The effects of the volume and pH of the impregnation solution and of the calcination conditions were examined on the physicochemical and catalytic properties of a 13 wt% MoO3/Al2O3 extrudate catalyst. The Al2O3 support and drying procedures (static conditions without flowing air) were fixed in the preparations. In the present series of catalysts, the amount of crystalline MoO3 was marginally small. It was found that the dispersion of Mo oxide species increased as the volume of the impregnation solution increased, gradually approaching a maximum value. The increase in pH (2–8) of the impregnation solution was found to reduce the dispersion of Mo oxide species. The Mo dispersion increased slightly for the impregnation catalysts as the calcination temperature increased (673–873 K), whereas it decreased for the equilibrium adsorption catalysts. The effects of the calcination atmosphere (with or without flowing air, or with flowing humid air) were very small on the dispersion of Mo oxide species under the present preparation conditions. On the other hand, the methanol oxidation activity of MoO3/Al2O3 was sensitive to the preparation parameters examined here. It was demonstrated by means of EPMA and XPS that a considerable migration of Mo took place during the calcination.
In the present study on the preparation of a 13 wt% MoO3/Al2O3 catalyst, an impact index is proposed to measure the magnitude of the effects of the respective parameter(s) on the physicochemical and catalytic properties. With the Mo dispersion, the effects of the preparation parameter decreased in the order, surface area of the support >> drying process > volume of the impregnation solution > pH, calcination temperature and atmosphere. The size of the impact index for the dispersion of Mo sulfide species is 70–75% of that for the Mo oxide species. The HDS activity of the catalyst was less affected by the preparation parameters than the Mo sulfide dispersion. The preparation parameters affected the segregation of Mo on the outer surface of extrudates in a decreasing order: drying process > volume of the impregnation solution > pH, calcination conditions. It was found that the oxidation of methanol was affected most intensely by the drying procedures. The volume of the impregnation solution, calcination conditions and pH of the impregnation solution also strongly affected the oxidation activity. The impact index suggests that the sensitivity to the preparation variables of the physicochemical and catalytic properties of MoO3/Al2O3 decreases in the order, methanol oxidation activity > surface Mo segregation > Mo oxide dispersion > Mo sulfide dispersion > HDS activity. 相似文献
Network copolyesters were prepared from trimesic (Y), pyromellitic (X) or mellitic (YH) acids and 1,6-hexanediol (6G). Prepolymers prepared by meltpolycondensation were cast from dimethylformamide solution and postpolymerized at 260°C for 6h to form a network. The resultant films were transparent, flexible and insoluble in any organic solvents. Degree of reaction estimated from the infrared absorbance of ester and methylene groups was almost the same for all films, 94–96%. X-ray diffraction intensity curves and densities showed that the ordering of networks was decreased by the copolymerization, which was remarkable for 6G–X/YH copolymer films and was consistent with the higher decreases of heat-distortion temperature for these copolymer films. The copolymerization also caused decrease of thermal stability, tensile properties and alkali resistance and increase of dye absorption. 相似文献
The rapid hydrolysis of potato starches differing in phosphorus content, as well as sweet potato, cassava and yam starches, was accomplished by treatment of gelatinised starches with bacterial liquefying α-amylase at 50 °C for 1 h, followed by Bacillus licheniformis α-amylase at 55 °C up to 24 h, and then by glucoamylase at 40 °C for a further 24 h. Among the potato starches, the high-phosphorus starches showed higher starch resistant capacity than the medium-phosphorus starches, as well as other tuber and root starches. The hydrolysis rate of tuber and root starches was not greatly influenced by their amylose content and median granule size. Only glucose was detected in the almost completely hydrolysed tuber and root starch samples, indicating that the concomitant enzymes treatment could hydrolyse both the α-1,4 and α-1,6 linkages of the starches examined. 相似文献
A PCR method for the effective detection of Coxiella burnetii in commercially available mayonnaise was developed. Sample preparations were isolated from 50 g portions of each mayonnaise product by four successive extraction steps in phosphate buffer with 2.0 M NaCl. These extracts were then centrifuged at 20,000 x g for 60 min. DNA was isolated from the solution containing the precipitate with a commercial kit, and amplified quantitatively using real-time PCR that targeted the com1 region of C. burnetii. The recoveries of C. burnetii from 2 kinds of commercial mayonnaise specimens, with a baseline control of 1 x 10(7) particles of the Nine Mile phase II strain, were 85.0 +/- 6.0% and 72.0 +/- 0.4%, respectively. The determination limit of this method was 500 C. burnetii particles per 50 g of mayonnaise. The DNA specimens isolated from 50 different commercial mayonnaise samples sold in Tokyo using this method were amplified using both nested PCR and real-time PCR. No contamination by C. burnetii was detected in any of the mayonnaise samples. 相似文献
We demonstrate here a novel method for self-assembling in dimensional alignment the alkoxy-capped silicon nanoparticles synthesized through a room-temperature chemical route. The alkoxy-capped silicon nanoparticles were prepared via a reduction of silicon tetrachloride with sodium-naphthalide and subsequent surface capsulation with 1-octanol monolayers. In the present method, a sublimation process, which was employed as a final purification process for removing the residual naphthalene, influenced significantly on the final morphology of the resultant nanoparticles. Scanning transmission electron microscope (STEM) confirmed the spherical nanoparticles on a holey carbon grid after sublimation process, while only the fibril-like morphology just before sublimation process. In the former sample, the resultant particle size was measured by STEM to be about 9.5 nm +/- 3.4 nm. On the other hand, in the latter sample, the fibril-like structures were shaped by self-assembled silicon nanoparticles in dimensional alignment. The diameters and lengths of the fibril-like assemblies were approximately measured to be 10 to 20 nm and over 5 microm, respectively. 相似文献
Semiconductor photocatalysis has received much attention as a potential solution to the worldwide energy shortage and for counteracting environmental degradation. This article reviews state-of-the-art research activities in the field, focusing on the scientific and technological possibilities offered by photocatalytic materials. We begin with a survey of efforts to explore suitable materials and to optimize their energy band configurations for specific applications. We then examine the design and fabrication of advanced photocatalytic materials in the framework of nanotechnology. Many of the most recent advances in photocatalysis have been realized by selective control of the morphology of nanomaterials or by utilizing the collective properties of nano-assembly systems. Finally, we discuss the current theoretical understanding of key aspects of photocatalytic materials. This review also highlights crucial issues that should be addressed in future research activities. 相似文献
We investigated effects of delithiation on crystal, electronic structure, thermodynamic stability and physical property of LixNi0.5Mn0.5O2 by using a chemical delithiation treatment with ammonium peroxodisulfate, and compared the results with those of electrochemical delithiation. X-ray diffraction and thermodynamic data indicated that there was no phase transition in the samples after the chemical delithiation treatment within the lithium range of 0.50 ≤ x ≤ 1.00. From the ICP measurements and potentiometric titration, it was found that the chemical treatment successfully remove Li from the structure without any elution of Ni and Mn, but it accompanied O2 removal at an initial process of the delithiation, i.e. 0.80 ≤ x ≤ 1.00. Crystal and electronic structure analyses also suggested such a O2 removal at the lithium content range in the chemical delithiation method, although the estimated structure changes below x = 0.80 showed similar tendencies to those by the electrochemical delithiation. 相似文献