二苯并噻吩合成方法的改进

对文献报道的由联苯和硫在AlCl3催化下反应合成二苯并噻吩(DBT方法中的提纯过程作了改进，大大简化了提纯步骤，使制备DBT的时间缩短了一半，产率为63．4％，经提纯后的成品含量达99．7％，其纯度、外观、晶相均优于进口试剂，但成本远低于进口试剂。产品用FT-IR、LRS、XRD和^1H NMR表征结果与文献报道完全相符合。     

Isotopic Oxygen Exchange and EPR Studies of Superoxide Species on the SrF2/La2O3 Catalyst

By using the in situ IR spectroscopy, the superoxide species (O₂⁻), characterized by the O–O stretching peak at 1130 cm⁻¹, was detected on the SrF₂/La₂O₃ catalyst at temperatures up to 973 K. The introduction of ¹⁸O₂ isotope caused the 1130 cm⁻¹ peak to shift to lower wavenumbers (1095 and 1064 cm⁻¹), consistent with the assignment of the spectra to the superoxide species. A good correlation between the rate of the disappearance of the O₂⁻ species and that of the formation of C₂H₄ was observed, suggesting that O₂⁻ was the active oxygen species responsible for the oxidative coupling of methane (OCM) on the SrF₂/La₂O₃ catalyst. This conclusion was reinforced by the EPR experiments (g_xx = 2.0001, g_yy = 2.0045, g_zz = 2.0685), showing that O₂⁻ was the only paramagnetic oxygen species detectable on the O₂-preadsorbed SrF₂/La₂O₃ catalyst. These results suggest that superoxide O₂⁻ can be a stable active oxygen species, whose role in the OCM reaction cannot be overlooked.     

Effect of clay on the morphology of binary blends of polyamide 6 with high density polyethylene and HDPE‐graft‐acrylic acid

Polyamide 6 (PA6)/HDPE/organo‐bentonite (Oclay) and PA6/HDPE‐grafted‐acrylic acid (PEAA)/Oclay nanocomposites were prepared via melt compounding. The influence of Oclay on the morphology of composites was investigated. Scanning electron microscopy results revealed the size of the dispersed HDPE, and PEAA phase decreased with increasing Oclay content. Transmission electron microscopy and X‐ray diffraction results revealed that the Oclay was predominately intercalated with some evidence of partial exfoliation. The majority of Oclay platelets were concentrated in the PA6 phase and in the interfacial region between PA6 and HDPE (PEAA). The Oclay platelets played the role of coupling species between the two polymers, increasing the interaction of the two phases in certain extent. These results were proved by FTIR and positron annihilation lifetime spectroscopy. Consequently, apparent emulsifying effect was induced. A schematic mechanism of the apparent compatibilization effect was presented. POLYM. ENG. SCI., 47:551–559, 2007. © 2007 Society of Plastics Engineers.     

Simulation of transient process in melting section of reciprocating extruder

Plastic injection molding machine that can be classified as reciprocating extruders are among the most widely used machines in industry. However, most studies in the injector design were based on steady state models developed for extruders that involved no reciprocation. This over-simplified model leaves out the most important aspect of reciprocation. The authors of this paper have derived a transient melting model that takes care of the change from the conventional steady extrusion to that of a discontinuous transient process. This paper describes simulations conducted on the derived model to explain observation that cannot be explained by the steady extrusion model in practical experiments. The simulation was conducted by using parameters given in Donovan's experiment [Polym Engng, 11 (1971) 353]. The simulation results are found to qualitatively match with the experimental results. It proves the validity of the model. Simulation has also been conducted with the model on materials that their viscosities are temperature and shear rate dependent. The result has shown that screw rotation speed, screw axial movement speed, barrel thickness, barrel heat capacity, temperature of heater and polymer are factors affecting the melting speed and the transient effects.     

Effect of filler network on dynamic viscoelastic properties of uncured polymethylvinylsiloxanes filled with silica and carbon black

Dynamic properties of polymethylvinylsiloxane (PMVS) filled with filler‐blends composed of carbon black (CB) and silica (SiO₂) were investigated using an advanced rheometric expansion system. A variety of weight fraction of CB to SiO₂ were 0/100, 10/90, 30/70, 50/50, 70/30, 90/10, and 100/0, and a bifunctional organsilane, bis(3‐triethoxysilylpropyl)tetrasurfane, was used to facilitate the filler dispersion. The results reveal that the incorporation of CB/SiO₂ filler‐blends into PMVS result in a reduced Payne effect. This effect reaches a minimum when the ratio of CB/SiO₂ approaches 1, and then it began to rebound with the ratio increase. Meanwhile, a characteristic Newtonian viscosity plateau appearing in low frequencies also significantly decreases, depending on the amount of CB or SiO₂ added. On the basis of a simplified Fowke model, we ascribe this phenomenon to the deteriorated filler network, which is predominantly induced by the totally different surface activity between CB and SiO₂. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 99: 3477–3482, 2006     

高层级轮胎各层帘布裁断角度的计算方法

提出一种新的确定高层级轮胎内外各层帘布裁断角度的方法。根据各层帘布在成品胎内部的材料分布图和在成型机头上的材料分布图，计算该层所在的机头宽度，比较计算的机头宽度和实际的机头宽度，通过调整帘布裁断角度使两者近似相等。以此确定各层帘布的裁断角度，达到内外层帘线均匀伸张的目的。     

陶瓷磨光弧面板的开发与应用

研究了陶瓷板材在各种温度及压力下产生的应力、应变与板材断裂之间的关系和规律,提出了陶瓷板材的弯曲方法,研制各种专用试验、生产设备,将成品陶瓷平板加工成为园柱板、弧面、球面、圆锥面、双曲面等各种曲面板.     

Thermal and kinetic properties of poly(lactic acid) and transglutaminase‐crosslinked wheat gluten blends

Wheat gluten (10 g) was crosslinked (XL) using 10 units of transglutaminase. Different blends of XL gluten and poly(lactic acid) (PLA) were mixed in a Brabender mixer at 180°C for 10 min. Neat PLA and blends were analyzed using modulated DSC (MDSC). Neat PLA displayed a glass transition (T_g) and exothermic (Cry) followed by endothermic (Mel) transitions. The profile showed a T_g of 0.46 J/g/°C, Cry with 29.9 J/g, whereas Mel exhibited 28.7 J/g. XL wheat gluten displayed one T_g with 0.45 J/g/°C. Samples were subjected to repeated heating and cooling cycles to show the level of compatibility between the two polymers. The activation energy (E_a) and pre‐exponential factor (Z) were determined according to Borchardt and Daniels (B/D) kinetics approach. The blends showed increased E_a values with an increase in the amount of XL gluten. In the presence of 5 and 20% XL gluten, the E_a of PLA increased from 150 to 200 kJ/mol, respectively. A higher number of cycles caused an increase in E_a. The T_g temperature of different PLA/XL gluten blends can be predicted by Gordon–Taylor equation and its modified forms. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Synthesis and Morphology of TiO2 Nanotube Arrays by Anodic Oxidation Using Modified Glycerol-Based Electrolytes

Titanium dioxide (TiO₂) nanotube arrays were prepared by electrochemical anodization of titanium sheets in the glycerol 176 mL/H₂O 44 mL/NH₄F 0.5 wt% electrolytes modified with H₂SO₄ and NaAc addition. The surface morphologies, average inner diameter, and the length of the nanotube arrays changed with the solution pH in the range from 5.6 to 4.0 by adding H₂SO₄. A uniform surface morphology of the nanotubes with average inner diameter of ∼80 nm and a length of ∼1000 nm was obtained when the solution pH was 5.0. The growth rates of the nanotubes were remarkably enhanced by NaAc addition in the range of 0.04–0.14 M . With NaAc addition of 0.10 M , the length of the nanotube arrays reached 4.16 μm after an 8-h anodization, increasing 3.23 μm compared with no NaAc addition. The relationship between solution pH and growth of TiO₂ nanotubes was analyzed by current–time curves, solution electrical conductivities, and scanning electron microscopy (SEM), and the role of NaAc was also discussed based on SEM and solution electrical conductivities.     

Nanocrystalline CeO2 in SBA-15: Performance of Pt/CeO2/SBA-15 Catalyst for Water-gas-shift Reaction

CeO₂ particles confined within the pores of an SBA-15 mesoporous silica host were prepared by incipient wetness impregnation (IMP) and deposition precipitation (DP) methods. The materials were characterized by XRD, N₂-adsorption and temperature programmed reduction (TPR) to evaluate the structure, texture, and redox properties. The preparation procedure had significant impact on the assembling mode of CeO₂ inside the SBA-15 mesopores. A high dispersion of CeO₂ particles was achieved via DP, whereas the dispersion of CeO₂ prepared by IMP was found to be inhomogeneous and CeO₂ partially blocked the pores. The CO conversion in the water-gas-shift reaction was enhanced over 1 wt% Pt supported on CeO₂-modified SBA-15 obtained by DP.