Sharif Digital Repository

The present work describes the application of nano CoCuFe2O4 toward the coupling reaction of acyl chlorides with terminal alkynes. By this catalytic system, ynone derivatives were formed in high yields via a palladium-free strategy. This protocol avoids the use of phosphine ligands as well as toxic CO sources. Recovery of catalyst by employing an external magnetic field and its reuse up to 9 consecutive trials confirm the robustness of this catalytic system. © 2017 Elsevier B.V  

The synthesis and catalytic behavior of palladium loaded magnetic nanocomposite based on natural polysaccharide salep modified with poly (amino pyridine) is described. The synthesized support is loaded with relatively large amounts of palladium ions (0.34mmol g−1). This is a simple, ecologically safe and cost-effective route for the preparation of the novel heterogeneous catalyst that shows high activity for Suzuki coupling reactions under remarkably mild conditions. Furthermore, the prepared catalyst is magnetically recovered and effectively reused for seven cycles of reactions without significant loss of its catalytic activity and loaded palladium nanoparticles. © 2017  

Two mononuclear coordination complexes of fullerene[60] with Pd(dba)2 (dba = dibenzylideneacetone), [(η2-C60)Pd(Ph2P(CH2)2PPh2C(H)C(O)R)2] (R = C10H7 (1), C6H4Cl (2)), have been prepared using a simple procedure to explore new directions in palladium catalysis and nanocarbon chemistry. The palladium(0)-[60]fullerene complexes incorporating unsymmetrical phosphorus ylides have been characterized by 1H, 13C and 31P NMR spectroscopic methods and other conventional techniques such as IR, TGA, SEM, ICP-OES, EDX and TEM analysis. Attributed to the enhanced dispersity and uniform size of the Pd nanoparticles with phosphine-functionalized fullerenes, the prepared catalysts exhibited comparable... 

This paper reports a simple, low-cost, and effective electrochemical technique for sensing and reducing CrVI based on a Au-Pd bimetallic nanoparticle (BNP)-decorated indium tin oxide (ITO) conducting glass electrode. It was observed that the Au-Pd BNP-decorated ITO electrode could significantly boost the electrochemical reduction of CrVI when compared with either Au nanoparticle- or Pd nanoparticle-decorated ITO electrodes. These BNP-decorated electrodes exhibited a wide linear concentration range of 0.001-100 μM, a very low detection limit (signal-to-noise ratio = 3) of 0.3 nM, and a high sensitivity of 1.701 μA μM-1. From electrochemical impedance spectroscopy, it was revealed that this... 

A multi-layered catalyst based on poly(imidazole/imidazolium) and graphene oxide, with high loading capacity for immobilization of palladium nanoparticles was prepared. The catalyst was proven to be highly efficient for reduction of nitroarenes and also for Heck reaction with the use of only 0.1 mol% of the catalyst. The reduction of nitroarenes and Heck reaction were performed in water medium and excellent yields of products were achieved. The synthesized catalyst was readily recovered and reused for up to 10 subsequent runs without significant loss of activity  

Liquid phase hydro-purification of crude terephthalic acid (CTA) was performed using supported Pd and Pd-Sn catalysts on functionalized multi-wall carbon nanotubes (FMWCNT). Pd/FMWCNT catalysts were prepared by wet impregnation with Pd loadings of 0.05 to 0.6 wt.%. Pd-Sn/FMWCNT catalysts were prepared by co-impregnation (CI) and successive impregnation (SI) using 0.3 wt.% Pd loading and Sn/Pd molar ratios of 0.1 and 0.35 for the CI method and 0.05 to 0.35 for the SI method. Pd loading of 0.3 wt.% for Pd/FMWCNT was sufficient to decrease the 4-carboxybenzaldehyde (4-CBA) content of CTA from 2100 ppm to 5.5 ppm without excessive hydrogenation of terephthalic acid (TA). The commercial catalyst... 

This study describes an efficient method for ortho-selective halogenation of N-arylcarbamates under mild conditions for the first time. Although being weakly coordinating, N-arylcarbamates act very well as a removable directing group for activation of C-H bonds. The developed procedure results in extremely valuable halogenated N-arylcarbmates that can further be hydrolyzed to halogenated anilines. The obtained reaction conditions showed broad scope and wide functional group tolerance. All the products were formed in good yields with extremely high selectivity  

In the present work, a simple, green, rapid, and catalyst-free procedure for the synthesis of benzamide derivatives by ring opening of azlactones with diamines such as ethylene diamine and 1,3-propylenediamine is described. The present method offers several advantages such as short reaction times, easy work-up, and mild reaction conditions in the absence of catalyst and any toxic solvent and material. In addition, the structure obtained by X-ray crystallography was compared with the theoretical results obtained by density functional theory using the B3LYP functional and cc-pVDZ basis sets  

Palladium catalysts supported on functionalized multi-wall carbon nanotubes were synthesized for hydro-purification of crude terephthalic acid containing 2100ppm 4-carboxybenzaldehyde (4-CBA) as impurity. PdCl2 and Pd(OAc)2 were used as precursors. Palladium loadings were 0.05 to 0.6wt.% with catalysts reduced at 200 to 400°C. Catalysts prepared from both precursors with least 0.3wt.% palladium resulted in 99%+ removal of 4-CBA. The most desired selectivity was obtained for the catalyst with PdCl2 as precursor, reduction temperature of 300°C, and palladium loading of 0.3wt.%. This catalyst had slightly better performance than the commercial catalyst (0.5wt.%... 

Gold nanoparticles (Au NPs) were synthesized by co-deposition of RF-sputtering and RF-PECVD from acetylene gas and Au target on the carbon nanotubes (CNTs). The CNTs were prepared by thermal chemical vapor deposition (TCVD) and Pd nanoparticles catalyst. TEM image shows that high-density and uniform distribution of Au NPs were grown on the CNTs. XRD analysis indicates that Au NPs have fcc crystal structure and CNTs have a good graphite structure. Raman spectroscopy results suggest that our sample includes double-walled CNTs. It is resulted that intensity of D-band reduces and G-band intensity raises and radial breathing mode (RBM) is changed by immobilizing of Au NPs on the CNTs. Raman... 

We use field emission scanning electron microscope (FE-SEM) to investigate the growth of palladium colloids over the surface of thin films of WO3/glass. The film is prepared by Pulsed Laser Deposition (PLD) at different temperatures. A PdCl2 (aq) droplet is injected on the surface and in the presence of steam hydrogen the droplet is dried through a reduction reaction process. Two distinct aggregation regimes of palladium colloids are observed over the substrates. We argue that the change in aggregation dynamics emerges when the measured water drop Contact Angel (CA) for the WO3/glass thin films passes a certain threshold value, namely CA ≈ 46°, where a... 

Two nanocatalysts of palladium over multi-walled carbon nanotubes (MWCNT) were synthesized and their catalytic properties evaluated in selective hydrogenation of acetylene. Different procedures were applied to synthesize catalysts which resulted in two distinct average particle sizes of palladium (Pd) over the MWCNT. The resulting catalysts displayed dissimilar NH3-TPD behaviors as well as different selectivity performances at lower temperatures. While enhancement of the hydrogen transfer mechanism occurred upon the temperature increase, similar behaviors for the aforementioned materials were obtained. Furthermore, it was revealed that the catalytic performance at higher temperatures did not... 

An efficient heterogeneous palladium catalyst system has been developed based on immobilization of Pd nanoparticles on silica-bonded N-propylpiperazine sodium N-propionate (SBPPSP) substrate. SBPPSP substrate can stabilize the Pd nanoparticles effectively so that it can improve their stability against aggregation. In addition, grafted piperazine species on to the silica backbone prevent the removing of Pd nanoparticles from the substrate surface. Transmission electron microscopy (TEM) of catalyst is shown the size of Pd nanoparticles, also it confirmed by particle size analyzer which shown the average size of 21 nm for Pd. The catalytic activity of these catalysts was investigated in the... 

Pd doped WO3 fibers were synthesized by electro-spinning. The sol gel method was employed to prepare peroxopolytungstic acid (P-PTA). Palladium chloride and Polyvinyl pyrrolidone (PVP) was dissolved in the sol Pd:WO3 = 10% molar ratio. The prepared sol was loaded into a syringe connected to a high voltage of 18.3 kV and electrospun fibers were collected on the alumina substrates. Scanning electron microscope (SEM), X-ray powder diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) techniques were used to analyze the crystal structure and chemical composition of the fibers after heat treatment at 500 °C. Resistance-sensing measurements exhibited a sensitivity of about 30 at 500 ppm... 

An efficient heterogeneous palladium catalyst system has been developed based on immobilization of Pd nanoparticles on silica-bonded N-propylpiperazine (SBNPP) substrate. SBNPP substrate can stabilize the Pd nanoparticles effectively so that it can improve their stability against aggregation. Also, grafted piperazine species onto the silica backbone prevents the removing of Pd nanoparticles from the substrate surface. It seems that the high recyclable capability of Pd-SBNPP catalysts is resulted from these two characteristics. Transmission electron microscopy (TEM) of catalyst is shown the size of Pd nanoparticles in Pd-SBNPP average of 20 nm. Furthermore, X-ray photoelectron spectroscopy... 

In this study, tungsten oxide films were deposited by pulsed-laser deposition (PLD) technique. The as-deposited films were annealed at 250 °C in air for 1 h. The surface morphology, microstructure, crystalline phase, and chemical composition of the films were characterized by SEM, XRD and XPS techniques. Pt nanoparticles were deposited onto the tungsten oxide films through a two-step process. First of all, a layer of PtCl2 was coated on the WO3 surface by drop-drying the PtCl2 solution onto the WO3 surface at 60 °C. Consequently, the reduction of the PtCl2 into the metallic Pt nanoparticles was performed at 200 °C. In this study, the effect of the temperature during hydrogen reduction of... 

PANI/Pd/TiO2NTs electrodes with highly porous structures and good capacitive characteristics were prepared by electrodeposition of polyaniline on palladium nanoparticles loaded TiO2 nanotubes. The loading of small palladium nanoparticles was carried out by sonochemical reduction of Pd+2 onto TiO2NTs and affected the ordered growth of PANI, reducing the charge transfer resistance and increasing surface area of PANI. The specific capacitance and the stability of electrode showed improvements. The results illustrated that the specific capacitance of these electrodes was around 1060 F g-1 in 1.0 M H2SO4 electrolyte as measured at a constant current of 2.0 A g-1, whereas it was 210 F g-1 for the... 

The 2,6-bis(diphenylphosphino)pyridine/palladium catalytic system successfully catalyzes the Heck coupling reaction of less reactive aryl chlorides as well as aryl bromides with styrene to give the corresponding olefins in reasonable yields. TBAB (tetrabutylammoniumbromide) as an additive was found to be essential for these reactions. The results of Heck reaction exhibited a high selectivity (>99/1) favoring the trans product  

Conditions for an efficient ligand-free Heck C-C coupling reaction of aryl iodides and bromides with terminal olefins under aerobic conditions have been developed. Critical to the success of this new protocol is the use of palladium acetate as an extremely active catalyst for the Heck reaction in water and aqueous media. Both the base and the solvent were found to have a fundamental influence on the efficiency of the reaction, with K2CO3 and a mixture of (2:1) H2O/DMSO being the optimal base and solvent, respectively  

Reduced graphene oxide (RGO) was used to improve the hydrogen sensing properties of Pd and Pt-decorated TiO2 nanoparticles by facile production routes. The TiO2 nanoparticles were synthesized by sol-gel method and coupled on GO sheets via a photoreduction process. The Pd or Pt nanoparticles were decorated on the TiO2/RGO hybrid structures by chemical reduction. X-ray photoelectron spectroscopy demonstrated that GO reduction is done by the TiO2 nanoparticles and Ti-C bonds are formed between the TiO2 and the RGO sheets as well. Gas sensing was studied with different concentrations of hydrogen ranging from 100 to 10,000 ppm at various temperatures. High sensitivity (92%) and fast response time...