Recent advances in the synthesis, characterization, and catalytic consequence of metal species confined within zeolite for hydrogen-related reactions

Zeolites-encapsulated metal and metal oxide species are important heterogeneous catalysts.They give performances that steadily outperform traditional supported catalysts in many important reactions and have become a research hotspot.Remarkable achievements have been made with respect to the synthesis,characterization,and performances of metal species(typically metal and metal oxide clusters)confined in zeolites.The development in the strategies for the encapsulation of metal species including posttreatment and in situ synthesis method are introduced and compared.For the characterization of zeoliteencapsulated metal catalysts,the structural and surface properties of metal species are studied by several useful techniques,such as electron microscopy,X-ray absorption(XAS),Fourier transform infrared spectroscopy of CO(FTIR-CO),and chemisorption,which confirm the successful confinement of metal species in zeolites and their unique physiochemical properties.In addition,the encapsulation fraction can be determined by a probe molecular titration reaction.For the catalytic performance of zeoliteencapsulated metal catalysts,the activity,selectivity,and stability are emphasized.Finally,applications of zeolite-encapsulated metal catalysts in hydrogen-related reactions are summarized.

Microstructural characterization and mechanical properties of(TiC+TiB)/TA15 composites prepared by an in-situ synthesis method

Titanium matrix composites reinforced with ceramic particles are considered a promising engineering material due to their combination of high specific strength,low density,and high modulus.In this study,the TA15-based composites reinforced with a volume fraction of 10% to 25%(TiB+TiC)were prepared using powder metallurgy and casting technique.Microstructural characterization and phase constitution were examined using optical microscopy(OM),scanning electron microscopy(SEM),and X-ray diffraction(XRD).In addition,the microhardness,room temperature(RT)and high temperature(HT)tensile properties of the composites were evaluated.Results revealed that the reinforcements are distributed uniformly even in the composites with a high volume of TiB and TiC.However,as the volume fraction exceeds 15%,TiB and TiC particles become coarsening and exhibit rod-like and dendritic-like morphology.Microhardness increases gradually from 321.2 HV for the base alloy to a maximum of 473.3 HV as the reinforcement increases to 25vol.%.Tensile test results indicate that a reinforcement volume fraction above 20% is beneficial for enhancing tensile strength and yield strength at high temperatures,but it has an adverse effect on room temperature elongation.Conversely,if the reinforcement volume fraction is below 20%,it can improve high-temperature elongation when the temperature exceeds 600℃.

Synthesis, Characterization and Optical Morphology of ZnO Nanoparticles

The ZnO molecule plays an important role in the industry due to it special features, anti-corrosion anti-bacterial properties, as well as due to its low electrical conductivity and heat resistance. In these experimental researches, the sol-gel method was chosen, which enables control of nucleation, aging and growth of particles in the solution. ZnO synthesis was prepared utilizing chemical method with Zinc acetate dyhidrate and NaOH with the appropriate methanol solvent and heating (60˚C). The methods used in identification and characterization are FTIR, UV/VIS, OPTICAL MICROSCOPY, SEM and XRD. The FTIR spectra of synthesized ZnO with corresponding ones show characteristic bands at the corresponding wavelengths, which confirm the presence of ZnO nanoparticles. SEM characterization of ZnO shows the morphology of needle-shaped nanoparticles. XRD spectar in this research by chemical method indicates the particle size of 17.76 nm.

Navigating the pathways:TAR-DNA-binding-protein-43 aggregation,axonal transport,and local synthesis in amyotrophic lateral sclerosis pathology

Neurons are highly polarized cells with axons reaching over a meter long in adult humans.To survive and maintain their proper function,neurons depend on specific mechanisms that regulate spatiotemporal signaling and metabolic events,which need to be carried out at the right place,time,and intensity.Such mechanisms include axonal transport,local synthesis,and liquid-liquid phase separations.Alterations and malfunctions in these processes are correlated to neurodegenerative diseases such as amyotrophic lateral sclerosis(ALS).

Hydrothermal synthesis, characterization and optical properties of La_2Sn_2O_7:Eu^(3+) micro-octahedra

Pyrochlore structure La2Sn2O7：Eu3＋ microcrystals with uniform octahedron shape were successfully synthesized via a hydrothermal route at 180 °C for 36 h. The crystal structure, particle size, morphologies, and optical properties of the as-synthesized products were investigated by XRD, TEM, SEM, EDS, FT-IR, Raman spectroscopy and PL. The effects of pH of precursor solution, precursor concentration, reaction temperature, and time were investigated. The results reveal that pH of the precursor solution not only plays an important role in determining the phase of the as-synthesized products, but also has a significant influence on the morphologies of the samples. High-quality and uniform octahedrons with an average size of about 700 nm could be easily obtained at the pH value of 12. The possible formation mechanism of octahedral-like La2Sn2O7：Eu3＋ microcrystals was briefly proposed. The photoluminescence spectra show that La2Sn2O7：Eu3＋ micro-octahedra display stronger emission in the range of 582-592 nm compared with the samples with other shapes.

Synthesis and characterization of arginine-modified and europium-doped hydroxyapatite nanoparticle and its cell viability

The arginine-modified and europium-doped hydroxyapatite nanoparticles（HAP-Eu） were synthesized by hydrothermal synthesis.The prepared nanoparticles were characterized by transmission electron microscopy（TEM）,X-ray diffractometry（XRD）,Fourier transform infrared（FTIR） and zeta potential analyzer.The cell viability of HAP-Eu was tested by image flow cytometry.The results indicated that HAP-Eu is short column shapes and its size is approximately 100 nm,its zeta potential is about 30.10 mV at pH of 7.5,and shows no cytotoxicity in human epithelial cells and endothelial cells.

Synthesis and Characterization of Quaternary Complexes Ln(CH_2ClCOO)_2 (NO_3) (phen)

Many binary lanthanide complexes have been studied. However, few mixed anion complexes with bidentate heterocyclic amines were synthesized. We synthesized mixed anion complexes Ln ( CH2 ClCOO )2 (NO3 ) ( phen) which was determined by elemental analyses . The IR spectra analyses indicate that NO3- , CH2 ClCOO- and phen are coordinated with Ln . The molar conductances of the complexes at 10-3 mol · L-1 were founded to be between 32.4 and 35.8 S·cm2· mol-1 , suggesting the nonelectrolytes in N-Dimethylformamide. And we determined the fluorescent spectra Eu(CH2ClCOO)2(NO3) ( phen ) and ESR spectra of Gd ( CH2 ClCOO )2 ( NO3) ( phen) .

Synthesis and Characterization of Novel N-Ferrocenesulfonyl Benzimidazole

A new series of ferrocenesulfonyl benzimidazle has been synthesized and characterized by 1H NMR, FT-IR and elemental analysis. They are expected to have special bio-activity.

Synthesis,characterization and gas-sensing properties of Pd-doped SnO_2 nano particles

SnO2 nano particles with various Pd-doping concentrations were prepared using a template-free hydrothermal method.The effects of Pd doping on the crystal structure,morphology,microstructure,thermal stability and surface chemistry of these nano particles were characterized by transmission electron microscope,X-ray diffractometer and X-ray photoelectron spectroscope respectively.It was observed that Pd-doping had little effect on the grain sizes of the obtained SnO2 nano particles during the hydrothermal route.During thermal annealing,Pd-doping could restrain the growth of grain sizes below 500℃ while the grain growth was promoted when the temperature increased to above 700℃.XPS results revealed that Pd existed in three chemical states in the as-synthesized sample as Pd^0,Pd^2＋ and Pd^4＋,respectively.Pd^4＋ was the main state which was responsible for improving the gas-sensing property.The optimal Pd-doping concentration for better gas-sensing property and thermal stability was 2.0%-2.5% （mole fraction）.

The Synthesis and Characterization of High Molecular Weight Poly(phenylene sulfide/ether)

Poly（phenylene sulfide/ether） （PPSE） was synthesized from 4,4＇-dihydroxydiphenyl sulfide and 4,4＇-dichlorodiphenyl sulfide in solution by nucleophilic substitution reaction. The resulting polymer was characterized by viscosity measurement, elemental analysis, FT-IR, ^1H NMR, X-ray diffraction and thermal analysis. The results showed that the viscosities of the resulting polymer were above 0.68 dL/g, and the linear chain structure of product was confirmed. PPSE had the same reflex indices as poly（p-phenylene sulfide）, an orthorhombic crystalline with unit cell a=0.853, b=0.562, c=1.026nm. The melting temperature, glass transition temperature and initial decomposition temperature were found to be 228℃, 85℃ and 325℃, respectively. The product was soluble in common organic solvents such as NMP, N, N＇-dimethylformamide, N, N＇-dimethylacetamide and 1,2-dichloroethane.

Synthesis and characterization of ε-VOPO_4 nanosheets for secondary lithium-ion battery cathode

Vanadium （III） phosphate monoclinic VPO4·H2O was synthesized hydrothermally. The ε-VOPO4 nanosheets, formed by the oxidative de-intercalation of protons from monoclinic VPO4·H2O, can reversibly react with more than 1 mol lithium atoms in two steps. Crystal XRD analysis revealed that the structure of the ε-VOPO4 nanosheets is monoclinic with lattice parameters of α=7.2588（4） A, b=6.8633（2） A and c=7.2667（4） A. The results show that the ε-VOPO4 nanosheets have a thickness of 200 nm and uniform crystallinity. Electrochemical characterization of the ε-VOPO4 monoclinic nanosheets reveals that they have good electrochemical properties at high current density, and deliver high initial capacity of 230.3 mA· h/g at a current density of 0.09 mA/cm2. Following the first charge cycle, reversible electrochemical lithium extraction/insertion at current density of 0.6 mA/cm2 affords a capacity retention rate of 73.6% （2.0？4.3 V window） that is stable for at least 1000 cycles.

Characterization and catalytic performance of CeO_2-Co/SiO_2 catalyst for Fischer-Tropsch synthesis using nitrogen-diluted synthesis gas over a laboratory scale fixed-bed reactor

The surface species of CO hydrogenation on CeO2-Co/SiO2 catalyst were investigated using the techniques of temperature programmed reaction and transient response method. The results indicated that the formation of H2O and CO2 was the competitive reaction for the surface oxygen species, CH4 was produced via the hydrogenation of carbon species step by step, and C2 products were formed by the polymerization of surface-active carbon species （-CH2-）. Hydrogen assisted the dissociation of CO. The hydrogenation of surface carbon species was the rate-limiting step in the hydrogenation of CO over CeO2-Co/SiO2 catalyst. The investigation of total pressure, gas hourly space velocity （GHSV）, and product distribution using nitrogen-rich synthesis gas as feedstock over a laboratory scale fixed-bed reactor indicated that total pressure and GHSV had a significant effect on the catalytic performance of CeO2-Co/SiO2 catalyst. The removal of heat and control of the reaction temperature were extremely critical steps, which required lower GHSV and appropriate CO conversion to avoid the deactivation of the catalyst. The feedstock of nitrogen-rich synthesis gas was favorable to increase the conversion of CO, but there was a shift of product distribution toward the light hydrocarbon. The nitrogen-rich synthesis gas was feasible for F-T synthesis for the utilization of remote natural gas.

Hydrothermal in situ Ligand Synthesis from 1,10-Phenanthroline-5,6-dione and Characterization of 1D Coordination Polymers [Co(bpdc)(H_2O)_3]·H_2O and [Cu(bpy)V_2O_6]

Hydrothermal treatment of MCl2 （ M = Co or Cu ） , NH4 VO3, and 1,10-phenanthroline-5,6-dione （pdon） resulted in the formation of a duplex coordination polymer [ Co （ bpdc ） （ H2O ） 3 ] · H2O （ bpdc = 2,2＇-bipyridine-3,3＇-dicarboxylate） and a chain-like coordination polymer [ Cu （bpy） V2O6 ] （ bpy = 2,2＇-bipyridine ）. X-ray single-crystal structural analysis shows that under hydrothermal conditions and in the presence of different transition metals, the organic reagent pdon was transformed in situ into bpdc and bpy, respectively. Mechanism of the in situ ligand synthesis reaction has been discussed.

Preparation and characterization of LaB_6 ultra fine powder by combustion synthesis

High-purity,homogeneous and ultra fine LaB6 powders were prepared by combustion synthesis.The effects of reactant ratio and molding pressure on the phase and morphology of the combustion products were studied.The combustion products and leached products were analyzed by XRD,SEM and EDS.The results indicate that the combustion product consists of LaB6,MgO and a little Mg3B2O6.The combustion product becomes denser and harder when the molding pressure increases.The purity of LaB6 is higher than 99.0%.The LaB6 particle size is in range of 1.92-3.00 μm and the lattice constant of LaB6 is a=0.414 8 nm.

Synthesis and Characterization of Picolinamide Calix[6]arenes Derivatives

Three full-substituted calix[6]arenes containing the picolinamide groups were synmesized and characterized by IR, ^1HNMR and MS, after series reactions, including lower rim etherification, upper rim ipso-nitration, reduction, amidation.

Synthesis and characterization of ZnTiO_3 with high photocatalytic activity

Perovskite ZnTiO3 was prepared through a new method which contained a hydrothermal process for the preparation of titanate nanotubes and an ion-exchange process.The titanate nanotubes were inferred to be H2Ti3O7·3H2O.X-ray diffraction（XRD）result revealed the presence of cubic perovskite phase of ZnTiO3.The unique chain-like morphology of ZnTiO3 was observed by scanning electron microscopy（SEM） and transmission electron microscopy（TEM）.UV-Vis diffusive reflection spectra of ZnTiO3indicated that the absorbance obviously increased in the visible light region.The degradation rate of methyl orange solution（15 mg/L）reached 95.3%over ZnTiO3（0.3 g/L） after 20 min xenon light irradiation,which was higher than that using the commercial catalyst P25 under the same reaction condition.The degradation kinetic results follow the first-order equation and the rate constant is 0.1020.

Synthesis and Characterization of Magnesium Substituted Aluminophosphate Molecular Sieves with AEL Structure

MAPO-11 molecular sieves were synthesized by hydrothermal methods. The influence of precursor of magnesium, Mg/Al ratio, synthesis temperature, synthesis time and the type of template on the formation and properties of MAPO-11 molecular sieves was examined. The samples were characterized by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermogravimetric analysis (TG-DGA), etc. The results show that the shape and size of crystal were influenced by the precursor of Mg, the Mg/Al ratio and the type of template, and the TG-DGA analysis shows that MAPO-11 molecular sieves as-synthesized have poor thermal stability.

Rh_2O_3/mesoporous MO_x-Al_2O_3(M = Mn,Fe,Co,Ni,Cu,Ba)catalysts:Synthesis,characterization,and catalytic applications

Recently,a one-pot self-assembly method was proposed for the synthesis of mesoporous Al2O3 and MOx-Al2O3 composite materials.However,few attempts have been made to use mesoporous MOx-Al2O3 composites to support metal oxides for catalysis.In the present work,mesoporous MOx-Al2O3（M = Mn,Fe,Co,Ni,Cu,Ba）materials were prepared by a one-pot self-assembly method using Pluronic P123 as a structure-directing agent.The obtained mesoporous materials were loaded with Rh2O3 nanoparticles via impregnation with Rh（NO3）3 followed by calcination in air at 500°C.The resulting catalysts were characterized by X-ray diffraction,N2 adsorption-desorption measurements,transmission electron microscopy,inductively coupled plasma optical emission spectrometry,X-ray photoelectron spectroscopy,and their catalytic activity and stability for CO oxidation and N2O decomposition were tested.The Rh2O3 nanoparticles were found to be on the order of1 nm in size and were highly dispersed on the high surface area mesoporous MOx-Al2O3 supports.A number of the Rh2O3/mesoporous MOx-Al2O3 catalysts exhibited higher catalytic activity than the Rh2O3/mesoporous Al2O3 prepared for comparison.

Synthesis and Characterization of Microcapsules with Chlorpyrifos Cores and Polyurea Walls

Microcapsules with chlorpyrifos cores and polyurea walls were synthesized with 2,4-tolylene diisocyanate as an oil-soluble monomer and ethylenediamine as a water-soluble monomer via an interracial polycondensation reaction. The products were characterized by means of Fourier transform infrared spectrometry, ^13C NMR spectrometry and ^31p NMR spectrometry. The morphology, the particle size and the particle size distribution, and the thermal properties were also evaluated. The prepared microcapsules exhibit clear and smooth surfaces and have a mean diameter of 28. 13 μm. These microcapsules also have a good thermal stability for long-term use, and have potential applications in minimizing the toxicity of chlorpyrifos through controlled release.

Synthesis,characterization and catalytic properties of Y-β zeolite composites

Y-β zeolite composites were hydrotherrnally synthesized by using high silica Y zeolite as the precursor and characterized by XRD, N2 adsorption, SEM and IR spectra of pyridine. The result showed that the N2 adsorption-desorption isotherm of the zeolite composites had a distinct hysteresis loop, and the SEM result showed that the zeolite composites had a different morphology from Y, β and the corresponding physical zeolite mixture. The acid catalytic performance of the zeolite composite catalysts was investigated in the hydrocracking and hydroisomerization of n-octane, and the results showed that the composite materials exhibited an excellent hydrocracking activity and good hydroisomerization performance. The yield of i-C4 over the zeolite composite catalyst was 4.45% higher than that on the corresponding zeolite mixture in the n-octane hydrocracking process at 553 K. The isomerization ability of n-octane over the composite catalyst was 3.6 fold that of the corresponding mixture at 503 K.