На основании данных комплекса физико-химических методов (термический анализ, низкотемпературная адсорбция азота, рентгенофазовый анализ, спектроскопия комбинационного рассеяния, электронная микроскопия, температурно-программируемое восстановление водородом) проведен сопоставительный анализ свойств массивных и нанесенных на оксид алюминия оксидов Ce1-xNixOy (x = 0.2–0.8; y = 1.2–1.8), проявляющих каталитическую активность в реакциях риформинга. Показано, что синтезированные образцы – мезопористые материалы с удельной поверхностью 100±10 м2/г, которые содержат в своем составе твердые растворы замещения с кубической структурой типа флюорита. В отличие от образцов массивных сложных оксидов Ce1-xNixOy, для Ce1-xNixOy/Al2O3 наблюдается устойчивость к спеканию при высокотемпературных обработках в ходе активации и последующей реакции, увеличение температуры формирования металлических Ni-частиц (540 vs. 350°C) и сохранение дисперсности Ni0 фазы после реакции (6.5 vs. 50 нм). Выявлена взаимосвязь между характеристиками материалов и их функциональными свойствами.
A comparative analysis of the properties of bulk and aluminum oxide supported Ce1–xNixOy oxides (x = 0.2-0.8; y = 1.2-1.8) exhibiting catalytic activity in reforming reactions is performed using a complex of physical and chemical methods (thermal analysis, low-temperature nitrogen adsorption, powder XRD, Raman spectroscopy, electron microscopy, hydrogen temperature-programmed reduction). It is shown that the obtained samples are mesoporous materials with a specific surface area of 100±10 m2/g, containing substitutional solid solutions with fluorite cubic structure in their composition. In contrast to bulk Ce1–xNixOy complex oxide samples, the Ce1–xNixOy/Al2O3 material exhibits resistance to sintering during high temperature treatments in the course of activation and the subsequent reaction. At the same time, the formation temperature of metal Ni particles increases (540 °C vs. 350 °C) and the dispersion of the Ni0 phase after the reaction is preserved (6.5 nm vs. 50 nm). A relationship between characteristics of these materials and their functional properties is revealed.
By means of elemental and X-ray powder diffraction analysis, N2 adsorption at –196°C and CO2 adsorption at 0°C the textural properties of KNaLSX zeolite were studied after ion exchange modification in 1M NH4Cl solution followed by vacuum degassing at 40°C or drying in air at 120°C. The possibility of retaining the microporous structure of zeolite in the former case and its partial destruction in the latter case is shown.
By means of elemental and X-ray powder diffraction analysis, N 2 adsorption at –196°C and CO 2 adsorption at 0°C the textural properties of KNaLSX zeolite were studied after ion exchange modification in 1M NH 4 Cl solution followed by vacuum degassing at 40°C or drying in air at 120°C. The possibility of retaining the microporous structure of zeolite in the former case and its partial destruction in the latter case is shown.
By means of elemental and X-ray powder diffraction analysis, N2 adsorption at –196°C and CO2 adsorption at 0°C the textural properties of KNaLSX zeolite were studied after ion exchange modification in 1M NH4Cl solution followed by vacuum degassing at 40°C or drying in air at 120°C. The possibility of retaining the microporous structure of zeolite in the former case and its partial destruction in the latter case is shown.
Alteration of adsorption properties and porous structure (texture) of the KNaLSX zeolite at the initial stages of its destruction during ion-exchange modification in solutions of NH4Cl and thermal shock under vacuum degassing has been studied. Transmission electron microscopy, X-ray diffraction, low-temperature nitrogen adsorption and adsorption of CO2 and CH4 at 273 K were applied for characterization of the obtained materials. Conversion of the predominantly microporous material to the material with threemode pore-size distribution is shown. Significant fraction of the faujasite phase and corresponding micropores are preserved in the material. This is accompanied with formation of pores of two types: quasi-spherical mesopores with the characteristic size of 5 nm and the meso-macropores with typical size exceeding 40 nm. Basing on the obtained results, a mechanism of textural changes in the LSX zeolite treated under applied conditions is proposed.
AbstractThe adsorption and textural properties of LSX zeolite after cation exchange both in LiCl and NH