具有新结构类型的化合物CsIn[PO3(OH)]2的合成与结构(英)

水热法合成了新结构类型化合物CsIn[PO₃(OH)]₂，并通过单晶X-射线衍射表征结构。标题化合物空间群为P1 2₁/c 1 (No.14)，晶体学参数为：M_r=439.69，mP56，a=0.532 86(6) nm，b=0.916 53(7) nm，c=1.478 39(14) nm，β=93.849(9)°，V=0.720 4(1) nm³，Z=4，D_x=4.054 g·cm^-3，μ=8.713mm^-1，F(000)=800，R₁= 0.032 5，wR₂=0.087 4。在该化合物中，2个InO₆八面体和4个PO₄四面体形成交连的六元环柱，并沿a轴方向形成近六方密堆积并连接成Cs⁺离子占据的十二元环结构隧道，六元环和十二元环连接构筑了三维网络结构。与类似化学计量比化合物Na₂In₂[PO₃(OH)]₄·H₂O比较，标题化合物中十二元环的形成明显取决于隧道阳离子的大小，其拓扑构造可看作扩展的6，3-网格连接，化合物 RbIn[PO₃(OH)]₂与之同构。     

FeSb2纳米棒的溶剂热合成与电化学脱嵌锂性能

用溶剂热法合成了作为一种新型锂离子电池负极材料的FeSb2纳米棒. 高分辨透射电镜(HRTEM)观察表明, FeSb2纳米棒的直径为20～40 nm, 长度为0.2～1.0 μm. 恒流充放电测试和循环伏安测试显示, FeSb2纳米棒首次可逆容量达到543 mAh•g−1, 经过10次循环后, 可逆容量保持在353 mAh•g−1. 虽然首次库仑效率仅为64%, 但仍明显优于FeSb2纳米颗粒, 并在10次循环后基本稳定在90%. FeSb2纳米棒在循环过程中仍可能发生粉化和破裂, 导致电极逐渐失效.     

喷气燃料中抗氧剂2,6-二叔丁基对甲酚的高效液相分析

 采用高效液相法分析喷气燃料HDF 1中的抗氧化剂 2 ,6 二叔丁基对甲酚 (简称BHT)含量 ,研究了二元混合流动相中甲醇 乙酸缓冲液的比例对燃料主体和BHT分离效果的影响 ,选择了最佳分离条件 (甲醇所占体积分数为 85 % ,流速为 1mL/min) ,在此条件下 ,可测出质量分数为 1× 10 -5的BHT。用该喷气燃料配制了BHT质量分数在 2 0× 10 -6到 12 0× 10 -6之间的标准溶液 ,考察了BHT质量分数与峰面积之间的关系 ,结果表明线性关系良好。     

超顺磁性Fe3O4@SiO2复合纳米粒子的制备、表征和性能研究

采用化学共沉淀法制备了超顺磁性Fe3O4纳米粒子,用改进的Stber方法在Fe3O4纳米粒子外面包覆一层SiO2。采用IR、XRD、SEM、PPMS等方法对Fe3O4纳米粒子和Fe3O4@SiO2复合纳米粒子进行了表征。分析研究了Fe3O4@SiO2复合纳米粒子的磁学性能和热稳定性。结果表明:Fe3O4@SiO2复合粒子比Fe3O4纳米粒子有更好的热稳定性和分散性。Fe3O4@SiO2复合粒子的饱和磁化强度(Ms)随着正硅酸乙酯(TEOS)浓度的升高而下降,随着氨水浓度的升高而先增加再减小,呈线性依赖关系。且Fe3O4纳米粒子在600℃热处理3h后已经完全转化为Fe2O3,复合粒子在800℃热处理后仍然只显示Fe3O4的物相。     

PIV measurements of turbulent jets issuing from triangular and circular orifice plates

The present study experimentally investigated the near-field flow mixing characteristics of two turbulent jets issuing from equilateral triangular and circular orifice plates into effectively unbounded surroundings,respectively.Planar particle image velocimetry(PIV) was applied to measure the velocity field at the same Reynolds number of Re=50,000,where Re = UeDe /with Ue being the exit bulk velocity and the kinematic viscosity of fluid,D e the equivalent diameters.The instantaneous velocity,mean velocity,Reynolds stresses were obtained.From the mean velocity field,the centreline velocity decay rate and half-velocity width were derived.Comparing the mixing characteristics of the two jets,it is found that the triangular jet has a faster mixing rate than the circular counterpart.The triangular jet entrainments with the ambient fluid at a higher rate in the near field.This is evidenced by a shorter unmixed core,faster Reynolds stress and centreline turbulence intensity growth.The primary coherent structures in the near field are found to break down more rapidly in the triangular jet as compared to the circular jet.Over the entire measurement region,the triangular jet maintained a higher rate of decay and spread.Moreover,all components of Reynolds stress of the triangular jet appear to reach their peaks earlier,and then decay more rapidly than those of the circular jet.In addition,the axis-switching phenomenon is observed in the triangular jet.     

螯合稀土金属标记蛋白质技术的建立与优化

建立了一种基于螯合稀土金属标记蛋白质的技术,优化了影响标记效率的各种条件.在50 mmol/L TEAB缓冲体系(pH 7.5),DTPA与肽段摩尔比为100: 1,常温反应30 min的条件下,DTPA标记完全;在100 mmol/L乙酸铵缓冲液(pH 6.0),稀土金属与DTPA摩尔比为4: 1,37 ℃反应1 h的条件下,稀土金属螯合反应完全.考察了不同稀土金属的螯合效率,发现离子半径最小的Lu螯合效率最高.本方法被成功应用于肽混合物标记.     

Diels-Alder Addition of Dicyclopentadiene with Cyclopentadiene in Polar Solvents

Diels-Alder addition of dicyclopentadiene and cyclopentadiene in polar solvents has been studied to produce tricyclopentadiene（TCPD） that is a potential high-density fuel precursor. GC and MS analysis shows that the adducts contain two isomers, namely exo- and endo-TCPD. Theoretical simulation shows that although the transition state of endo-TCPD has a lower activation energy, exo-TCPD is thermodynamically preferred. Polar solvents can accelerate the reaction rate and improve the exo/endo ratio of TCPD because the transition state of exo-TCPD has a higher polarity than that of endo-TCPD. The solvent effect follows the order of polarity： benzyl methanol〉cyclohexanone〉toluene. The conversion rises when the temperature ranges from 120 to 150 ℃, but the selectivity of TCPD slightly decreases. Increasing the pressure can improve the conversion but the exo/endo ratio of TCPD is unchanged. The apparent kinetics in different solvents was determined via nonlinear regression. The activation energies are 99.47, 101.15, and 107.32 kJ/mol for benzyl methanol, cyclohexanone, and toluene, respectively. The optimal reaction conditions are as follows： benzyl methanol as solvent, temperature 150 ℃, and pressure 900 kPa. After an 11-hour reaction, a conversion of 58.0%, a TCPD selectivity of 95.7%, and an exo/endo ratio of 1/5.3 has been obtained.     

5-羟基-5-甲基-3,4-二苯基异唑的合成

以苯乙氰和苯甲酸甲酯为起始原料,经Claisen缩合、羟胺化、环合制得伐地考昔的关键中间体--5-羟基-5-甲基-3,4-二苯基异唑,总产率54.68%.其结构经1H NMR,IR和MS确证.     

玻璃纤维增强MC尼龙复合材料的摩擦磨损性能研究

通过碱催化阴离子聚合反应制备玻璃纤维增强单体浇铸尼龙复合材料(GFMCPA),在MM-200型摩擦磨损试验机上研究了在干摩擦和水润滑条件下,不同玻璃纤维含量对尼龙复合材料摩擦磨损特性的影响,并借助扫描电子显微镜观察其磨损表面形貌.结果表明:玻璃纤维含量对尼龙复合材料的摩擦性能具有显著影响;玻璃纤维质量分数达到30%后复合材料具有较好的耐磨性;在水润滑条件下,复合材料的摩擦系数和磨损量较干摩擦时大幅度降低;玻璃纤维含量低的尼龙复合材料的磨损机制主要为粘着磨损和磨粒磨损;玻璃纤维含量高的尼龙复合材料的粘着磨损减少,磨损机制主要表现为磨粒磨损和疲劳磨损.     

基于数字图像相关技术的岩样破坏实验的应用研究

为了解喀喇昆仑公路(中国段)沿线岩石裂纹演化及受力后的力学性能(位移和应变),采用数字图像相关技术,对三点弯曲加载条件下的灰白石英粉砂岩和片麻岩试件在万能试验机上进行了破坏实验,得到了外力作用下裂纹生成、扩展等演化过程及两种岩样在加载直至破坏过程中的位移场和平均应变曲线。实验结果表明,在相同条件下,灰白石英粉砂岩比片麻岩更易脆断,片麻岩在受力断裂破坏时出现了多条裂纹,导致试件加剧断裂,研究成果为了解这一地域的岩石强度及破坏规律提供了实验依据。