高含量钒的钼钒磷杂多化合物的合成和性质研究

本工作改进了文献[4]报导的几种原料同时混合、加热煮沸合成的方法采用分步加入原料,控制反应温度、多次重结晶的方法合成了6、7、8个钒原子取代的钼钒磷杂多酸铵;并以铵盐为原料,用离子交换、冷冻分离和真空抽吸相结合的提纯方法制备了未见文献报导的相应的固体杂多酸;H₅[PMo₅V₇O_37.5]·xH₂O,H₆[PMo₄V₈O_37.5]·xH₂O。通过元素组成分析确定了它们的组成。这些杂多酸在水溶液、非水溶液中的电位滴定表明,杂多阴离子在分解前没有发生自电离、水解等情况,它们在水溶液中是稳定的。酸的碱度分别为5、5、6。通过纸上色谱实验,讨论了杂多酸的分解过程。由热重分析和溶解性实验得到它们的分解温度,本文还讨论了这些化合物的红外、紫外光谱,x光粉末衍射及极谱性质。光谱结果表明,它们可能具有Keggin结构,由导数脉冲极谱得到它们的峰电位。     

Supported dual‐acidic 1,3‐disulfoimidazolium chlorozincate@HZSM‐5 as a promising heterogeneous catalyst for synthesis of indole derivatives

HZSM‐5‐supported Brönsted and Lewis acidic ionic solid 1,3‐disulfoimidazolium chlorozincate materials ([dsim]₂[ZnCl₄]@HZSM‐5) were synthesized with various ratios (3, 6, 9, 17 and 50% w/w). The heterogeneous materials were characterized via a variety of spectroscopic techniques. Dual acidity of these materials was determined using specified techniques. These acidic solids were examined as stable heterogeneous catalysts for the Fischer indole reaction of equimolar amounts of phenylhydrazine hydrochloride and various aliphatic or aromatic ketones at 80–90°C in neat condition to produce substituted indole derivatives. The efficient 17% ionic salt‐loaded HZSM‐5 composite was easily reused for ten consecutive cycles with a slight loss of its activity. The recycled catalyst was further analysed using powder X‐ray diffraction and inductively coupled plasma optical emission spectrometric techniques.     

Depolarization properties of cirrus clouds from polarization lidar measurements over Hefei in spring

A new polarization lidar has been developed for detecting depolarization characteristics of aerosol and cirrus over Hefei (31.90°N, 117.16°E), China. The fundamental principle of polarization lidar is briefly introduced.     

A note on approximate Bayesian credible sets based on modified loglikelihood ratios

Higher-order asymptotic arguments for a scalar parameter of interest have been widely investigated for Bayesian inference. In this paper the theory of asymptotic expansions is discussed for a vector parameter of interest. A modified loglikelihood ratio is suggested, which can be used to derive approximate Bayesian credible sets with accurate frequentist coverage. Three examples are illustrated.     

电致变色薄膜锂化技术的研究

提出了一种新的电致变色薄膜的锂化方法，通过电子枪蒸镀锂单质，提高了锂的离化率，从而提高了锂化效果，采用此技术研制的全固态电致变色薄膜器件获得了较好的变色特性，透射式和反射式全固态电致变色薄膜器件的变色性能分别为５０％￣５％和７０％￣２０％。     

Diethyldisulfoammonium chlorometallates as heterogeneous Brønsted–Lewis acidic catalysts for one‐pot synthesis of 14‐aryl‐7‐(N‐phenyl)‐14H‐dibenzo[a,j]acridines

A new series of Brønsted–Lewis acidic diethyldisulfoammonium chlorometallates, [DEDSA][FeCl₄] and [DEDSA]₂[Zn₂Cl₆], were synthesized as solid materials from the reaction of [(Et)₂N(SO₃H)₂][Cl] ionic liquid with transition metal chlorides (FeCl₃ and ZnCl₂) at 80 °C in neat condition for 2 h. The chlorometallates were fully characterized using various spectroscopic and analytical techniques such as Fourier transform infrared, UV–visible and Raman spectroscopies, powder X‐ray diffraction, scanning electron microscopy, energy‐dispersive X‐ray and thermogravimetric analyses, Hammett acidity and elemental analyses. Their catalytic activity was studied as reusable heterogeneous catalysts for the three‐component synthesis of novel 14‐aryl‐7‐(N‐phenyl)‐14H‐dibenzo[a,j]acridines under solvent‐free conditions at 100 °C.     

Green Synthesis of Tetraalkylammonium Tribromide using Cerium(IV) Ammonium Nitrate (CAN) as Oxidant

Cerium(IV) ammonium nitrate (CAN) mediates oxidation of tetraalkylammonium bromide to tetraalkylammonium tribromide in greener reaction conditions using water as solvent. The procedure is simple, convenient, and environmentally benign for the synthesis of tetraalkylammonium tribromide with great yields.     

偏振-米散射激光雷达对卷云的探测

 研制了一台偏振-米散射激光雷达,用于卷云和沙尘气溶胶后向散射光退偏振比的探测研究。介绍了偏振-米散射激光雷达的探测原理,叙述了偏振-米散射激光雷达的结构、技术参数、测量方法和数据处理方法。给出了偏振-米散射激光雷达对合肥市西郊上空卷云的结构、退偏振比垂直廓线以及光学厚度的典型探测结果,对这些结果进行了分析和讨论。初步探测结果表明,合肥西郊上空高度在6～10 km的卷云的退偏振比在0.2～0.5之间,该激光雷达可以对卷云进行有效的探测,能较好地反映卷云及其光学特性的时空分布。