The Problem of Estimating the Uncertainty of the Fixed Point Temperature Due to the Presence of Impurities

The main problems in estimating the uncertainty due to the presence of impurities in the material: the absence in the documents of a unique definition of the quantity being measured – the fixed point temperature, the lack of agreed methods of realizing the fixed points and the insufficient justification of the equations used for the estimate, are analyzed. The results of a measurement of the melting point of gallium are presented, which differ in the conditions in which they were realized – with one and two liquid-solid interfaces and different solidification conditions, are presented. The reasons for the considerable difference between the values of the temperatures obtained in these experiments are discussed.     

Synthesis of p‐aminophenol from the hydrogenation of nitrobenzene over metal–solid acid bifunctional catalyst

BACKGROUND: A single‐step conversion of nitrobenzene (NB) to p‐aminophenol (PAP) through catalytic hydrogenation is a widely used synthesis route for PAP. The main shortcoming of this route is the use of sulfuric acid for rearrangement of the phenylhydroxylamine (PHA) intermediate. In this paper, S₂O₈^2?/ZrO₂ (PSZ) solid acid and Pt‐S₂O₈^2?/ZrO₂ (Pt‐PSZ) bifunctional catalysts were prepared for the synthesis of PAP in non‐acid medium. RESULTS: Calcination temperature has a substantial effect on the acidity, structure and activity for PHA rearrangement of PSZ. The highest PAP yield was 33.8% over PSZ calcined at 823 K when the reaction was carried out in water at 423 K. A high PAP yield of 23.9% was achieved by a single‐step reaction of nitrobenzene over Pt‐PSZ bifunctional catalysts. CONCLUSION: PSZ solid acid exhibits high activity for PHA rearrangement. Perfect tetragonal ZrO₂ and much stronger acid sites play important roles in catalytic activity. Inhibiting the hydrogenation activity by reducing the amount of Pt loading on Pt‐PSZ can improve the competition of PHA rearrangement on acid sites with hydrogenation of PHA on metal active sites, resulting in better selectivity to PAP. Copyright © 2008 Society of Chemical Industry     

Growth and morphology of nanometer LiMn2O4 powder

The growth of Li_1+xMn₂O₄ via detonation reaction was investigated with respect to the presence of an energetic precursor, such as the metallic nitrate and the degree of confinement of the explosive charge. The detonation products were characterized by scanning electron microscopy. Powder X-ray diffraction and transmission electron microscopy were used to characterize the products. Li_1+xMn₂O₄ with 1-2 μm spherical morphology and more uniform secondary particles, but with smaller primary particles of diameters from 20 to 60 nm and a variety of morphologies were found. The oxides produced by this cheap method affirmed the validity of detonation synthesis of nano-size powders.     

FEM model of the ohmic resistance of IP-SOFCs

In the present work, the ohmic resistance of an integrated planar-SOFC (IP-SOFC) has been evaluated by developing a model whose equations have been solved numerically through an FEM method. The model allows to estimate the distribution of voltage and current density in the cell. A comparison between simulated and experimental data of area specific resistance is reported, which shows satisfactory agreement. The mathematical model has also been used to carry out some parametric studies for optimisation purposes. Indeed, a reduction in cell pitch length and an increase in electrode thickness are predicted to lead to a reduction in ohmic losses in IP-SOFCs.     

Synthesis and characterization of a novel proton‐exchange membrane for fuel cells operating at high temperatures and low humidities

The synthesis of a p‐toluidine/formaldehyde (PTF) resin was performed, and the effects of the molar ratio of the individual monomers and the polymerization conditions on the structure of the PTF resin were studied. Fourier transform infrared and ¹³C‐NMR spectra were used to characterize the PTF. Wide‐angle X‐ray diffraction patterns revealed the crystalline structures of various PTFs. Polarized optical microscopy revealed that the molar ratio of the monomers had a strong effect on the crystalline morphologies. A longer polymerization time turned out a polymer with a higher intrinsic viscosity and molecular weight, which led to differences in the proton conductivity. All of the PTFs showed a higher proton conductivity than a commercial Nafion membrane at 90–100°C and 0% relative humidity. The proton conductivity of the PTF series could be improved by sulfonation with sulfuric acid and could be maintained after blending with polyurethane. Pure methanol could be used as a fuel source because of the insolubility and nonwetting properties of PTF in methanol to increase the output current density for a PTF membrane electrode assembly. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Nonpathological Lyapunov functions and discontinuous Carathéodory systems

Differential equations with discontinuous right-hand side and solutions intended in Carathéodory sense are considered. For these equations, sufficient conditions which guarantee both Lyapunov stability and asymptotic stability in terms of nonsmooth Lyapunov functions are given. An invariance principle is also proven.     

固体超强酸S_2O_8~(2-)/SnO_2-SiO_2催化合成环己酮1,2-丙二醇缩酮

采用沉淀-浸渍法制备了固体超强酸S2O28-/SnO2-SiO2,以它为催化剂催化环己酮和1,2-丙二醇合成了环己酮1,2-丙二醇缩酮;考察了带水剂种类及用量、酮醇摩尔比、催化剂用量、反应时间对产品收率的影响,并用正交实验对反应条件进行了优化。实验结果表明,适宜的反应条件为:n(环己酮)∶n(1,2-丙二醇)=1∶1.6、催化剂用量为反应物料总质量的2.0%、带水剂环己烷用量5.0mL、反应时间50min。在此条件下,环己酮1,2-丙二醇缩酮收率达到91.47%;催化剂的稳定性良好,在重复使用5次后环己酮1,2-丙二醇缩酮收率为82.20%,活性下降的主要原因为催化剂表面积碳和吸附了有机物;经傅里叶变换红外光谱和气相色谱质谱分析表明,产物为环己酮1,2-丙二醇缩酮,纯度为100%。     

用热分析法研究硝化棉的熔化过程

用ＭＤＳＣ，显微镜温台熔点测定仪和固体原位反应池／快速扫描傅立叶变换红外光谱联用装置考察了硝化棉的熔化过程。ＭＤＳＣ曲线表明吸热过程是可逆的，它系由ＮＣ和部分分解凝聚相产物的混合物的固液相变所引起。由ＮＣ的ＭＤＳＣ曲线得到的熔点，熔化含，熔化熵，分解含和分解反应热温熵分别为４７６．８４Ｋ，２０５．６Ｊ．ｇ＾－１，０．４３１２Ｊ．ｇ＾－１．Ｋ＾－１，－２４７５．０Ｊ．ｇ＾－１，－５．２４２Ｊ．ｇ＾－     

液相对流对固液界面稳定性的影响

以模型合金丁二腈－乙醇的强制性晶体生长为基础，利用自行研制的液相对流驱动装置，详细考查了液相自然对流及强迫对流作用下，模型合金平界面失稳的动态生长过程，证实了液相的流动加快了液相温度与浓度分布的均匀化，从而增强了液／固界面的稳定性。并且随流动速度的增加，界面稳定性提高。     

聚氧乙烯 - 聚氧丙烯 - 聚苯乙烯多嵌段聚合物的力学和导电性能研究

研究了聚苯乙烯含量对聚氧乙烯－聚氧丙烯－聚苯乙烯多嵌段聚合物的力学性能及其与ＬｉＣｌＯ４络合物的离子导电性能的影响；并以电导率较高的络合物为电解质，Ｎａ１＋ｘＶ３Ｏ８复合物和Ｌｉ片分别为正、负极组装了薄型锂电池并测定其放电性能。