新型催化剂载体材料—镁铝复合氧化物的制备及其物理化学性质

以ＮａＯＨ，Ｎａ２ＣＯ３混合或以ＮＨ４ＯＨ，（ＮＨ４）２ＣＯ３混合液为沉淀制备了Ｍｇ／Ａｌ＝３－６．７的Ｍｇ－Ａｌ为滑石。将水滑石在５００－６００℃下焙烧制得了具有与Ｍｇｏ相同的晶体结构的Ｍｇ（Ａｌ）Ｌ复合氧化物，它们的比表面积大于或接近γ－Ａｌ２Ｏ３，而且具有良好的热稳定性。     

The Effect of Styrene-Butadiene-Styrene Modification on the Characteristics and Performance of Bitumen

Summary. In order to cover the effect of styrene-butadiene-styrene (SBS) modification on the characteristics of bitumen, two types of bitumen, one plain bitumen, and one polymer modified bitumen produced with the plain bitumen as base material were characterized in terms of chemical composition, microstructure, micromechanical properties, and thermoanalytical behavior. In order to determine the complex chemical composition of bitumen, elemental analysis, gel permeation chromatography, and the Iatroscan method were employed. Microstructure and micromechanical properties were determined using an environmental scanning electron microscope and the nanoindentation technique. Modulated differential scanning calorimetry was used to determine phase-change temperatures and endo/exotherms associated with molecular movement. The addition of SBS leads to different rheological behavior over the whole service temperature range. This is reflected in bitumen chemistry by differences in elemental composition and molecular weight distribution with much higher M _w values for the modified bitumen. Accordingly, the polymer leads to a shift in molecular fractions. Electron microscopy reveals two distinct phases building up the bitumen microstructure. The chosen mode of quantification leads to similar material parameters for both bitumens, which is explained by the use of the same base material. In contrast, nanoindentation delivers viscosities in the micro-range corresponding to large-scale rheological properties. Modulated differential scanning calorimetry indicates two glass transitions corresponding with two material phases also confirmed by other experiments. Due to modification, these glass transitions depart from each other and the amount of the two material phases changes, correlating with the shift in molecular fractions observed in Iatroscan analyses.     

A bio-waste derived sustainable heterogenous catalyst for Biginelli reaction

This study is targeted at agricultural waste-derived heterogeneous catalysts, which have been effectively employed for Biginelli reaction. The application of cotton waste (Gossypium) derived lignin as a heterogeneous catalyst for C–C bond formation via one pot multicomponent Biginelli reaction. Here we hypothesize that the preparation of bio-waste derived catalyst by high temperature pyrolysis method under anaerobic conditions. The bio-waste derived heterogeneous catalyst (BDC) was well characterized by using different analytical techniques such as BET, SEM, TEM, XRD, DSC, TGA, ICP. The acidity of the catalyst was determined by a Hammett indicator test and titration method. An excellent yield of 6-methyl-2-oxo/thio-4-phenyl substituted-1,2,3,4-tetrahydropyrimidine-5-ethyl carboxylate derivatives was obtained in shorter reaction time (>80% yield in 15–30 min). The catalyst used in these studies has the advantage of being a waste material. Consequently, it is a low-cost, easily prepared, recyclable and environmentally benign. In addition, the use of a biogenic renewable catalyst, its atom economy, and room temperature and solvent-free reaction conditions and the avoidance of column chromatography make the protocol highly significant from green and sustainable chemistry perspectives. The synthesized compounds were characterized by modern analytical techniques like NMR, MS, FT-IR, CHNS analysis. The experimental parameters like % mole of catalyst, mole ratio, temperature and time for reaction completion were also optimized to achieve maximum yield and purity. The surface interaction between BDC and reactant was also studied.     

基于可见光催化分解水制氢的物理化学综合实验设计

将可见光催化分解水制氢引入物理化学综合实验,系统介绍了催化剂制备、表征及光催化反应性能评价等实验内容.以无毒、易制备的g-C3N4作为实验用可见光催化剂,考查了制备温度对催化剂的结构及光催化性能的影响.     

Structure and surface properties of praseodymium modified alumina

Mixed PrO₂-Al₂O₃ oxides with different PrO₂ content (1-20 wt.%) were prepared by wetness impregnation of γ-alumina with aqueous solution of praseodymium nitrate. The samples were characterized by different techniques, using surface adsorption-desorption of N₂ (S_BET), thermogravimetric analysis (TGA), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectroscopy (DRS), temperature-programmed reduction (TPR) and temperature-programmed desorption of CO₂ (TPD-CO₂). TGA and XRD showed the presence of small praseodymium oxide species on the alumina surface. XPS and DRS detected electron deficient interaction between deposited praseodymium oxide and alumina. It was observed a lower reduction temperature for supported Pr oxide species compared to that of the bulk Pr₆O₁₁. TPD-CO₂ studies suggested that the deposition of Pr oxide on alumina leaded to increase of the basicity of mixed oxides.     

New hydrofluoropolyethers II: Physico-chemical characterization

We obtained, through an original multi step synthetic approach with 60-80% selectivity, a novel family of hydrofluoropolyethers (HFPEs) characterized by a macromeric perfluoropolyether (PFPE) body end-capped, on one or both sides, by a 1,1-difluoroethoxy group. We synthesized these HFPEs trough an apparently conventional hydrogenation of PFPE precursors end-capped by reducible acyl halide groups and subsequent Cl cleavage by hydrogen, promoted by UV light in presence of hydrogen radical donor or by a metal catalytic system in presence of H₂. The physico-chemical properties of these HFPEs were described and compared to those of similar perfluorinated or partially hydrogenated molecules, obtaining master curves of general validity when temperature dependent properties, like viscosity, were compared under temperature reduced condition. The contribution of the end-groups to the specific property, vanishing at a sufficient high molecular weight, was demonstrated more and more important at the lowest oligomerization degrees.     

Development and Optimization of a Procedure for the Determination of Indium-Tin Oxide Particle Size and Concentration in Cellular Media

Indium-tin oxide (ITO) is a solid mixture often comprised of approximately 90% indium oxide and 10% tin oxide by weight. ITO is employed as a transparent conductive coating for flat panel, liquid crystal, and plasma displays and is typically deposited after sintering as a thin film on a substrate through a variety of processes. Unfortunately, there have been published reports of workers who have been adversely impacted through exposure to this compound. When these reports are coupled with the industrial utility of ITO, future toxicological investigations are likely. Comprehensive characterization of ITO test materials would be an essential component of these studies. Ideally, characterization would include assessment of ITO particle size as administered during dosing because this physicochemical parameter can significantly impact solubility. The objective of this task was to develop, optimize, and apply a dynamic light scattering (DLS) sample preparation and measurement protocol for determination of particle size for a suite of sintered/non-sintered ITO samples prepared in cellular growth media at nominal 0.3 mg/mL doses. Sonication time was evaluated from 15 to 90 minutes over a 24-hour, continuous DLS measurement period. Resulting suspensions from samples subjected to 30 minute sonication times were stable with respect to hydrodynamic particle size between 10 and 24 hours after sonication. Throughout the 24-hour DLS measurement period, suspension aliquots were analyzed by inductively coupled plasma mass spectrometry to determine indium concentration. The developed protocol enabled investigators to use ITO suspensions of known hydrodynamic particle size and concentration in their in vitro cellular study.     

Acetonitrile - 2-Methyl-Propan-1-ol and Acetonitrile - 2-Methyl-Propan-2-ol Binary Mixtures and their Physicochemical Properties

The 1 H-NMR spectra of liquid binary mixtures of acetonitrile with 2-methyl-propan-1-ol (i-BtOH) and 2-methyl-propan-2-ol (t-BtOH), were recorded at 298 K over almost the whole range of mixed solvent compositions. From these data the values of spectral parameters, j i (ACN-i-BtOH) and j i (ACN-t-BtOH) were found. The relative permittivities ( k 12 ) and the densities ( d 12 ) of the mixed solvents were measured at 288.15 K, 293.15 K, 298.15 K, 303.15 K and 308.15 K. The experimental data were used to test some empirical equations of the type: y 12 = y 12 ( t ) and y 12 = y 12 ( X 1 ) [where: y 12 = d 12 or k 12 ]. From all these data, the deviations from ideality molar volumes , temperature coefficients of relative permittivities ( f 12 ) and the excess extrathermodynamic parameters were calculated. The values of these structural parameters are discussed in terms of interactions of acetonitrile with both alcohols.     

甲醇对1-丁基-3-甲基咪唑四氟硼酸离子液体结构与性质影响的模拟研究

采用分子动力学模拟方法研究了298.15 K、0.1 MPa下摩尔分数为0.1-0.9 的甲醇对1-丁基-3-甲基咪唑四氟硼酸盐([BMIM][BF₄])结构与性质的影响. 获得了体系的密度、径向分布函数、配位数、自扩散系数、粘度和电导率, 模拟得到的密度值与实验值符合较好. 结果显示: 体系各组分之间的径向分布函数随甲醇摩尔分数的增加呈规律性变化; 体系内阴阳离子的自扩散系数随着甲醇摩尔分数的增加不断增大; 甲醇的加入削弱了阴阳离子之间的相互作用, 体系粘度随着甲醇摩尔分数的增加逐渐减小, 电导率不断增大. 分析空间分布函数得到体系中各组分的三维空间分布情况.     

Analytical tools for the physicochemical profiling of drug candidates to predict absorption/distribution

The measurement of physicochemical properties at an early phase of drug discovery and development is crucial to reduce attrition rates due to poor biopharmaceutical properties. Among these properties, ionization, lipophilicity, solubility and permeability are mandatory to predict the pharmacokinetic behavior of NCEs (new chemical entities). Due to the high number of NCEs, the analytical tools used to measure these properties are automated and progressively adapted to high-throughput technologies. The present review is dedicated to experimental methods applied in the early drug discovery process for the determination of solubility, ionization constants, lipophilicity and permeability of small molecules. The principles and experimental conditions of the different methods are described, and important enhancements in terms of throughput are highlighted. Figure Scheme of the Drug Research Process.