Reinforcement effect of MAA on nano‐CaCo3‐filled EPDM vulcanizates and possible mechanism

Methacrylic acid (MAA) was used as in situ surface modifier to improve the interface interaction between nano‐CaCO₃ particle and ethylene–propylene–diene monomer (EPDM) matrix, and hence the mechanical properties of nano‐CaCO₃‐filled EPDM vulcanizates. The results showed that the incorporation of MAA improved the filler–matrix interaction, which was proved by Fourier transformation infrared spectrometer (FTIR), Kraus equation, crosslink density determination, and scanning electron microscope (SEM). The formation of carboxylate and the participation of MAA in the crosslinking of EPDM indicated the strong filler–matrix interaction from the aspect of chemical reaction. The results of Kraus equation showed that the presence of MAA enhanced the reinforcement extent of nano‐CaCO₃ on EPDM vulcanizates. Crosslink density determination proved the formation of the ionic crosslinks in EPDM vulcanizates with the existence of MAA. The filler particles on tensile fracture were embedded in the matrix and could not be observed obviously, indicating that a strong interfacial interaction between the filler and the matrix had been achieved with the incorporation of MAA. Meanwhile, the presence of MAA remarkably increased the modulus and tensile strength of the vulcanizates, without negative effect on the high elongation at break. Furthermore, the ionic bond was thought to be formed only on filler surface because of the absolute deficiency of MAA, which resulted in the possible structure where filler particles were considered as crosslink points. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 1226–1236, 2006     

纳米碳酸锌的制备和热分解动力学参数的测定

Nanosized zinc carbonate was prepared in the droplet of nano-reactor based on microemusion. The influences of the concentration of the surfactant and reactant on the diameter of nanoparticles were studied and the kinetic pa-rameters of thermal decomposition reaction were determined. It can be shown from experimental results， the di-ameter of the droplet in the microemulsion which have dissolved reactant zinc nitrate and sal volatile is between 4.9nm and 7.7nm， 6.2nm and 12.4nm， respectively. Nanosized zinc carbonate prepared by the method of mi-croemusion has shown good dispersion， narrow distribution and light agglomeration. The particle size of nanosized zinc carbonate is between 5nm and 40nm， and its kinetic parameters of thermal decomposition reaction-activation energy E and reaction order n are 110kJ·mol^-1 and 0.9， respectively.     

Gas-stirred solvent extraction with propylene carbonate for separation and direct polarographic determination of thallium (III)

Gas-stirred propylene carbonate (PC) extraction can be performed by bubbling nitrogen without loss of volume. This extraction technique has proved to be highly useful for the separation and subsequent direct polarographic estimation of Tl(III) in the recovered PC phase. Tl(III) can be determined by differential-pulse polarography over the concentration range of 0.4 10 g ml^–1 without any interferences due to most metal ions such as Pb(II), Bi(III), Cu(II), Sb(III) and As(III). This proposed technique would be possible to use as a simple extraction step prior to the final estimation by instrumental method of analysis such as atomic absorption spectrometry or spectrophtometry.     

The thermal decomposition of NaHCO3 powders and single crystals

The thermal decomposition of four commercial powders and of differently stored single crystals of sodium hydrogen carbonate is studied by power compensation DSC and by optical and FT-IR microscopy. Independently of manufacturer, specified purity and price, the thermal curves of all the commercial powders show a more or less pronounced low temperature peak preceding the one due to the main decomposition. Such small peak is not observed when samples of laboratory recrystallized material are used. However the thermal behaviour of the latter preparation differs remarkably depending on storage conditions: the material kept in closed glass containers decomposes at temperatures higher than those of the material stored in a dessiccator in the presence of concentrated H₂SO₄. The observation by optical microscopy of the behaviour of the surfaces of single crystals coming from different storage conditions when the temperature is raised in a Kofler heater helps the interpretation of the data collected. The mechanism of the decomposition is discussed and the relevant kinetic parameters reported.     

酯交换法合成碳酸二苯酯用氧化铅－氧化锌催化剂的研究

 制备了一种用于苯酚与碳酸二甲酯酯交换合成碳酸二苯酯的新型氧化铅－氧化锌多相催化剂．研究了制备方法、焙烧温度、不同母体和母体配比对催化剂催化性能的影响．应用XRD，TPR和原子吸收光谱对催化剂结构进行了表征，发现Pb3O4是主活性物相，ZnO为助催化剂，并以非晶态或微晶态存在于催化剂体系中．当焙烧温度为500℃，n（Pb）／n（Zn）≈2时，催化剂的活性最高，碳酸二苯酯产率可达45．6％．考察了催化剂的重复使用效果，并对失活原因进行了探讨．     

高活性锆掺杂钴催化剂的制备及其催化甲烷燃烧性能研究

由水热法制备了掺杂锆摩尔百分比为0，10，20，30．40，50％的钴催化剂，该系列催化剂对甲烷的低温催化燃烧显示出高活性．其中，10％Zr掺杂的催化剂活性最好，可在370℃使甲烷转化率达100％．XRD分析表明，该法制得的催化剂中的活性四氧化三钴物种是由一种晶态的碳酸钴前体分解而成，Co3O4为粒径在20～40nm之问的纳米粒子．用热重分析(TG)研究了碳酸钴前体的热分解行为．     

氯化钠在球形纳米氧化铈形成过程中的作用

以水合碳酸铈为原料, 以氯化钠作为助磨剂和阻聚剂, 采用机械活化法制备了球形纳米氧化铈, 用XRD法研究了水合碳酸铈与氯化钠质量比、球磨时间、煅烧温度对CeO2粉体晶粒度的影响, 用TEM对最终产物粒子进行形貌观察. 结果表明: 在碳酸铈的球磨过程及其随后的煅烧过程中, 氯化钠的存在起到了很好的助磨和阻聚作用, 所得CeO2为类球形粒子, 分散性较好, 晶粒度约为30～50 nm.     

典型无机含氧酸自由基的特性

碳酸自由基、硝酸自由基、磷酸自由基和硫酸自由基是化学反应的重要中间体，都具有氧化性，对污染物在自然和人为环境中的迁移转化会产生重要的影响.文中较为详细地介绍这几种自由基的电极电位、产生方式、检测方法及与有机物的反应方式.总结四种自由基的特性及与有机物的反应方式可发现，四种自由基和羟自由基电极电位不同，导致它们和有机物反应速率的不同；碳酸自由基并不是羟自由基去除剂，对于一些容易被氧化的化合物，碳酸自由基氧化效果比羟自由基好；四种自由基均可由羟自由基转化而来，并且这四种自由基和羟自由基与有机物反应方式基本一致，都通过电子转移、夺氢和加成的方式进行.可以预测四种自由基和羟自由基降解有机物的机理将非常相似，今后应研究四种自由基与羟自由基相互转化的规律，以及与代表性有机物的反应机理.     

Activation of Carbon Dioxide and Synthesis of Propylene Carbonate

Cycloaddition of carbon dioxdie and propylene oxide to propylene carbonate catalyzed by tetra-tert-butyl metal phthalocyanine in the presence of tributylamine(TBA) shows higher yield than catalyzed by unsubstituted metal phthalocyanine.Comparing different catalysts of diverse metals,(t-Bu)4PcMg is more active than (t-Bu)PcFe ,But(t-Bu)4PcCo and (t-Bu)4PcNi only have low catalytic activities towards the reaction.Moreover,the yield will increase as the temperature increases.