A novel method for <Emphasis Type=Italic>N</Emphasis>-alkylation of aliphatic amines with ethers over γ-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>

A novel and simple method for the N-alkylation of amines with different ethers as alkylating reagents has been developed, using cheap γ-Al₂O₃ as the catalyst at atmospheric pressure in the temperature range of 260–320°C. For example, the reaction of equimolar amounts of morpholine and diethyl ether gave N-ethylmorpholine quantitatively. The present catalytic system is applicable to the N-alkylation of both primary and secondary amines. Since only water is generated as byproduct, the protocol proved to be eco-friendly and atom-economic.     

Characterization of double oxide system Cu-Cr-O supported on <Emphasis Type="Italic">γ</Emphasis>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>

Series of alumina supported chromium-copper catalysts were prepared by co-impregnation method. The samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy and UV-visible diffuse reflectance spectroscopy. Dispersion and porosity was also obtained. The experimental and catalytic test results have drawn a conclusion that an interaction between copper and chromium ions takes place. This interaction is responsible for the enhanced catalytic activity of studied catalysts in reaction of total oxidation of industrial formaldehyde production exhaust gas, which contains CO, dimethyl ether and methanol as main components. The article is published in the original.     

Thermal behavior of LaPO<Subscript>4</Subscript>·<Emphasis Type=Italic>n</Emphasis>H<Subscript>2</Subscript>O and NdPO<Subscript>4</Subscript>·<Emphasis Type=Italic>n</Emphasis>H<Subscript>2</Subscript>O nanopowders

Thermal behavior of LaPO₄·nH₂O and NdPO₄·nH₂O nanopowders from room temperature to 973 K was investigated by DSC, TA/DTG, ESM, and X-ray study. Mass loss due to the release of adsorbed and hydrate water was found in the range from 323 to 623 K. Phase transitions from hexagonal structure nanopowders to monoclinic one for bulk specimens were found above 873 K.     

X-ray,SEM, and DSC studies of ferroelectric Pb<Subscript>1−<Emphasis Type=Italic>X</Emphasis></Subscript>Ba<Subscript><Emphasis Type=Italic>X</Emphasis></Subscript>TiO<Subscript>3</Subscript> ceramics

The polycrystalline ferroelectric compounds of general formula Pb_1−X Ba _X TiO₃ with X = 0.00, 0.1, 0.2 and 0.5 were prepared by high temperature solid-state reaction technique using high purity oxides and carbonates. The compounds formation was confirmed by X-ray diffraction and all the X-ray peaks were indexed with tetragonal structure of space group P4mm. Morphology and particle size of the compounds were obtained using scanning electron microscopy. Ferroelectric phase transition, enthalpy change, and specific heat of the compounds were obtained using modulated differential scanning calorimetry. It was observed that the phase transition temperature decreased linearly with the increase of substitution concentration.     

Magnetic and thermal analysis of <Emphasis Type=Italic>M</Emphasis>Fe<Subscript>2</Subscript>O<Subscript>4</Subscript> (<Emphasis Type=Italic>M</Emphasis> = Co,Mn, Zn) nanoparticles

Magnetic nanoparticles were prepared by a wet chemical method. Precursors of MFe₂O₄ (M = Co, Mn, Zn) were prepared from a mixture of metal chloride and metasilicate nonahydrate aqueous solutions. The precipitates obtained in the wet chemical method were calcined to obtain MFe₂O₄ nanoparticles encapsulated by amorphous SiO₂. The blocking temperatures T _B’s were between 20 and 320 K, in this temperature range, the anisotropy energy of the particles decreased below their thermal energy. T _B increased with the particle size. In order to clarify the nanoparticle formation process, differential thermal analysis and thermogravimetric (TG-DTA) measurements were performed for the as-prepared samples.     

<Emphasis Type="Italic">N</Emphasis>-alkylation of ethylenediamine with alcohols catalyzed by CuO-NiO/<Emphasis Type="Italic">γ</Emphasis>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>

A simple method for N-alkylation of 1,2-diaminoethane with different alcohols in a fixed-bed reactor using cheap CuO-NiO/γ-Al₂O₃ as the catalyst has been developed. The present catalytic system was applicable in the N-alkylation of 1,2-diaminoethane with both primary and secondary alcohols. Mono-N-alkylation of 1,2-diaminoethane with low-carbon alcohols resulted in high yields; the yields of tetra-N-alkylation of 1,2-diaminoethane with low-carbon alcohols declined markedly with the increase of the molecular volume of alcohols.     

Synthesis and X-ray diffraction of Cd<Subscript><Emphasis Type=Italic>x</Emphasis></Subscript>Hg<Subscript>1 − <Emphasis Type=Italic>x</Emphasis></Subscript> Te solid solutions

The Cd _x Hg_{1 − x} Te solid solutions were synthesized by combining two methods: immersion of CdTe single crystals in liquid mercury and thermal homogenization in mercury vapors. The samples obtained were studied by X-ray diffraction and X-ray fluorescence analyses. Nonstoichiometric cadmium microinclusions were shown to present in the initial CdTe single crystals and the solid solutions synthesized. The samples annealed in mercury vapors have smaller unit cell volumes than unannealed samples.     

Catalytic dehydrogenation of cyclohexene over MoO<Subscript>3</Subscript>/γ-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> catalysts

A series of MoO₃/γ-Al₂O₃ catalysts with different Mo surface densities (Mo atoms/nm²) has been prepared by incipient wetness impregnation method. Structural characteristics of the prepared catalysts were investigated by atomic absorption spectroscopy, X-ray diffraction, Fourier Transform Infrared spectroscopy, N₂ adsorption at −196 °C, and temperature-programmed reduction (TPR). The catalytic activities of the prepared catalysts were tested by cyclohexene conversion between 200 and 400 °C. XRD results indicated that molybdenum oxide species were dispersed as a monolayer on the support up to 4.04 Mo atoms/nm², and the formation of crystalline MoO₃ was observed above this loading. FTIR and TPR results showed that molybdenum oxide species were present predominantly in tetrahedral form at lower loading, and polymeric octahedral forms were dominant at higher loading. Cyclohexene conversion reaction proceeded mainly through the simple dehydrogenation pathway in the studied temperature range 200–400 °C and was found to be highly dependent on MoO₃ dispersion.     

Synthesis and studies of magnesium hexafluorozirconates MgZrF<Subscript>6</Subscript> · <Emphasis Type=Italic>n</Emphasis>H<Subscript>2</Subscript>O (<Emphasis Type=Italic>n</Emphasis> = 5, 2, 0)

Crystalline magnesium hexafluorozirconate MgZrF₆ · 5H₂O isostructural to MnZrF₆ · 5H₂O, and having a chain-like structure, was synthesized and studied. According to thermogravimetry, the compound undergoes stepwise dehydration in the temperature range of 50–420°C to give the stable phase MgZrF₆ · 2H₂O and the final product MgZrF₆ isostructural to the cubic modification of MZrF₆ (M = Cu, Fe). The vibrational spectra of the initial compound and the dehydration products are analyzed and the structures of the compounds are considered.     

Electrophysical properties of layered perovskites LnBaCo<Subscript>2 − <Emphasis Type=Italic>x</Emphasis></Subscript>Cu<Subscript><Emphasis Type=Italic>x</Emphasis></Subscript>O<Subscript>5 + δ</Subscript> (Ln = Sm,Nd) for solid oxide fuel cells

The influence of doping with copper oxide on the phase composition, electric conductivity, and linear thermal expansion coefficient (LTEC) of SmBaCo₂O_{5 + δ} and NdBaCo₂O_{5 + δ} was studied. The sample homogeneity region has been determined with using XRD. The samples conductivity decreased as the dopant concentration increased. The character of the temperature dependence of conductivity changed at high copper contents. In a reductive atmosphere, the conductivity of the samples at first decreased and then remained constant. The linear thermal expansion coefficient decreased as the amount of the incorporated dopant increased.