scholarly journals Synthesis of MCM-41 Immobilized (Phenoxy)Imine Palladium(II) Complexes as Recyclable Catalysts in the Methoxycarbonylation of 1-Hexene

Catalysts ◽  
2019 ◽  
Vol 9 (2) ◽  
pp. 143 ◽  
Author(s):  
Saphan Akiri ◽  
Stephen Ojwach

The immobilization of 2-phenyl-2-((3(tryethoxysicyl)propyl)imino)ethanol (HL1) and 4-methyl-2-(((3(triethoxysilyl)propyl)imino)methyl)phenol (HL2) on MCM-41 afforded the respective ligands HL1-MCM-41 (HL3) and HL2-MCM-41 (HL4). The treatment of complexes Pd(L1)2 and Pd(L2)2 with MCM-41 afforded the immobilized complexes (Pd(L1)2)-MCM-41 (1) and (Pd(L2)2)-MCM-41 (2) respectively. Separately, the reactions of HL3 and HL4 with Pd(NCMe)2Cl2 produced the immobilized complexes Pd(HL3)Cl2 (3) and Pd(HL4)Cl2 (4) respectively. The immobilized compounds were characterized by FT-IR, Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), energy-dispersive X-ray (EDX), Thermogravimetric Analysis (TGA) and X-ray Powder Diffraction (XRD). All the complexes (1–4) formed active catalysts in the methoxycarbonylation of 1-hexene to give linear and branched esters. The catalysts were recycled four times without the loss of catalytic activity. Hot filtration experiments established the absence of leaching, and the heterogeneous nature of the active species was derived from mercury drop experiments.

Crystals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 456
Author(s):  
Fahad A. Alharthi ◽  
Hamdah S. Alanazi ◽  
Amjad Abdullah Alsyahi ◽  
Naushad Ahmad

This study demonstrated the hydrothermal synthesis of bimetallic nickel-cobalt tungstate nanostructures, Ni-CoWO4 (NCW-NPs), and their phase structure, morphology, porosity, and optical properties were examined using X-ray Diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), Scanning electron microscopy- energy dispersive X-ray spectroscopy (SEM-EDS), high resolution Transmission electron microscopy (HR-TEM), Brunauer-Emmett-Teller (BET) and Raman instruments. It was found that as-calcined NCW-NPs have a monoclinic phase with crystal size ~50–60 nm and is mesoporous. It possessed smooth, spherical, and cubic shape microstructures with defined fringe distance (~0.342 nm). The photocatalytic degradation of methylene blue (MB) and rose bengal (RB) dye in the presence of NCW-NPs was evaluated, and about 49.85% of MB in 150 min and 92.28% of RB in 90 min degraded under visible light. In addition, based on the scavenger’s study, the mechanism for photocatalytic reactions is proposed.


2017 ◽  
Vol 50 ◽  
pp. 18-31 ◽  
Author(s):  
Rudzani Sigwadi ◽  
Simon Dhlamini ◽  
Touhami Mokrani ◽  
Patrick Nonjola

The paper presents the synthesis and investigation of zirconium oxide (ZrO2) nanoparticles that were synthesised by precipitation method with the effects of the temperatures of reaction on the particles size, morphology, crystallite sizes and stability at high temperature. The reaction temperature effect on the particle size, morphology, crystallite sizes and stabilized a higher temperature (tetragonal and cubic) phases was studied. Thermal decomposition, band structure and functional groups were analyzed by Brunauer-Emmett-Teller (BET), Scanning Electron Microscopy (SEM), Transmission electron microscopy (TEM), X-ray diffraction (XRD), Thermo-gravimetric analysis (TGA) and Fourier transform infrared (FT-IR). The crystal structure was determined using X-ray diffraction. The morphology and the particle size were studied using (SEM) and (TEM). The shaped particles were confirmed through the SEM analysis. The transmission electron microscopic analysis confirmed the formation of the nanoparticles with the particle size. The FT-IR spectra showed the strong presence of ZrO2 nanoparticles.


2021 ◽  
Vol 66 ◽  
pp. 61-71
Author(s):  
Tahereh Heidarzadeh ◽  
Navabeh Nami ◽  
Daryoush Zareyee

The principal aim of this research is using biosynthesized ZnO-CaO nanoparticles (NPs) for preparation of indole derivatives. ZnO-CaO NPs have been prepared using Zn(CH3COO)2 and eggshell waste powder in solvent-free conditions. Morphology and structure of NPs were determined by FT-IR, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy dispersive spectra (EDS). It was used as a highly efficient catalyst for the synthesis of indole derivatives. Some indole derivatives were synthesized by the reaction of indole, formaldehyde, aromatic and aliphatic amines in the presence of ZnO-CaO NPs (5 mol%) in ethanol under reflux conditions. The assigned structure was further established by CHN analyses, NMR, and FT-IR spectra. Because of excellent capacity, the exceedingly simple workup and good yield, eco-friendly catalyst ZnO-CaO NPs were proved to be a good catalyst for this reaction.


Polymers ◽  
2019 ◽  
Vol 11 (9) ◽  
pp. 1417 ◽  
Author(s):  
Wang ◽  
Xiao ◽  
Huang ◽  
Zheng ◽  
Luo ◽  
...  

Chitosan microspheres modified by 2-pyridinecarboxaldehyde were prepared and used in the construction of a heterogeneous catalyst loaded with nano-Cu prepared by a reduction reaction. The chemical structure of the catalyst was investigated by Fourier Transform Infrared Spectroscopy (FT-IR), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and X-ray Photoelectron Spectroscopy (XPS). Under mild conditions, such as no ligand at room temperature, the catalyst was successfully applied to catalyze the borylation of α,β-unsaturated receptors in a water-methanol medium, yielding 17%–100% of the corresponding -hydroxy product. Even after repeated use five times, the catalyst still exhibited excellent catalytic activity.


2011 ◽  
Vol 239-242 ◽  
pp. 2839-2842
Author(s):  
Hong Mei Mu ◽  
Peng Fei ◽  
Bi Tao Su ◽  
Zi Qiang Lei

A series of Fe3+-dopped polyaniline (Fe3+/PANI) nanomaterials with different morphologies and a higher conductivity were successfully synthesized using a simple and static interfacial polymerization by using FeCl3 as both oxidant catalyst and dopant. The effect of surfactants CTAB and SDS and the concentration of FeCl3 on the morphology and conductivity of Fe3+/PANI nanomaterial were investigated. The samples were characterized by Transmission Electron Microscopy (TEM), SDY-4 probes conductivity meter, X-ray Diffractometry (XRD), Energy dispersive spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy techniques. TEM’s results showed that their morphologies changed with the type of the surfactant and the concentration of FeCl3. Introducing surfactants CTAB and SDS into Fe3+/PANI remarkably improved the conductivity of the material. The conductivities of CTAB/Fe3+/PANI and SDS /Fe3+/PANI nanomaterials were respectively about 4.8×10-2 and 1.3×10-2 S/cm while the conductivity of Fe3+/PANI was found to be 1.5×10-4 S/cm. The different morphology and high conductivity may be ascribed to the mutual effects of the surfactant and oxidant.


2019 ◽  
Vol 11 (11) ◽  
pp. 1064-1070 ◽  
Author(s):  
Nkosinathi G. Dlamini ◽  
Albertus K. Basson ◽  
V. S. R. Rajasekhar Pullabhotla

Bioflocculant from Alcaligenis faecalis HCB2 was used in the eco-friendly synthesis of the copper nanoparticles. Nanoparticles were characterized using a scanning electron microscope (SEM), transmission electron microscopy (TEM), UV-visible spectroscopy, thermo gravimetric analysis (TGA) and Fourier Transform Infrared Spectroscopy (FT-IR). The transmission electron microscopy images showed close to spherical shapes with an average particle size of ∼53 nm. Energy-dispersive X-ray spectroscopy analysis confirmed the presence of the Cu nanopartilces and also the other elements such as O, C, P, Ca, Cl, Na, K, Mg, and S originated from the bioflocculant. FT-IR results showed the presence of the –OH and –NH2 groups, aliphatic bonds, amide and Cu–O bonds. Powder X-ray diffraction peaks confirmed the presence of (111) and (220) planes of fcc structure at 2 of 33° and 47° respectively with no other impurity peaks.


2013 ◽  
Vol 32 (2) ◽  
pp. 157-162 ◽  
Author(s):  
Mahdiyeh Esmaeili-Zare ◽  
Masoud Salavati-Niasari ◽  
Davood Ghanbari

AbstractMercury selenide nanostructures were synthesized from the reaction of N, N′-bis(salicylidene)propane-1,3-diamine mercury complex, (Hg(Salpn)) as a novel precursor, via sonochemical method. The effect of different surfactant on the morphology and particle size of the products was investigated. Products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy and X-ray energy dispersive spectroscopy (EDS).


2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Chaturbhuj K. Saurabh ◽  
Asniza Mustapha ◽  
M. Mohd. Masri ◽  
A. F. Owolabi ◽  
M. I. Syakir ◽  
...  

Cellulose nanofibers (CNF) were isolated fromGigantochloa scortechiniibamboo fibers using sulphuric acid hydrolysis. This method was compared with pulping and bleaching process for bamboo fiber. Scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and thermogravimetric analysis were used to determine the properties of CNF. Structural analysis by FT-IR showed that lignin and hemicelluloses were effectively removed from pulp, bleached fibers, and CNF. It was found that CNF exhibited uniform and smooth morphological structures, with fiber diameter ranges from 5 to 10 nm. The percentage of crystallinity was significantly increased from raw fibers to cellulose nanofibers, microfibrillated, along with significant improvement in thermal stability. Further, obtained CNF were used as reinforcement material in epoxy based nanocomposites where tensile strength, flexural strength, and modulus of nanocomposites improved with the addition of CNF loading concentration ranges from 0 to 0.7%.


2013 ◽  
Vol 678 ◽  
pp. 248-252
Author(s):  
K. Kavi Rasu ◽  
Dhandapani Vishnushankar ◽  
V. Veeravazhuthi

Bismuth sulfide (Bi2S3) and Polyvinyl pyrrolidone (PVP) encapsulated Bi2S3 Nanoparticles are synthesized from aqueous solutions at room temperature. Synthesized samples are subjected to UV-Visible Spectroscopy, X-Ray Diffraction (XRD), Scanning electron microscopy (SEM), Energy Dispersive Analysis of X-ray (EDAX), Transmission Electron Microscopy (TEM) and FT-IR studies and their results are compared. X-ray diffraction spectrum reveals the crystalline nature of the synthesized samples. Grain size value of PVP/ Bi2S3 nanoparticles show a decrease when compared to Bi2S3 nanoparticles and this ensures the good encapsulant effect of PVP on Bi2S3 nanoparticles. SEM images show that all the particles in the synthesized sample are nearly equal in size. From the TEM image we conclude that the particle size lies between 30nm to 70nm. Finally the samples are subjected to EDAX studies for determining their composition.


2011 ◽  
Vol 175-176 ◽  
pp. 341-344 ◽  
Author(s):  
Byoung Suhk Kim ◽  
Kyu Oh Kim ◽  
Ick Soo Kim

We report the electrospun poly(L-lactide) (PLA) nanofibers incorporating polyhedral oligosilsesquioxane (POSS)-modified multiwalled carbon nanotubes (MWNTs). FT-IR, transmission electron microscopy (TEM) and Raman analysis confirmed the existence of POSS macromers bonded to the MWNTs as an extra phase. The thermal and microstructure properties of the PLA hybrid nanofibers with POSS-modified MWNTs were investigated by thermogravimetric analysis (TGA) and Wide-angle X-ray diffraction (WAXD).


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