scholarly journals PREPARATION AND CHARACTERIZATION OF POROUS ALUMINA-TITANIA AEROGEL VIA CO2 SUPERCRITICAL EXTRACTION

2010 ◽  
Vol 4 (3) ◽  
pp. 149-155 ◽  
Author(s):  
Silvester Tursiloadi ◽  
Hiroaki Imai ◽  
Hiroshi Hirashima

Porous aerogel of titania-alumina were prepared by hydrolysis of metal alkoxides and supercritical extraction of the solvent.  Monolithic wet-gel of 0.2TiO2-0.8Al2O3, prepared by hydrolysis of metal alkoxides in alcoholic solutions, and the solvent in wet gel was supercritically extracted in CO2 at 60oC and 24Mpa for 2h. Thermal evolutions of the microstructure of the gel were evaluated by differential thermal analysis (TG-DTA), N2 adsorption, scanning electron microscopy and X-ray diffractometer. After calcination at 500oC, the specific surface area of the gel was more than 400m2g-1. The average pore radius of aerogel, about 8nm, was about 50% of that for alumina aerogel, but about 4 times larger than that of the xerogel.  The specific surface area of the aerogel was more than 200m2g-1 after calcination at 800oC. The pore size and pore volume of aerogel hardly decreased after calcinations at 800oC, although those values of the xerogel remarkably decreased after calcination up to 800oC. The thermal stability of the microstructure of porous titania-alumina is improved by supercritical extraction.   Keywords: Oxides, Sol-gel chemistry, X-ray diffraction, Infrared pectroscopy

2010 ◽  
Vol 7 (2) ◽  
pp. 121-127
Author(s):  
Silvester Tursiloadi ◽  
Dinie Mansur ◽  
Yeny Meliana ◽  
Ruslan Efendi

Stable anatase is attractive because of its notable functions for photocatalysis and photon-electron transfer.  TiO2-nanoparticles dispersed SiO2 wet gels were prepared by hydrolysis of Ti(OC4H9n)4 and Si(OC2H5)4 in a 2-propanol solution with acid catalyst.  The solvent in the wet gels was supercritically extracted using CO2 at 60 oC and 22 Mpa in one-step.  Thermal evolution of the microstructure of the extracted gels (aerogels) was evaluated by XRD measurements, TEM and N2 adsorption measurements. The as-extracted aerogel with a large specific surface area, more than 365 m2g-1, contained anatase nanoparticles, about 5 nm in diameter.  The anatase phase was stable after calcinations at temperatures up to 1000 oC, and BET specific surface area, total pore volume and average pore diameter did not change significantly after calcinations at temperature up to 800 oC.   Keywords: Stable anatase, sol-gel, CO2 supercritical extraction.


MRS Advances ◽  
2017 ◽  
Vol 2 (57) ◽  
pp. 3505-3510
Author(s):  
Jiankai Zhang ◽  
Xiaohong Chen ◽  
Ran Liu ◽  
Huaihe Song ◽  
Zhihong Li

ABSTRACTMagnesium oxide aerogels were made by sol-gel process using magnesium methoxide as precursor, methanol and deionized water as solvent with ethanol supercritical fluid drying. The influences of the different factors on the gel time and the specific surface area of magnesium oxide aerogels were studied, and the structure and morphology were characterized by Scanning Electron Microscopy (SEM), Transmission Electron Microscope (TEM) and X-ray diffraction (XRD), and the Small Angle X-ray Scatter (SAXS) was utilized to determine the fractural structure of the magnesium oxide aerogels. The results show that MgO aerogels belong to the typical mesoporous materials with rich network and highly developed pore structure, and the specific surface area is 904.9 m2/g, the apparent density is 0.055 g/cm3, the average pore size is 19.6 nm. The results of SAXS analysis show that the fractal dimension of the MgO aerogels is 2.32 in high q area which proves the existence of rough surface and pore fractal structure.


2017 ◽  
Vol 68 (3) ◽  
pp. 483-486
Author(s):  
Constantin Sorin Ion ◽  
Mihaela Bombos ◽  
Gabriel Vasilievici ◽  
Dorin Bombos

Desulfurisation of atmospheric distillation gasoline and gas oil was performed by adsorption process on Fe/ bentonite. The adsorbent was characterized by determining the adsorption isotherms, specific surface area, pore volume and average pore diameter. Adsorption experiments of atmospheric distillation gasoline and gas oil were performed in continuous system at 280�320oC, 5 atm and volume hourly space velocities of 1�2 h-1. The efficiency of adsorption on Fe / bentonite was better at desulphurisation of gasoline versus gas oil.


Crystals ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 344
Author(s):  
Chengwu Dong ◽  
Changlong Yin ◽  
Tongtong Wu ◽  
Zhuyan Wu ◽  
Dong Liu ◽  
...  

Unsupported NiMo catalyst has high hydrogenation activity due to its high active site distribution. However, low specific surface area and pore distribution greatly limit the efficient utilization of the active components. The Y-zeolite nanoclusters were hydrothermally synthesized and introduced into the unsupported NiMo catalysts from a layered nickel molybdate complex oxide. The XRD, N2 adsorption-desorption, FT-IR, Py-IR, SEM, NH3-TPD, and TEM were used to characterize all catalysts. The dibenzothiophene (DBT) hydrodesulfurization (HDS) reaction was performed in a continuous high pressure microreactor. The results showed that the specific surface area, pore volume, and average pore size of the unsupported NiMo catalysts were greatly increased by the Y-zeolite nanoclusters, and a more dispersed structure was produced. Furthermore, the Lewis acid and total acid content of the unsupported NiMo catalysts were greatly improved by the Y-zeolite nanoclusters. The HDS results showed that the unsupported NiMo catalysts modified by the nanoclusters had the same high desulfurization efficiency as the unmodified catalyst, but had more proportion of direct desulfurization (DDS) products. The results offer an alternative to reducing hydrogen consumption and save cost in the production of ultra clean diesel.


Materials ◽  
2020 ◽  
Vol 13 (5) ◽  
pp. 1230
Author(s):  
Fabien Léonard ◽  
Zhen Zhang ◽  
Holger Krebs ◽  
Giovanni Bruno

The mixture of ammonium nitrate (AN) prills and fuel oil (FO), usually referred to as ANFO, is extensively used in the mining industry as a bulk explosive. One of the major performance predictors of ANFO mixtures is the fuel oil retention, which is itself governed by the complex pore structure of the AN prills. In this study, we present how X-ray computed tomography (XCT), and the associated advanced data processing workflow, can be used to fully characterise the structure and morphology of AN prills. We show that structural parameters such as volume fraction of the different phases and morphological parameters such as specific surface area and shape factor can be reliably extracted from the XCT data, and that there is a good agreement with the measured oil retention values. Importantly, oil retention measurements (qualifying the efficiency of ANFO as explosives) correlate well with the specific surface area determined by XCT. XCT can therefore be employed non-destructively; it can accurately evaluate and characterise porosity in ammonium nitrate prills, and even predict their efficiency.


Polymers ◽  
2019 ◽  
Vol 11 (6) ◽  
pp. 1067 ◽  
Author(s):  
Vyacheslav V. Rodaev ◽  
Svetlana S. Razlivalova ◽  
Andrey O. Zhigachev ◽  
Vladimir M. Vasyukov ◽  
Yuri I. Golovin

For the first time, zirconia nanofibers with an average diameter of about 75 nm have been fabricated by calcination of electrospun zirconium acetylacetonate/polyacrylonitrile fibers in the range of 500–1100 °C. Composite and ceramic filaments have been characterized by scanning electron microscopy, thermogravimetric analysis, nitrogen adsorption analysis, energy-dispersive X-ray spectroscopy, and X-ray diffractometry. The stages of the transition of zirconium acetylacetonate to zirconia have been revealed. It has been found out that a rise in calcination temperature from 500 to 1100 °C induces transformation of mesoporous tetragonal zirconia nanofibers with a high specific surface area (102.3 m2/g) to non-porous monoclinic zirconia nanofibers of almost the same diameter with a low value of specific surface area (8.3 m2/g). The tetragonal zirconia nanofibers with high specific surface area prepared at 500 °C can be considered, for instance, as promising supports for heterogeneous catalysts, enhancing their activity.


2011 ◽  
Vol 403-408 ◽  
pp. 1205-1210
Author(s):  
Jaleh Babak ◽  
Ashrafi Ghazaleh ◽  
Gholami Nasim ◽  
Azizian Saeid ◽  
Golbedaghi Reza ◽  
...  

In this work ZnO nanocrystal powders have been synthesized by using Zinc acetate dehydrate as a precursor and sol-gel method. Then the products have been annealed at temperature of 200-1050°C, for 2 hours. The powders were characterized using X-ray diffraction (XRD), UV-vis absorption and photoluminescence (PL) spectroscopy. The morphology of refrence ZnO nanoparticles have been studied using Transmission Electron Microscope (TEM). During the annealing process, increase in nanocrystal size, defects and energy gap quantitative, and decrease in specific surface area have been observed.


Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2839 ◽  
Author(s):  
Renata F. Botti ◽  
Murilo D.M. Innocentini ◽  
Thais A. Faleiros ◽  
Murilo F. Mello ◽  
Danilo L. Flumignan ◽  
...  

This work investigates the catalytic activity of geopolymers produced using two different alkali components (sodium or potassium) and four treatment temperatures (110 to 700 °C) for the methyl transesterification of soybean oil. The geopolymers were prepared with metakaolin as an aluminosilicate source and alkaline activating solutions containing either sodium or potassium in the same molar oxide proportions. The potassium-based formulation displayed a higher specific surface area and lower average pore size (28.64–62.54 m²/g; 9 nm) than the sodium formulation (6.34–32.62 m²/g; 17 nm). The reduction in specific surface area (SSA) after the heat treatment was more severe for the sodium formulation due to the higher thermal shrinkage. The catalytic activity of the geopolymer powders was compared under the same reactional conditions (70–75 °C, 150% methanol excess, 4 h reaction) and same weight amounts (3% to oil). The differences in performance were attributed to the influences of sodium and potassium on the geopolymerization process and to the accessibility of the reactants to the catalytic sites. The Na-based geopolymers performed better, with FAME contents in the biodiesel phase of 85.1% and 89.9% for samples treated at 500 and 300 °C, respectively. These results are competitive in comparison with most heterogeneous base catalysts reported in the literature, considering the very mild conditions of temperature, excess methanol and catalyst amount and the short time spent in reactions.


Nanomaterials ◽  
2020 ◽  
Vol 10 (12) ◽  
pp. 2527
Author(s):  
Tingting Niu ◽  
Bin Zhou ◽  
Zehui Zhang ◽  
Xiujie Ji ◽  
Jianming Yang ◽  
...  

Resorcinol-formaldehyde/titanium dioxide composite (RF/TiO2) gel was prepared simultaneously by acid catalysis and then dried to aerogel with supercritical fluid CO2. The carbon/titanium dioxide aerogel was obtained by carbonization and then converted to nanoporous titanium carbide/carbon composite aerogel via 800 °C magnesiothermic catalysis. Meanwhile, the evolution of the samples in different stages was characterized by X-ray diffraction (XRD), an energy-dispersive X-ray (EDX) spectrometer, a scanning electron microscope (SEM), a transmission electron microscope (TEM) and specific surface area analysis (BET). The results showed that the final product was nanoporous TiC/C composite aerogel with a low apparent density of 339.5 mg/cm3 and a high specific surface area of 459.5 m2/g. Comparing to C aerogel, it could also be considered as one type of highly potential material with efficient photothermal conversion. The idea of converting oxide–carbon composite into titanium carbide via the confining template and low-temperature magnesiothermic catalysis may provide new sight to the synthesis of novel nanoscale carbide materials.


NANO ◽  
2020 ◽  
Vol 15 (06) ◽  
pp. 2050079
Author(s):  
Xuelei Li ◽  
Jinfeng Bai ◽  
Jiaqi Li ◽  
Chao Li ◽  
Junru Zhang ◽  
...  

In this study, nitrogen-deficient graphitic carbon nitride (M-LS-g-C3N4) with a mesoporous structure and a large specific surface area was obtained by calcination after melt pretreatment using urea as a precursor. X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption, X-ray photoelectron spectroscopy (XPS), UV-Vis, ESR and photoluminescence (PL) were used to characterize the structure, morphology and optical performance of the samples. The TEM results showed the formation of a mesoporous structure on the 0.1[Formula: see text]M-LS-g-C3N4 surface. The porous structure led to an increase in the specific surface area from 41.5[Formula: see text]m2/g to 124.3[Formula: see text]m2/g. The UV-Vis results showed that nitrogen vacancies generated during the modification process reduced the band gap of g-C3N4 and improved the visible light absorption. The PL spectra showed that the nitrogen defects promoted the separation of photogenerated electron–hole pairs. In the visible light degradation of methyl orange (MO), the reaction rate constant of 0.1[Formula: see text]M-LS-g-C3N4 reached 0.0086[Formula: see text][Formula: see text], which was 5.05 times that of pure g-C3N4. Superoxide radicals and photogenerated holes were found to be the main active species in the reaction system. This study provides an efficient, green and convenient means of preparing graphitic carbon nitride with a large specific surface area.


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