氮掺杂多壁纳米碳管的合成和定量表征

 采用化学气相沉积法制备了 N 掺杂多壁纳米碳管, 并运用透射电子显微镜、N2 物理吸附、热重-差示扫描量热、程序升温氧化和 X 射线光电子能谱等手段对样品进行了表征. 结果表明, 纯化处理的纳米碳管表面 N 含量为 4.2%, 其中包括吡啶、己内酰胺、氧化吡啶、吡啶酮和吡咯等含氮官能团. 研究了各种含氮官能团燃烧的动力学行为. N 原子掺杂进入碳管的石墨结构中, 提高了表面碱性, 有可能用于催化与能源转化领域. 另外, 本文提供了一种可用于场发射器件的杯状闭合结构纳米碳合成方法.     

Synthesis and Crystal Structure of a New Zn(Ⅱ) Complex Exhibiting Strong Luminescence

The title complex,[Zn(ip)2(H2O)2][ZnCl4]·H2O·2DMF 1(ip=imidazo[4,5-f][1,10] phenanthroline),has been synthesized via the slow evaporation of concentrated reaction solution at room temperature.It was characterized by single-crystal X-ray diffraction.Crystal data for C32H36Cl4N10O5Zn2:white prism,0.17mm×0.15mm×0.10mm,monoclinic,space group P2/c,a=11.928(8),b=9.868(6),c=16.520(11),β=104.879(12)°,V=1879(2)3,Z=2,Mr=913.25,Dc=1.614 g/cm3,F(000)=932,μ=1.616 mm-1,λ(MoKα)=0.71073,GOOF=1.045,R=0.0710 and wR=0.1755 for 3055 observed reflections with Ⅰ2σ(Ⅰ).X-ray diffraction study reveals that the title complex has an interesting 3D architecture via hydrogen bonding interactions and π-π interactions.The IR,TGA,XRD and luminescent properties of complex 1 were also studied.     

SYNTHESIS AND CHARACTERIZATION OF POLY(PHTHALAZINONE ETHER PHOSPHINE OXIDE)S BY N―C COUPLING REACTION

<正>Based on several unsymmetrical,twist,noncoplanar phthalazinone-containing monomers 2a-2e and an active bis(4-fluorophenyl)phenyl phosphine oxide(BFPPO) monomer,a series of novel poly(phthalazinone ether phosphine oxide)s (PPEPO) was synthesized by anhydrous K_2CO_3 mediated N—C coupling reaction in DMAc.The polymers exhibited good thermal properties with T_gs ranging from 267℃to 306℃and 5%weight loss temperatures in nitrogen higher than 430℃, together with high char yield upon prolonged heating at 800℃(35%—56%).Moreover,the polymers were readily soluble in common organic solvents,such as N-methyl-2-pyrrolidone,chloroform and m-cresol.These polymers had inherent viscosities in the range of 0.45-0.72 dL/g and could be cast into flexible and colorless films by spin coating or casting approach.     

土壤颗粒表面电场作用下固-液界面Mg2+-K+与Ca2+-K+交换动力学的比较研究

通过恒流法研究了不同表面电场作用下Mg2+、Ca2+吸附动力学. 结果发现: (1)实验初期阶段是强静电力作用下的零级动力学过程和一定反应时间后的弱静电力作用下的一级动力学过程, 且零级速率过程和一级速率过程之间存在明显的转折点; (2)不同电解质构成中Ca2+的吸附速率明显快于Mg2+的, 平衡吸附量也大于Mg2+的, 且Ca2+在土壤颗粒表面的覆盖度比Mg2+在土壤颗粒表面的覆盖度高; (3)离子的相对有效电荷系数与土壤颗粒表面电场作用的不同是各体系中Ca2+、Mg2+吸附动力学有差别的根本原因; (4)根据离子吸附的理论模型可以分别计算出速率系数、平衡吸附量、离子在土壤颗粒表面的覆盖度以及固定液的体积, 这些参数可以定量评估土壤颗粒表面电场对离子吸附动力学的影响.     

N—O键解离焓的密度泛函理论研究

在高精度计算方法G3和G3B3的基础上,比较了密度泛函理论(DFT)十几种方法对N—O键解离焓(BDE)相对于实验值的计算精度,发现用B3P86方法计算15种化合物N—O键的BDE,均方根误差最小,仅为6.36kJ·mol-1,计算值与实验值的线性相关系数为0.991.在此基础上,用该方法分别计算了非芳香化合物及芳香化合物的N—O键BDE.通过自然键轨道分析,发现部分N—O键的BDE与N—O键的键长、原子电荷密度及键级之间存在定量关系.此外,在B3P86方法的基础上预测了几种典型的杂环芳香化合物N—O键BDE值.     

利用水热法制备氧化锌微米球

利用水热法制备出具有特殊形貌的ZnO微米球.利用X射线粉末衍射仪(XRD)和扫描电镜(SEM)对ZnO进行了表征.     

Effect of isothermal annealing on degree of crystallinity and mechanical properties of poly(l‐lactide‐co‐glycolide)

We investigated the effect of isothermal annealing on the degree of crystallinity and mechanical properties of a random copolymer‐poly(l‐lactide‐co ‐glycolide) (PLLGA)‐with monomer molar ratios of 85/15 (PLLGA85/15) by performing polarizing optical microscopy, differential scanning calorimetry, and X‐ray diffraction, and studying the tensile properties. Isothermal annealing of PLLGA at 130 °C was conducted to improve the degree of crystallinity of the copolymer; the maximum degree of crystallinity (44.5%) was achieved after 60 min of annealing. The crystal size/perfection was observed to increase with annealing time. The highest tensile strength of 65.8 MPa was achieved after 80 min of annealing. However, the degree of crystallinity and tensile strength can only reach to certain extent. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

疏水介孔SiO2的制备与性能表征

以廉价的工业级正硅酸乙酯为原料,经过酸碱两步催化制备二氧化硅凝胶,以三甲基氯硅烷/六甲基二硅氧烷混合液对凝胶进行直接表面改性,常压干燥下得到高比表面积疏水性二氧化硅气凝胶.用SEM、IR、N2吸脱附、TG-DTA、接触角的测定等分析方法对二氧化硅化学成分、结构形貌、比表面积、热稳定性和疏水性能进行了研究.结果表明,经改...     

铈(V)与左旋多巴的荧光反应及其分析应用

研究了左旋多巴与Ce(Ⅳ)在碱性体系中的荧光特性.实验发现,左旋多巴具有弱的内源性荧光,在pH为9.15的伯瑞坦-罗比森Britton-robinson(BR)缓冲介质中可与Ce(Ⅳ)发生反应,使其荧光强度显著增强,据此提出了测定左旋多巴含量的荧光分析新方法.左旋多巴含量在0.08-3.6μg/mL范围内与其荧光强度呈...     

气相色谱法测定缩水甘油丁酸酯

采用气相色谱快速分析方法测定环氧氯丙烷反应体系中的缩水甘油丁酸酯.采用SE-30( φ3mm×1.5mm)填充柱,载气流量:48.86mL/min;柱温:100℃;气化室温度:185℃;热导检测器温度185℃;缩水甘油丁酸酯的量(x)与峰面积(y)有良好的线性关系; y=1594.1x+1370.1,R2=0.9993...