Synthesis of vanadium-phosphorus oxide catalysts deposited onto silica-carbon supports

Effect of conditions of hydrothermal and microwave synthesis of supported vanadium-phosphorus oxide catalysts in an aqueous medium on the physicochemical properties of the vanadyl hydrophosphate obtained was studied. The transformations occurring in the system were examined using X-ray phase and differential-thermal analyses, adsorption-structural method, and scanning electron microscopy.     

Structural and Adsorptive Characteristics of Pyrocarbon/Silica Gel Si-60

Pyrocarbon/silica gel adsorbents (carbosils, CS) with mesoporous Si-60 (Merck, granule size 0.2–0.5 mm) modified by pyrolysis of CH₂Cl₂ at 823 K and reaction time from 0.5 to 6 h and then hydrothermally treated at 473 K for 6 h were studied by means of TEM, adsorption and ¹H NMR methods. Changes in the structural and adsorptive characteristics of hybrid adsorbents before and after hydrothermal treatment, which depend on pyrocarbon content (C _C), were analyzed on the basis of TEM micrographs and p-nitrophenol and nitrogen adsorption isotherms treated using a constrained regularization method. Interfacial water layers in aqueous suspension of CS were investigated by means of ¹H NMR with freezing-out of bulk water at T < 273 K showing nonlinear changes in the Gibbs free energy of interfacial water with increasing C _C because of nonlinear dependence of the structural characteristics of pyrocarbon deposits and CS as a whole on C _C.     

Preparation of nano-dispersed lithium niobate by mechanochemical route

Interaction in the system of lithium carbonate–niobium pentoxide during mechanochemical treatment in air and water has been studied. Prepared samples have been investigated with the help of DTA–TG, XRD, FTIR, Raman, and UV–Vis spectroscopy, adsorption–desorption of nitrogen and TEM. Activation of reagents and direct mechanochemical synthesis are observed at 600–850 and 1,000 rpm, respectively. Lithium metaniobate samples prepared via milling possess high dispersity, defective structure, and improved photocatalytic activity, including under visible illumination.     

Solid-state interactions of vanadium and phosphorus oxides in the closed systems

Physicochemical processes during thermal treatment of vanadium and phosphorus oxides mixture (1) as well as with diammonium hydrophosphate (2) in the closed system (autoclave) have been studied. In the first case, at 300 °C, the defective structure γ-VOPO₄ is formed and in the second case, there was established possibility of synthesis of vanadyl hydrophosphate—the precursor of vanadyl pyrophosphate (the catalyst of n-butane oxidation to maleic anhydride). At the same time, various phases of mixed ammonium and vanadium phosphates were obtained at lower and higher temperatures.     

Interaction of methoxy- and methylenedioxyamphetamines with carbon and polymeric adsorbents in polar liquids

Solid phase extraction (SPE) of methoxy- and methylenedioxyamphetamines from diluted aqueous solutions was investigated on carbon and polymeric adsorbents of different textures and chemical compositions. Those adsorbents were applied cartridges packed with three chemically modified carbons prepared from plum stones (initial A2PS, oxidized A2PS-O, and reduced A2PS-H) and commercially available adsorbents (polymeric LiChrolut EN, graphitized Hypercarb and Carboprep). Several factors influence the recovery rates of amphetamine derivatives such as the polarity of adsorbates (free energy of salvation), the specific surface area and surface composition of adsorbents, and the solvent characteristics. Different combinations of these factors affect the recovery rate (R1) for high- and low-surface area adsorbents. The minimal R1 values are observed for an amphetamine derivative at a maximal solvation effect and for a set of amphetamines adsorbed on graphitized carbons.      

The study of cyclooctene oxidation with molecular oxygen catalyzed by VSi2

The catalytic effect of VSi₂ on initial stages of the liquid-phase oxidation of cyclooctene by molecular oxygen was studied. The vanadium disilicide influences on the oxidation process in the presence of hydroperoxide. VSi₂ takes part in a radical formation stage by catalysis of hydroperoxide decomposition reaction. The catalyst was investigated before and after reaction using FTIR spectroscopy. From the data obtained, the kinetic model of the catalytic oxidation process was proposed and the equation for the reaction rate was derived. The equation has described all observed dependences of reaction rate on the concentration of reactants and content of catalyst.      

On the preparation of synthetic carbon adsorbents using the sulfonated ion exchange resin duolite C-20

Thermal analysis was used to study thermal behavior of the sulfonated ion exchange resin Duolite C20 in the hydrogen, sodium and calcium forms. The aim of this paper was to prepare spherical carbon adsorbents. SEM and AFM microscopic methods have been applied to describe their surface characteristics. It was stated that structural parameters of prepared active carbons depend on the kind of cation present in the resin. The use of calcium form of Duolite C20 as the initial polymer precursor allowed to obtain the active carbon with better yield and better developed pore structure compared with other forms of this ion exchanger.     

VPO catalysts synthesized on substrates with modified activated carbons

VPO catalysts were prepared on oxidized and unoxidized activated carbons differing in initial porous structure. Carbons were oxidized under relatively soft (30% H₂O₂, 200 °C) and hard (50% H₂O₂, 350 °C) conditions. Carbon modification was carried out hydrothermally in a traditional autoclave (HTT) or a microwave reactor (MWT). The synthesis was also carried out under hydrothermal (HTS or MWS) conditions. V₂O₅ and NH₄VO₃ were used as precursors. The samples are characterized by diversified porous structure at S_BET = 732-1617 m²/g and V_por = 0.44-0.90 cm³/g, as well as various degree of VPO crystallinity. Possibility of preparation of the VPO catalysts under ecologically appropriate conditions, i.e. in aqueous solutions, was shown.     

Some properties of milled vanadium phosphates

Mechanochemical modification of vanadium phosphates doped with Bi, Zr, Mo has been studied. Milled samples have been investigated by means of XRD, DTA-TG, FTIR, nitrogen adsorption, electrokinetic measurements. It was found that phase composition of the phosphates does not change upon the mechanochemical modification process. Milling in water causes formation of porous materials. Modification of surface results in changes of the electrokinetic and adsorption properties of the milled samples.     

Influence of mechanochemical activation on structure and some properties of mixed vanadium�Cmolybdenum oxides

Mechanochemical activation of individual V₂O₅, MoO₃ and mixed vanadium-molybdenum oxide system in various media (air, water, and ethanol) has been studied. Powder X-ray diffraction, nitrogen adsorption?Cdesorption, thermogravimetric and chemical analysis, FTIR and Raman spectroscopy, and scanning electron microscopy have been used for research of prepared milled samples. The electrokinetic properties (dependence zeta potential??pH, position of isoelectric point) of individual V₂O₅, MoO₃ and mixed vanadium?Cmolybdenum oxide system, synthesized via mechanochemical treatment in various medium, in aqueous solutions of electrolytes also have been determined. Initial, milled, and spent samples are characterized with the help of XRD, FTIR and Raman spectroscopy, and SEM and adsorption of nitrogen. The catalytic properties of vanadium?Cmolybdenum oxide composition activated in different media have been investigated in reaction of oxidation dehydrogenation of propane.