The Synthesis of Copper(II) Salicylaldiminato Complexes and their Catalytic Activity in the Hydroxylation of Phenol

2007 ◽  
Vol 62 (3) ◽  
pp. 331-338 ◽  
Author(s):  
Juanita L. van Wyk ◽  
Selwyn Mapolie ◽  
Anders Lennartson ◽  
Mikael Håkansson ◽  
Susan Jagner

The synthesis of copper(II) salicylaldiminato complexes and their application in the catalytic hydroxylation of phenol is reported. Tetracoordinated copper complexes (Cu(Ln)2) were obtained by reacting the N-phenylsalicylaldimine ligands (HL1 -HL7) with copper acetate in a 2 : 1 mole ratio. The reaction of N-(2,6-diisopropyl)phenyl-3,5-di-tert-butylsalicylaldimine (HL7) with copper acetate in a 1 : 1 mole ratio afforded a dinuclear complex, which was not obtained with the other ligand systems. All complexes were characterized using FT-IR and elemental analysis. X-Ray crystal structures of complexes 2, 5 and 8 have also been obtained. The catalytic activity of these complexes was evaluated in the hydroxylation of phenol using oxygen and hydrogen peroxide as co-oxidants in aqueous media in the pH range 3 - 6. All complexes studied were found to be active for the hydroxylation process over the pH range studied with higher selectivity for catechol formation.

2017 ◽  
Author(s):  
◽  
Sharista Raghunath

The presence of dyes in effluent poses various environmental as well as health hazards for many organisms. Although various remediation strategies have been implemented to reduce their effect, dyes still manage to infiltrate into the environment and hence new strategies are required to address some of the problems. This study investigated the innovation of two cationic water-soluble polymers viz., Proline-Epichlorohydrin-Ethylenediamine Polymer (PEP) and Thiazolidine-Epichlorohydrin-Ethylenediamine Polymer (TEP) that were used to remediate selected synthetic dyes from synthetic effluent by adsorption and dye reduction. Both polymers were synthesized using monomers of a secondary amine, epichlorohydrin and ethylenediamine and were subsequently characterized and modified and their remediation potential studied. In the first study, PEP was synthesized and characterized by 1H-NMR Spectroscopy, FT-IR Spectroscopy, dynamic light scattering, and thermogravimetric analysis (TGA). Thereafter PEP was modified with bentonite clay, by simple mixing of the reactants, to form a Proline-Epichlorohydrin-Ethylenediamine Polymer-bentonite composite (PRO-BEN); it was characterized by FT-IR Spectroscopy, scanning electron microscopy (SEM)/ energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Adsorption studies were then undertaken with a synthetic effluent containing three textile dyes, viz., Reactive Blue 222 (RB 222), Reactive Red 195 (RR 195) and Reactive Yellow (RY 145). Various conditions were investigated including pH of the solution, temperature, sodium chloride concentration, initial dye concentration and the dosage of adsorbent used. The experimental data for all dyes followed a Langmuir isotherm. The adsorption process was found to be pseudo-second order. According to the thermodynamic parameters, the adsorption of the dyes was classified as physisorption and the reaction was spontaneous and exothermic. The data were also compared using studies with alumina as an adsorbent. Results showed that PRO-BEN exhibited better absorptivity and desorption than alumina making its use a better recyclable remediation strategy for the removal of organic dyes in wastewater treatment plants. In the second study, TEP was synthesized and then characterized by FT-IR Spectroscopy, 1H-NMR Spectroscopy, TGA and DLS. Thereafter, TEP was used to prepare TEP capped gold nanoparticles (TEP-AuNPs). Herein, two methods were investigated: the Turkevich method and an adaptation of the Turkevich method using bagasse extract. The TEP-AuNPs was characterized by FT-IR Spectroscopy, SEM, EDX, DLS and TEM. Thereafter the reduction of each of Allura Red, Congo Red and Methylene Blue was investigated with the TEP-AuNPs for its catalytic activity toward dye reduction. This study showed that the batch of AuNPs prepared by the Turkevich method had higher rates of dye reduction compared with AuNPs prepared using bagasse extract. Also the quantity of TEP used as capping agent greatly influenced the size, shape and surface charge of the nanoparticles as well as their catalytic performance: the Vroman effect explained this behavior of the TEP-AuNPs. It was finally concluded that whilst PRO-BEN, in the first study, showed excellent dye remediation properties, the second study on TEP-AuNPs showed good catalytic activity for the reduction of selected dyes, however, it was more effective at lower polymer concentration. Finally, both materials displayed good potential for the clean-up of selected synthetic dyes from synthetic effluents.


2020 ◽  
Vol 2020 ◽  
pp. 1-7 ◽  
Author(s):  
Umair Qasim ◽  
Zulfiqar Ali ◽  
Muhammad Shahid Nazir ◽  
Sadaf Ul Hassan ◽  
Sikander Rafiq ◽  
...  

Environmental concerns due to excessive use of synthetic or petroleum-based materials have encouraged scientists to develop novel, sustainable, and multifunctional material using abundant lignocellulosic biomass. In this work, a study was conducted on the isolation of cellulose from wheat straw using two different methods: acidified sodium chlorite and alkaline hydrogen peroxide. A comparative study was carried out based on the yield and properties of extracted cellulose. The final product (after treatments) was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and thermogravimetric analysis (TGA) for the identification of properties. Both the treatments isolated pure white color cellulose. However, the yield of cellulose isolated through acidified sodium chlorite treatment (81.4%) was higher than alkaline hydrogen peroxide treatment (79%). Moreover, no huge difference was observed in the crystallinity and thermal properties of extracted cellulose.


Author(s):  
Pelin Aktaş

BaTi5O11 has been widely researched due to its unique microwave properties. Conventionally it is challenging to obtain this compound as a single phase. The BaTi5O11 was synthesized via co-precipitation technique using an aqueous solution of titanium(IV)(triethanolaminato) isopropoxide, barium nitrate and ammonia as precursors which are stable in an aqueous media. The phase evolution, purity, and structure were identified by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive X-ray (EDX) spectroscopy analysis. The desired BaTi5O11 structure was obtained by calcination at 900?C. Furthermore, the structure is characterized by TGA, FT-IR and Raman studies. The study showed that the particles were between 80 and 120 nm in size and the average crystallite size was determined from the Scherrer formula as 68.1 nm at 900?C.


Catalysts ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1235
Author(s):  
Muliani Mansor ◽  
Sharifah Najiha Timmiati ◽  
Wai Yin Wong ◽  
Azran Mohd Zainoodin ◽  
Kean Long Lim ◽  
...  

The direct methanol fuel cell (DMFC) is a portable device and has the potential to produce 10 times higher energy density than lithium-ion rechargeable batteries. It is essential to build efficient methanol electrooxidation reaction electrocatalysts for DMFCs to achieve their practical application in future energy storage and conversion. A catalyst consisting of nickel–palladium supported onto mesostructured silica nanoparticles (NiPd–MSN) was synthesized by the wet impregnation method, while MSN was synthesized using the sol-gel method. MSN act as a catalyst support and has very good characteristics for practical support due to its large surface area (>1000 m2/g) and good chemical and mechanical stability. The microstructure and catalytic activity of the electrocatalysts were analyzed by X-ray diffraction (XRD), Fourier transform infrared (FTIR), field emission scanning electron microscopy (FESEM), Brunauer–Emmet–Teller (BET) theory, X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), and chronoamperometry (CA). XRD showed that the NiPd–MSN electrocatalysts had a high crystallinity of PdO and NiO, while FESEM displayed that NiPd was dispersed homogeneously onto the high surface area of MSN. In alkaline media, the catalytic activity toward the methanol oxidation reaction (MOR) of NiPd–MSN demonstrated the highest, which was 657.03 mA mg−1 more than the other electrocatalysts. After 3600 s of CA analysis at −0.2 V (vs. Ag/AgCl), the MOR mass activity of NiPd–MSN in alkaline media was retained at a higher mass activity of 190.8 mA mg−1 while the other electrocatalyst was significantly lower than that. This electrocatalyst is a promising anode material toward MOR in alkaline media.


2011 ◽  
Vol 284-286 ◽  
pp. 909-912
Author(s):  
Bo Wei ◽  
Bing Shi Li ◽  
Hong Ding ◽  
Yuan Gao

Using a long alkyl-polyamine triethylene-tetramine as structure-directing agent, FeZSM-35 zeolites were synthesized and characterized by XRD, SEM, FTIR and TG-DTA techniques. EDS and ICP-AES indicate that the transition metal iron ions were framework elements and the mass fraction was 0.48%. The catalytic activity of as-synthesized crystals was examined for the aqueous hydroxylation of phenol with hydrogen peroxide. The phenol conversion was 18.8% and the selectivity on catechol and hydroquinone wasca.69.1% and 30.9%, respectively. The as-synthesized FeZSM-35 zeolites show relative high selectivity towards catechol and could be a promising catalyst.


2016 ◽  
Vol 20 (06) ◽  
pp. 677-688 ◽  
Author(s):  
Ahmad Shaabani ◽  
Zeinab Hezarkhani

Functionalized wool with cobalt(II), copper(II), and iron(II) tetrasulfophthalocyanine (CoTSPc@wool, CuTSPc@wool, and FeTSPc@wool) have been synthesized and their structures characterized by flame atomic absorption spectroscopy (FAAS), FT-IR, UV-vis, X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and the energy dispersive spectroscopy (EDS) analysis. The catalytic activity of the synthesized catalysts was investigated for the aerobic oxidation of alkyl arenes and alcohols to their corresponding carbonyl compounds in the absence of any co-promoter and additional oxidizing reagent. We found the best catalyst for the mentioned reactions is the CoTSPc@wool from the solvent, conversion, temperature, and reaction time point of views. The synthesized catalysts can be readily recycled and reused for several runs without significant loss of efficiency.


Polyhedron ◽  
2017 ◽  
Vol 124 ◽  
pp. 77-85 ◽  
Author(s):  
Paranthaman Vijayan ◽  
Panneerselvam Anitha ◽  
Mani Rajeshkumar ◽  
Periasamy Viswanathamurthi ◽  
Paramasivam Sugumar ◽  
...  

2019 ◽  
Vol 75 (7) ◽  
pp. 872-876
Author(s):  
Lukáš Krivosudský ◽  
Alexander Roller ◽  
Annette Rompel

The monovanadium-substituted polyoxometalate anion [VMo7O26]5−, exhibiting a β-octamolybdate archetype structure, was selectively prepared as pentapotassium [hexaikosaoxido(heptamolybdenumvanadium)]ate hexahydrate, K5[VMo7O26]·6H2O (VMo7 ), by oxidation of a reduced vanadomolybdate solution with hydrogen peroxide in a fast one-pot approach. X-ray structure analysis revealed that the V atom occupies a single position in the cluster that differs from the other positions by the presence of one doubly-bonded O atom instead of two terminal oxide ligands in all other positions. The composition and structure of VMo7 was also confirmed by elemental analyses and IR spectroscopy. The selectivity of the synthesis was inspected by a 51V NMR investigation which showed that this species bound about 95% of VV in the crystallization solution. Upon dissolution of VMo7 in aqueous solution, the [VMo7O26]5− anion is substantially decomposed, mostly into [VMo5O19]3−, α-[VMo7O26]4− and [V2Mo4O19]4−, depending on the pH.


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