Sharif Digital Repository

In this study, we investigate the use of catalytic copper-silver-palladium substrates for the growth of multiwalled carbon nanotubes via the thermal chemical vapor deposition. These layers are comprised of nanocrystals of Cu2O, CuO, Ag, Pd, Cu, and PdO and were grown using a DC magnetron sputtering method. Scanning electron microscopy characterizations confirmed the significant growth of carbon nanotubes on the catalytic layer. A comparison of the growth of nanotubes indicated that the thickness of the catalytic layers has a significant impact on the quality and the diameter of the carbon nanotubes. Two major peaks were seen in the Raman spectrum. The formation of graphite multiwalled... 

This is the first study of samarium powder catalyzed cyanation reaction of aryl halides, bearing electron-withdrawing and electron-releasing substituents, in the presence of NaCN to afford corresponding benzonitriles in high yields. This protocol takes the advantage of being done in the absence of additive, ligand and precious transition metals such as palladium. © 2019 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim  

A new zwitterionic Palladium (II) complex has been synthesized by the one-pot mixing of Pd(OAc)2, 2-aminophenol and (3-formyl-4-hydroxy-5-methylbenzyl) triphenylphosphonium chloride, in refluxing ethanol. The metal complex formed was characterized by 1H NMR, 13C NMR, 31P NMR and X-ray crystallographic technique and its efficiency tested as a homogeneous pre-catalyst in Heck-Mizoroki cross coupling reaction using γ-Valerolactone (GVL) as a biomass-derived green medium. All the products were obtained in good to excellent yields. © 2019  

We have explored the suitability of an O,N,N–donor Schiff base (H2SB) for obtaining dinuclear complexes with heavy metal ions such as Cu2+, Zn2+, Ni2+, and Co2+ (borderline acids) as well as Pd2+ and Cd2+ (soft acids). Spectroscopic studies demonstrated that the complexation of H2SB and Cu2+, Zn2+, Ni2+, Co2+, Pd2+, and Cd2+ occurred at a 1:1 stoichiometry. We have found two square planar centers with Pd-N-Pd angles of 93.08(11)◦ and a Pd–Pd distance of 3.0102(4) Å in Pd2(SB)2·Me2CO. This Pd–Pd distance is 30% shorter than the sum of the van der Waals radii, which is in accordance with a strong palladophilic interaction. Fluorescence studies on H2SB-M2+ interaction showed that H2SB can... 

In this work, PtxPd1-x (x = 0, 0.5, and 1)nanoparticles (NPs)were synthesized on the surface of SiO2@graphene oxide which covered by 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim]PF6)ionic liquid (IL)layer. FT-IR spectroscopy, zeta potential, CHN elemental analysis, XRD, XPS, SEM, EDX, TEM, TGA, BET, and ICP-AES techniques were applied for the characterization of the multiphasic catalyst. The as-prepared nanocomposite was used as an effective heterogeneous catalyst for the oxidation of cyclohexene by molecular oxygen, as a green oxidant. Different experimental conditions such as oxygen pressure, reaction time, reaction temperature and amount of catalyst were investigated in this... 

A resin-bound 1,2,4-triazolium ionic tag has been used as support for the preparation of solid palladium nanoparticles (Pd(0)-POLI-TAG-Pd). Owing to the pincer-type architecture of the triazolium ligand, the stabilization of a high amount of palladium nanoparticles (16 wt %) has been possible. The catalytic system has been fully characterized and used in low amounts (i.e., 0.1 mol % palladium loading) in representative Heck-Mizoroki cross-coupling processes. A negligible release of the metal was demonstrated, and a high activity was obtained over more runs. Besides, the protocol has been optimized for the use of safe biomass-derived γ-valerolactone reaction medium  

We report a facile method to synthesize a magnetically separable Pd-rGO/CNT/CaFe2O4 photocatalyst. The incorporation of CNTs into rGO can form a conductive network structure to bridge the gaps between rGO sheets. This conductive network can prevent the restacking of GO nanosheets during the reduction process. Also, for photocatalysis, the aforementioned conjugated network can provide rapid electronic conducting channels. It was found that the Pd-rGO/CNT/CaFe2O4 nanocomposite is an efficient photocatalyst for the Heck-Mizoroki coupling reaction under irradiation of visible light. Interestingly, the electrons which are excited by the photons can be transferred to the palladium nanoparticles... 

We report a facile method to synthesize a magnetically separable Pd-rGO/CNT/CaFe2O4 photocatalyst. The incorporation of CNTs into rGO can form a conductive network structure to bridge the gaps between rGO sheets. This conductive network can prevent the restacking of GO nanosheets during the reduction process. Also, for photocatalysis, the aforementioned conjugated network can provide rapid electronic conducting channels. It was found that the Pd-rGO/CNT/CaFe2O4 nanocomposite is an efficient photocatalyst for the Heck-Mizoroki coupling reaction under irradiation of visible light. Interestingly, the electrons which are excited by the photons can be transferred to the palladium nanoparticles... 

Reaction of 2-pyridinecarboxaldehyde with L-Alaninol (as a chiral amine) or 2-amino-2-methyl-1-propanol (AMP) in the presence of PdCl2 produced the new and attractive palladium(II) complexes which were synthesized by in situ method. The presence of an extra methyl group in AMP other than L-Alaninol induced the different chelating mode and, therefore, several structurally different palladium complexes obtained. Correspondingly, the chiral amine with PdCl2 produced the imine product, (Iminol (1)), and an oxazolidine compound (Imizol (1′)) as minor product. Also, the use of AMP in formation of palladium complexes led to the synthesis of imine (Ampynol (2)) and oxazolidine (Ampyzol (3))... 

Palladium nanoparticles immobilized on the magnetic nanoparticles@2-amino-N-(2-aminoethyl) benzamide (MNPs@A-N-AEB.Pd0) have been presented as an efficient, and reusable magnetically heterogeneous catalyst for the C-O coupling reaction, namely Ullmann condensation reactions in an aqueous medium. This heterogeneous catalyst shows superior reactivity for the C-O arylation of different aryl halide (chloride, bromide, and iodide) with phenol derivatives to afford the desired products in good to excellent yields within short reaction time. Moreover, the catalyst can be easily recovered and reused for seven runs without loss of catalytic activity. The catalyst was characterized by several... 

For the first time the new 32-membered macrocyclic dinuclear palladium complex of two aza-crown macrocycles, bearing two pyridine arms, Pd2L2Cl4 was synthesized and characterized by elemental analysis, IR, NMR spectroscopy and single crystal X-ray diffraction methods. Pd2L2Cl4 was investigated as a moisture/air-stable catalyst for Sonogashira cross-coupling reaction in the absence of copper and phosphine ligand in DMSO. Thermal stability, possible occurrence of tandem reactions, promoted catalytic performance as well as synergistic effects are of advantageous features of Pd2L2Cl4. By employing Taguchi method, optimum conditions (110 °C, 6 h, KOAc, 2 mol% cat.) were determined. Moreover, the... 

In this work, a new catalyst based on palladium nanoparticle supported SBA-15 has been introduced. The designed catalyst was characterized by Scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectroscopy (FT-IR), Brunauer–Emmett–Teller (BET) surface area analysis, thermo gravimetric analysis (TGA), Energy-dispersive X-ray spectroscopy (EDS) and atomic absorption spectroscopy (AAS) analyses. For the first time, phenyltetrazole has been used as a ligand to the functionalization of SBA-15 to design robust heterogeneous catalyst with high-loading metal for reduction and oxidation in short time using a low amount of the catalyst. © 2018... 

The present study reports a simple electrochemical approach to the fabrication of a new nanocomposite containing PtPd nanoflowers (NFs) promoted with two-dimensional (2D) nanosheets (NSs) structure cuprous oxide (Cu2O) supported on reduced graphene oxide (rGO) (PtPd-NFs/Cu2O-NSs/rGO). Scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectra, Raman spectroscopy, and energy dispersive X-ray spectroscopy are used for characterization of the PtPd-NPs/Cu2O-NPs/rGO. SEM images showed that vertical-standing arrays of Cu2O with an edge length up to 1 μm and thickness of about 20 nm are electrodeposited on the surface of rGO film. Also, PtPd needle-like NFs with visible and... 

The demonstration of high entropy alloys (HEAs), or more generally multi-principal-element alloys (MPEAs), which display a greater resistance to softening at elevated temperatures and embrittlement at cryogenic temperatures, has offered an accessible alternative alloying process for materials scientists and engineers. Although solidification is a fundamental process in synthesis of alloys which strongly affects their microstructure and properties, a firm understanding of this process in HEAs is scarce. Here, using molecular dynamics (MD) simulations, we study the rapid solidification of the multi-principal-element CoFeNiPd alloy as a prototypical single-phase HEA. Our simulations reveal an... 

Palladium(II) have been immobilized into the nano magnetic Fe3O4 which was functionalized with glucose in order to achieve a one-pot synthesis of 2-substituted benzoxazole derivatives with high yields in the diverse range of organic solvents. The nano catalyst is highly dispersive in polar solvents and can be easily recovered and reused for 6 runs without significant loss of its activity. Finally, the catalyst was fully characterized by FT-IR, TGA, CHN, SEM, EDX and atomic absorption spectroscopy. Copyright © 2018 John Wiley & Sons, Ltd  

The first example of a heterogeneous catalytically active system for Buchwald–Hartwig and Ullmann homocoupling of unactivated aryl halides (fluorobenzene) is presented. The novel magnetic heterogeneous palladium catalyst was synthesized by immobilization of palladium ions onto an aminopyridine-functionalized Fe3O4. The catalyst was fully characterized by FTIR spectroscopy, temperature-programmed reduction, thermogravimetric analysis, CHN elemental analysis, transmission electron microscopy, field-emission scanning electron microscopy, X-ray diffraction, energy-dispersive X-ray spectroscopy, and atomic absorption spectroscopy. By using this catalyst system, various types of primary and... 

Aryl halides and especially inactive aryl chlorides were coupled to benzenoid aromatic rings in a Suzuki–Miyaura coupling reaction in the absence of organic solvents and toxic phosphine ligands. The reaction was catalysed by a recoverable magnetic nanocatalyst, Pd@Fe3O4, in aqueous media. This method is green, and the catalyst is easily removed from the reaction media using an external magnetic field and can be re-used at least 10 times without any considerable loss in its activity. The catalyst was characterized using scanning and transmission electron microscopies, thermogravimetric analysis, inductively coupled plasma spectroscopy, Fourier transform infrared spectroscopy, CHN analysis,... 

Supportless Ni-Pd-0.1CNT foamy nanocatalyst with specific surface area of 611.3 m2/g was produced by electroless deposition of nickel, palladium and multiwall carbon nanotube (MWCNT) on interim polyurethane substrate. Application of temperature programmed reduction (TPR) and temperature programmed oxidation (TPO) data into Kissinger (Redhead) kinetic model showed lessening of their activation energies due to Pd and CNT addition. Presence of foamy Ni/SiC caused 8% higher steam reforming of methane; while Ni-Pd-0.1CNT presence resulted in 22% higher methane conversion. The catalytic behavior of the samples was described by morphological and compositional studies which were carried out by... 

The use of 1,3-bis(N-heterocyclic)carbene ligands with different alkyl wingtip groups (alkyl = methyl, isopropyl and tert-butyl) is an effective method for the palladium-catalysed direct S-arylation of methylphenyl sulfoxide and C–C coupling of various of aryl halides with alkenes. The reactions proceed in moderate to good yields. Interestingly, it is shown experimentally that, by using bulkier bidentate N-heterocyclic carbene ligands, more selective catalytic systems towards cis products in Heck coupling reactions can be achieved. Copyright © 2016 John Wiley & Sons, Ltd  

Palladium nanoparticles (Pd-NPs) were supported on functional and nonfunctional Co-coordination polymers (Pd/CoBDCNH2 and Pd/CoBDC). Advanced analytical techniques revealed that Pd-NPs are supported on the external surface of the polymer framework and the functionalized framework possesses effective influence to prevent Pd-NP aggregation. Supported Pd-NPs were effectively applied as heterogeneous recyclable catalysts in the Mizoroki–Heck C–C cross coupling reactions of iodobenzene and either aromatic or aliphatic terminal alkenes. Catalytic results exhibited that highly dispersed Pd-NPs with low loading (1%) on the functional polymer (Pd/CoBDCNH2) are more effective than aggregated Pd-NPs...