zinc(II) exhibits distorted tetrahedral configuration in compounds 2 and 5 due to the chelation effect of two sulfur atoms of the N-R-sulfonyldithiocarbimate ligands. The antifungal activities of the compounds were tested in vitro against Colletotrichum gloeosporioides, an important fungus that causes the plant disease known as anthracnose in fruit trees. All the complexes were active.
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