Authors:V. Sydorchuk, S. Khalameida, J. Skubiszewska-Zięba, and R. Leboda
Compositions based on oxides and containing 5–20% w/w of ammonium molybdophosphate have been synthesized by means of different routes. Prepared samples have been studied using nitrogen adsorption–desorption, XRD, DTA–TG, and FTIR spectroscopy. Keggin structure is retained at incorporation of ammonium molybdophosphate into siliceous framework or its deposition on oxide surface and duration following calcinations up to 500 °C. Compositions possess porous structure from micromesoporous to mesomacroporous depending on the preparation method.
Authors:S. Khalameida, V. Sydorchuk, J. Skubiszewska-Zięba, R. Leboda, and V. Zazhigalov
In this article, mechanochemical synthesis of barium titanate from different raw materials was studied. The prepared nanodispersed
powders were investigated by means of XRD, DTA-TG, DSC, FTIR, Raman, UV–VIS, ESR spectroscopy, and low-temperature adsorption
of nitrogen. Barium titanate possessing high specific surface area was produced directly during dry milling from the mixtures
of barium oxides and titanium dioxide low-temperature forms (amorphous and anatase).
Authors:S. Khalameida, J. Skubiszewska-Zięba, V. Zazhigalov, R. Leboda, and K. Wieczorek-Ciurowa
Mechanochemical treatment (MChT) in various media (water, air, ethanol) of the V2O5/ammonium dimolybdate composition at the ratio V:Mo = 0.7:0.3 has been carried out. Physicochemical transformations in this
system have been studied by means of X-ray powder diffraction (XRD) and thermal analysis as well as FTIR spectroscopy. Ammonium
dimolybdate undergoes hydration with formation of 4-aqueous ammonium paramolybdate during the MChT in water. Changes of phase
and chemical composition at activation are determined first of all by nature of medium in which milling was carried out. Maximal
interaction of components occurs during modification of the studied system in water.
Authors:V. Sydorchuk, O. Makota, S. Khalameida, L. Bulgakova, J. Skubiszewska-Zięba, R. Leboda, and V. Zazhigalov
The deposition of molybdenum and vanadium oxides onto fumed silica, titania, and alumina as supports through dry milling has been carried out. The structure of prepared compositions has been investigated by means of XRD, DTA–TG, FTIR, and UV–Vis spectroscopy, nitrogen adsorption. The deposited crystal phases are sufficiently uniformly distributed on support surface. The supported oxides are subjected to dispersion in process of milling to the state of oligomeric or isolated species. Milled bulk and deposited MoO3 (first of all, on alumina) possesses improved catalytic performance in process of epoxidation of 1-octene. Vanadium pentoxide also has higher activity in this process.
Authors:J. Skubiszewska-Zięba, B. Charmas, R. Leboda, V. A. Tertykh, and V. V. Yanishpolskii
Mesoporous titanium-containing silicas with different Titania contents were investigated. The structural parameters of the materials were characterized by low-temperature adsorption/desorption of nitrogen and X-ray diffraction analysis. The thermodesorption of water using the quasi-isothermal thermogravimetry as well as the differential scanning calorimetry were used to characterize thermal and surface properties of these materials. The adsorbed water layers and the concentration of weakly and strongly bound water as well as the surface free energy on the adsorbent/water interfaces were calculated. It was stated that the increase of Titania content causes a gradual decrease of specific surface area and formation of biporous structure inside the tested materials. The water thermodesorption from the surface proceeds in two or three stages, which is connected mainly with pore distribution and TiO2 content. One can observe the increase of the total surface free energy (ΔGΣ) with the increasing TiO2 content, but the largest ΔGΣ value at the adsorbent/strongly bound water interface is exhibited by the adsorbent of intermediate content (30%) of TiO2. Freezing temperature of water contained in the pores of the studied materials is connected largely with their porous structure. Due to the well developed porous structure, the water freezing process is a multi-stage one.
Authors:Yu. Trach, V. Sydorchuk, O. Makota, S. Khalameida, R. Leboda, J. Skubiszewska-Zięba, and V. Zazhigalov
Deposited catalysts composition H3PMo12O40/SiO2 and Ag/H3PMo12O40/SiO2 have been synthesized on the basis of fumed silica, including milling technique. Physical–chemical characteristics of prepared catalysts have been studied by means of XRD, DTA-TG, FTIR, UV–Vis spectroscopy, and adsorption of nitrogen. Catalysts possess meso- or meso-macroporous structure and contain deposited Keggin heteropolycompounds. Deposition of heteropolycompounds on support with high specific surface area results in increase of selectivity to epoxide in epoxidation reactions. The use of milling during catalyst synthesis leads to further growth of selectivity of epoxides formation.
Authors:V. Yanishpolskii, A. Pavlenko, V. Tertykh, V. Il'in, R. Leboda, and J. Skubiszewska-Zieba
Mesoporous titanium-containing silicas with TiO2 contents from 1 up to 70 mol% were prepared. The obtained samples have been characterized by the powder X-ray diffraction
data, the diffuse reflectance infrared Fourier transform method, and nitrogen adsorption at 77 K. Specific surface area, total
pore volume, distribution pore volume on pore sizes were determined from nitrogen adsorption isotherm for synthesized titanosilicas.
Authors:V. Sydorchuk, W. Janusz, S. Khalameida, E. Skwarek, J. Skubiszewska-Zięba, R. Leboda, and V. Zazhigalov
Deposited zirconium phosphate samples on the base of silica and titania have been prepared using the sol–gel and mechanochemical methods. Porous structure, phase composition, and electrokinetic parameters have been studied by means of nitrogen adsorption–desorption, XRD, DTA-TG, FTIR, electrophoresis, and potentiometric titration. The compositions possess varied parameters of porous structure, structure of deposited phase, and electrokinetic properties depending on support nature and synthesis conditions.
Authors:N. Ivashchenko, V. Tertykh, V. Yanishpolskii, J. Skubiszewska-Zięba, R. Leboda, and S. Khainakov
A promising approach to control palladium nanoparticle sizes by application of silane modified silicas was suggested. The combination of reductive properties of silicon hydride groups and hydrophobic properties of alkylsilyl groups which act as agglomeration limiters for metal nanoparticles gives an opportunity to synthesize uniformly distributed particles with a specified size. Silicas modified with triethoxysilane (TES) and diisopropylchlorosilane (DIPCS), as well as, the combination of hexamethyldisilazane (HMDS) and triethoxysilane were applied for formation of such bifunctional matrices. Properties of the silane-modified silica samples and changes occurred during the formation of palladium nanoparticles were studied by IR spectroscopy. Thermal stability of surface chemical compounds was investigated by thermogravimetric analysis (TGA); low-temperature nitrogen adsorption was used to study structural properties of the applied materials. With the use of transmission electron microscopy (TEM) the dependence of palladium nanoparticle size on the nature of support surface layer was found.
Authors:V. Sydorchuk, S. Khalameida, V. Zazhigalov, J. Skubiszewska-Zięba, and R. Leboda
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.