Preparation of modified fly ash hollow glass microspheres using ionic liquids and its flame retardancy in thermoplastic polyurethane

Diphenyl sulfide was oxidized to sulfoxide and sulfone over V-doped TiO₂ using a 30% solution of H₂O₂. The TiO₂ samples with different intended content of vanadium (0.02, 0.05, 0.1 and 0.18 mass%) were prepared by incipient wetness impregnation. Physicochemical properties of the V-doped TiO₂ were characterized by chemical analysis (ICP-OES), X-ray diffraction (XRD/in situ HT-XRD), UV–Vis diffuse reflectance spectrometry (UV–Vis DRS), N₂-sorption measurements, electron paramagnetic resonance and cyclic voltammetry. Both vanadium oxide loading and calcination temperature influenced the structure of the V-TiO₂ samples. Vanadium species deposited on TiO₂ decreased temperatures required for anatase to rutile phase transformation. The V-TiO₂ samples were found to be efficient catalysts for oxidation of sulfides to sulfones. The sample with the lowest vanadium content (0.02VTiO₂) presented among the studied catalysts the best catalytic properties with respect to high conversion of diphenyl sulfide to diphenyl sulfonate. An increase in vanadium loading resulted in decrease in catalytic activity of the samples. Also non-modified TiO₂ presented significantly lower catalytic activity in comparison with 0.02VTiO₂. This interesting effect was related to the formation of highly dispersed vanadium species catalytically active in Ph₂S oxidation in the case of the samples with lower V-content. An increase in vanadium loading results in the formation of more aggregated V-species inactive, or less active, in the process of diphenyl sulfide oxidation.     

增压空冷器用开缝翅片的结构优化设计

利用粒子图像测速技术和红外热成像技术,对增压空冷器用圆弧型和X型开缝翅片空气侧的流动和传热特性进行了可视化实验研究．在实验的雷诺数（800-3400）范围内,得到了阻力和换热特性曲线,以及能反映流动和传热微观特性的流场和温度场．实验结果表明,圆弧型开缝翅片的阻力小于X型开缝翅片,并且前者在强化圆管背风侧的换热特性方面优于后者,但后者整体的场协同性和换热性能优于前者．结合两种翅片的优点,优化设计出了一种新型的开缝翅片（X圆弧型）．对3种开缝翅片的流动和换热特性进行了数值模拟。模拟结果与实验结果吻合得很好．模拟结果表明,优化后的X圆弧型开缝翅片的场协同性、换热性能均优于前两种翅片．新翅片在考虑了阻力因素后的综合换热性能较圆弧型开缝翅片提高了7％～15％,较X型开缝翅片提高了3％～9％．     

In vitro corrosion of Mg–1.21Li –1.12Ca –1Y alloy

The influence of the microstructure on mechanical properties and corrosion behavior of the Mg–1.21Li–1.12Ca–1Y alloy was investigated using OM, SEM, XRD, EPMA, EDS, tensile tests and corrosion measurements. The results demonstrated that the microstructure of the Mg–1.21Li–1.12Ca–1Y alloy was characterized by α-Mg substrate and intermetallic compounds Mg2 Ca and Mg24Y5. Most of the fine Mg2 Ca particles for the as-cast alloy were distributed along the grain boundaries, while for the as-extruded along the extrusion direction. The Mg24Y5 particles with a larger size than the Mg2 Ca particles were positioned inside the grains. The mechanical properties of Mg–1.21Li–1.12Ca–1Y alloy were improved by the grain refinement and dispersion strengthening. Corrosion pits initiated at the α-Mg matrix neighboring the Mg2 Ca particles and subsequently the alloy exhibited general corrosion and filiform corrosion as the corrosion product layer of Mg(OH)2and Mg CO3 became compact and thick.     

Enolic Schiff-base aluminum complexes and their application in lactide polymerization

A series of NNOO-tetradentate enolic Schiff-base ligands were prepared where ligand L₁ = bis(benzoylacetone)propane-1,2-diimine, L₂ = bis(acetylacetone)-propane-1,2-diimine, L₃ = bis-(acetylacetone)cyclohexane-1,2-diimine. Their further reaction with aluminum tris(ethyl) formed complexes LAlEt (1a, 2a and 3a). The solid structure of complexes 1a, 2a and 3a confirmed by X-ray single crystal analysis manifested that these complexes were all monomeric and five-coordinated with an aluminum atom in the center. The configurations of these complexes varied from trigonal bipyramidal geometry (tbp) to square pyramidal geometry (sqp) due to their different auxiliary ligand architectures. ¹H NMR spectra indicated that all these complexes retained their configuration in solution states. Their catalytic properties to polymerize racemic-lactide (rac-LA) in the presence of 2-propanol were also studied. The diimine bridging parts as well as the diketone segment substituents had very close relationship with their performance upon the polymerization process. All these complexes gave moderately isotactic polylactides with controlled molecular weight and very narrow molecular weight distributions.     

杂多酸引发四氢呋喃开环聚合反应 Ⅳ.以环氧丙烷为促进剂

对杂多酸引发四氢呋喃开环聚合的研究从八十年代中期开始已有不少报道［１～４］,其引发聚合的活性低,当杂多酸浓度低时,聚合反应时间长,产物分子量高;而为制得工业通常使用的中等分子量四氢呋喃聚醚二醇,需要加大量的引发剂,且聚合收率低（最高仅为３５％）．针对以上问题,本实验室曾对以环氧乙烷（ＥＯ）促进低浓度十二磷钨杂多酸Ｈ３ＰＷ１２Ｏ４（ＰＷ１２）引发四氢呋喃开环聚合反应进行了系统的研究［５,６］,发现ＥＯ对ＴＨＦ聚合具有良好的促进效果,制得中等分子量聚醚二醇,转化率达到６０％以上．本文进一步研究了环氧…     

十二烷基聚氧乙烯硫酸钠胶束体系的流变性质研究

用流变学方法研究了无机电解质KBr存在时,阴离子表面活性剂十二烷基聚氧乙烯(3)硫酸钠(SDES)水溶液中胶束的生长和结构。通过测量体系的稳态剪切粘度(η)和应力(σ)关系,得到零剪切粘度(η0)、复合粘度(|η^*|)、动态模量[储能模量(G')和损耗模量(G")、平台模量(G0)、结构松驰时间(τ)等流变学参数,并应用Cox-Merz规则和Cole-Cole图,发现在SDES/KBr体系中可以形成蠕虫状胶束网络结构,体系为假塑性流体,偏离Maxwell模型,具有非线性粘弹性,没有单一的结构松驰时间。     

Simultaneous determination of bisphenols,benzophenones and parabens in human urine by using UHPLC-TQMS

An analytical method for the simultaneous determination of six bisphenols, five benzophenones and seven parabens by using ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry was developed and applied for human urine sample analysis.     

一种共轴微通道反应器设计及单分散生物质聚合物微珠的可控制备

采用不同尺寸的聚四氟乙烯(PTFE)微管为内外管、玻璃毛细管(glass capillary)或聚丙烯(PP)中空纤维为内管管头设计制作了一种共轴微通道反应器(N-CAMFR).以聚乳酸(PLA)/二氯甲烷(CH2Cl2)溶液和海藻酸钠(Na-alginate)水溶液分别作为分散相,在N-CAMFR内形成O/W和W/O乳液后,收集乳液并使其中的液滴固化,制备出单分散的生物质聚合物微珠(BPM).研究了固定管头尺寸时,改变连续相的流速及表面活性剂的种类对微珠尺寸的影响.结果表明,使用N-CAMFR制备微珠,反应过程流畅,所制得的微珠粒径分布均匀,其分散系数(f)可低至2.16%;通过改变内管管头的尺寸可方便地调控N-CAMFR的尺度,与传统微通道反应器相比,降低制作成本的同时拓宽了其应用的范围,而且降低了微通道反应器堵塞的几率.为粒径范围200~800μm的单分散聚合物微珠的可控连续制备提供了快捷绿色的新方法.     

Interaction of multi-podal open-chained compounds with anions

Six kinds of naphthyl urea and thiourea podands were designed and synthesized. The interaction between these compounds and various guest anions are studied in molecular level via absorption, fluorescence and 1H NMR spectra. The experiments show that tri-podal urea or thiourea host can bind H2PO4-or HSO4-selectively and form a host-guest complex thus inducing a change in photophysical properties of host molecule. Through comparison between urea and thiourea compounds used as host molecules, the stability constants and stoichiometry of the complexes have been determined. The binding manner and possible structures of them have been proposed.     

STUDIES ON THERMOTROPIC LIQUID CRYSTALLINE COPOLYESTERS——POLY (ARYLENE TEREPHTHALATE-CO-BUTYLENE TEREPHTHALATE)

A series of copolyesters based on bis(4-hydroxybutyl) terephthalate, terephthaloyl chloride andvarious aromatic diols (i.e. hydroquinone, chlorohydroquinone, bromohydroquinone or dihydroxybi-phenyl) was prepared. ~1H-NMR studies revealed that the monomer units had microstructures closeto random distribution in the chains. The copolymers showed composition-dependent liquid crystal-line properties as verified by visual observation of stir opalescence, polarizing microscope, DSC andX-ray diffration. The copolyesters with aromatic diol contents over a certain extent (for chloro-hydroquinone m≥0.33) were thermotropic with wide liquid crystalline temperature ranges. Theintroduction of chlorohydroquinone into the copolyesters could gradually destroy the crystallinityof the polymers but retain the liquid crystalline characteristics.