硝化法制备对氨基间硝基苯磺酸的研究

以对氨基苯磺酸为起始原料 ,经过乙酰化、硝化、水解三步来制备标题物。通过正交试验找出了酰化的最佳反应条件为 :对氨基苯磺酸与乙酐的摩尔比为 1∶1.0 5 ,反应总时间为 1.5h ,反应温度为 2 5℃ ,酰化介质为酰化反应前用碳酸钠及水将对氨基苯磺酸完全溶解 ,使混合液 pH值为 5～ 6 ,反应过程中不再补加碳酸钠 ,其酰化转化率可达 99.6 % ,酰化产物的固体收率可达 96 .0 % ;硝化反应的最佳条件为 :硝化剂用 90 .2 %的硝酸 ,对乙酰氨基苯磺酸与硝化剂的摩尔比为 1∶1.0 5 ,反应温度为 10℃ ,浓硫酸与对乙酰氨基苯磺酸的摩尔比为 8.3∶1,其硝化转化率可达 96 .0 % ,硝化反应的选择性好 ,对氨基邻硝基苯磺酸的量不到 1.0 %。     

Structure–Function Relations in Supported Ni–W Sulfide Hydrogenation Catalysts

Ni–W catalysts were prepared by impregnation of commercial -alumina and silica supports. The sulfidation, performed directly after drying at 100°C, yielded fully sulfided Ni–W species on both supports (SEM-EDAX, XPS, XRD). At optimal metals loading (50 wt% NiO + WO₃, Ni/W = 2), the sulfided catalysts had similar texture (N₂ adsorption) and displayed similar activity in dibenzothiophene hydrodesulfurization (DBT HDS), while the activity of the Ni–W/SiO₂ catalyst in toluene hydrogenation (HYD) was six times higher than that of Ni–W/Al₂O₃. This is due to the more than two times higher WS₂ slabs stacking number in Ni–W/SiO₂ compared with Ni–W/Al₂O₃ (XRD, HR-TEM), yielding stronger adsorption of toluene (TPD).     

Structural analysis of Aleksinac oil shale kerogen by high-resolution solid-state C n.m.r. spectroscopy

A sample of kerogen from Aleksinac oil shale was examined by high-resolution solid-state ¹³C n.m.r. spectroscopy. The presence and relative proportions of kerogen structural units were estimated using a combination of NQS and T_1C methods with a peak-synthesis technique applied to the ¹³C CP—MAS spectrum. Relaxation parameters from these experiments were used to estimate differences in relative ‘mobility’ of various structural units. The kerogen was found to be highly aliphatic and to contain 79% long-chain aliphatic plus alicyclic structures, as well as 9% aromatic structures. These findings are in good agreement with the characterization of the same kerogen from its oxidation products.     

溴素法α-溴代间氯苯丙酮合成研究

在金属卤化物催化剂 HD2 0 0 1存在下 ,溴与间氯苯丙酮在乙酸中反应得到盐酸安非他酮中间体 α-溴代间氯苯丙酮。最佳反应条件是 :n(间氯苯丙酮 )∶n(溴 ) =1∶ 1 ,催化剂用量为 1 %(质量分数 ) ,溴滴加时间为 1 h,反应温度为 1 0°C,此条件下 ,产物纯度为 98.83%,收率为 96.1 %。     

NH3-NO/NO2 SCR for diesel exhausts after treatment: mechanism and modelling of a catalytic converter

We review herein the key mechanistic and kinetic features of the reactions involved in the NH₃-NO/NO₂ SCR system investigated by dynamic reactive experiments over a V-based commercial powdered catalyst, eventually leading to the proposal of an original redox scheme which accounts for stoichiometry, selectivity and intrinsic kinetics of the global SCR process.     

Redox Properties and Catalytic Behavior of Praseodymium-Modified (Ce-Zr)O2 Solid Solutions in Three-Way Catalysts

The three-way catalyst promoters (Ce-Zr)O₂, (Pr-Ce-Zr)O₂ and (Pr-Zr)O₂ were prepared by the sol-gel method. The reduction/oxidation behavior of these mixed oxides was compared. It is shown that the formation of (Pr-Zr)O₂ cubic solid solution at high temperature up to 800 °C makes it more reducible, and that the ternary solid solution that formed in (Pr-Ce-Zr)O₂ mixed oxides plays an important role in the reduction process. The catalytic performance tests reveal that the introduction of a small amount of praseodymium into (Ce-Zr)O₂ favors the light-off temperature of C₃H₆ and NO and the effectiveness for NO conversion at the lean region.     

Persistence of nonprotein seed amino acid s-(β-carboxyethyl)-cysteine in young leaves ofCalliandra rubescens Ecological implications

The insecticidal nonprotein amino acid S-(-carboxyethyl)-cysteine (S-CEC) is the major free amino acid in the seeds of severalCalliandra spp. where it accounts for up to 2.9 % of dry weight. Lesser amounts of other related S-containing amino acids and an array of nonprotein imino acids derived from pipecolic acid are other constituents. High concentrations of imino acids, which also show insecticidal activity, are maintained in the mature leaves, but sulfur compounds are lacking. In this study the disappearance of S-CEC from the germinating seeds and young seedlings ofC. rubescens was monitored over time. After 10 weeks, S-CEC continues to be found in high concentrations in the stems and new leaves. As young leaves mature, sulfur compounds quickly decrease in concentration. Traces of S-CEC are found in new leaves of plants up to nine months after germination. Whether high concentration of S-CEC in young leaves is due to transportation from the seed or de novo synthesis is unclear. The ecological implications are discussed.     

漆酶氧化还原介质系统的作用机理及其应用

对漆酶-氧化还原介质系统作用机理及其应用的研究进展进行了综述。漆酶的催化反应发生在铜离子形成的活性中心,当介质存在时通过介质中间体传导电子使得反应的速度加快,效率提高,氧化底物范围可进一步扩大。这种漆酶介质系统作为新型的生物制剂在纸浆漂白、纺织品生物整理、环保等方面具有重要的应用价值。     

Long-term and seasonal nitrate trends illustrate potential prevention of large cyanobacterial biomass by sediment oxidation in Hamilton Harbour,Lake Ontario

Several studies have shown that large, experimental additions of nitrate (NO₃) to eutrophic systems can mitigate large populations of nuisance cyanobacteria and that high NO₃ concentrations can oxidize anoxic sediments. These studies are consistent with observations from numerous aquatic systems across a broad trophic range showing development of reduced surficial sediments precedes the formation of large cyanobacteria populations. We use 50+ years of data to explore whether high NO₃ concentrations may have been instrumental both in the absence of large populations of cyanobacteria in eutrophic Hamilton Harbour, Lake Ontario in the 1970s when total phosphorus (TP) and total nitrogen (TN) concentrations were high, and in delaying large populations until August and September in recent decades despite much lower TP and TN. Our results indicate that large cyanobacteria population events do not occur at the central station in July-September when epilimnetic NO₃ > 2.2 mg N L^?1. The results further suggest that remedial improvements to wastewater treatment plant oxidation capacity may have been inadvertently responsible for high NO₃ concentrations > 2.2 mg N L^?1 and thus for mitigating large cyanobacteria populations. This also implies that large cyanobacteria populations may form earlier in the summer if NO₃ concentrations are lowered.     

Sky Based Light Metering for High Dynamic Range Images

Image calibration requires both linearization of pixel values and scaling so that values in the image correspond to real‐world luminances. In this paper we focus on the latter and rather than rely on camera characterization, we calibrate images by analysing their content and metadata, obviating the need for expensive measuring devices or modeling of lens and camera combinations. Our analysis correlates sky pixel values to luminances that would be expected based on geographical metadata. Combined with high dynamic range (HDR) imaging, which gives us linear pixel data, our algorithm allows us to find absolute luminance values for each pixel—effectively turning digital cameras into absolute light meters. To validate our algorithm we have collected and annotated a calibrated set of HDR images and compared our estimation with several other approaches, showing that our approach is able to more accurately recover absolute luminance. We discuss various applications and demonstrate the utility of our method in the context of calibrated color appearance reproduction and lighting design.