固体酸催化合成二芳基甲酮化合物的研究进展

二芳基甲酮化合物是一类非常重要的化工产品和医药中间体,广泛应用于医药、涂料、电子及日用化工等领域综述了在不同类型固体酸催化下,利用Friedel-Crafts酰基化反应合成二芳基甲酮化合物的研究进展.     

Synthsis of 4‐Piperidones via Multicomponent Double Mannich Reaction Catalyzed by I2

A multicomponent double Mannich reaction of amines, aldehydes and ketones was efficiently catalyzed by molecular iodine, producing a series of 4‐piperidones in a stereoselective way. A variety of amines, aldehydes and ketones were tolerated in this tandem process, including those with labile functinal groups. Further investigation of the reaction between alkyl‐imines and ketones showed that imines from amines and ketones were formed in situ and isomerized to enamine in the presence of molecular iodine to accelerate the corresponding Mannich addition.     

氮化硅纳米薄膜非平衡热导率实验研究

3ω实验方法是一种可以对薄膜热导率进行瞬时测量的方法。根据3ω方法测试原理,搭建了薄膜导热系数测试平台,并且分别测试低频率段和高频段薄膜与基底的温升以及薄膜热导率。测试结果表明:Si3N4薄膜的热导率随温度的升高而增大;高频段下,热导率受频率影响大,误差大;在低频段下薄膜热导率与频率变化基本无关;基于电子与声子的局部热平衡运输方程假设,S i3N4薄膜的热导率具有极度非平衡性;通过比较电阻、热导率与温度的关系可以看出加热器的尺寸大小会影响薄膜的热导率,最佳加热器的宽度选用20μm左右。     

航空照明功率型LED结温的小电流K系数测量法

功率型LED已经越来越多地运用于航空照明领域,迅速准确地获得LED的结温对航空灯具的散热设计显得极为重要。介绍了一种运用小电流K系数测量LED结温的方法。利用了LED半导体芯片的伏安特性,通过构建测量系统获得LED两端瞬间压降值来算出LED的结温。具有获得LED结温快速、准确、非破坏性等特点。     

Simultaneous determination of 24 or more acidic and alkaline phytohormones in femtomole quantities of plant tissues by high-performance liquid chromatography–electrospray ionization–ion trap mass spectrometry

Phytohormones act at relatively low concentrations as major regulatory factors of plant growth and development, and cross talk of phytohormones is currently of great interest throughout the plant science community. To meet this demand, a method that is capable of simultaneously analyzing diverse plant hormones is essential. This paper introduces a high-performance liquid chromatographic separation technique coupled with sensitive and selective ion trap mass spectrometry to simultaneously determine 24 or more acidic and alkaline phytohormones, including auxin, cis- and trans-abscisic acid, 11 cytokinins, and 10 gibberellins, in a single injection of sample. A binary solid-phase extraction using Oasis MCX cartridges for cations and Oasis MAX cartridges for anions was used to prepurify more than 24 acidic and alkaline phytohormones from a single plant extract. The method showed good linearity for all 24 phytohormones with R ² values ranging from 0.9903 to 0.9997. Limits of detection for most of the phytohormones were in the femtomole range with some extending into the sub-femtomole range. This method was applied to hundreds of plant samples comprising different tissues from various plants, including herbaceous, woody climbing, and woody plants to demonstrate feasibility and to validate the methodology.     

关于SpaceWire总线接口可靠性的研究

为满足航天器有效载荷间高速数据传输的发展需求,提出了两种SpaceWire总线可靠性的改进方案;在SpaceWire总线描述的基础上,分析了字符的正确性校验和传输过程中的错误及检测恢复机制等提高可靠性的方法;针对通信链路发生物理性故障的问题,提出了两种基于硬件冗余机制的SpaceWire可靠性改进方案,一种是在系统间建立两个相独立的协议装置,另一种是使用多路输出选择器进行切换将数据传输给目的节点;通过实验验证,两种方案能够处理通信链路出现物理故障的问题。     

高斯光束在单轴晶体中的布拉格衍射特性

利用适当的坐标变换和黎曼方法建立了高斯光束在单轴晶体中布拉格衍射的严格的耦合波理论 ,获得了一组严格的耦合波方程和衍射效率计算公式 ,讨论了衍射效率随折射率调制量的关系以及波长选择性和角度选择性 ,同时分析了衍射效率对再现光宽度的要求。模拟计算表明 ,异常光与异常光 (ee)型布拉格衍射能够达到的最大衍射效率由记录时入射角决定 ,而且通过各参量的适当的选择 ,理论上ee型布拉格衍射能够在折射率调制量很低(如 8.2× 10 -5)的情况下获得接近 90 %的衍射效率。该理论模型为如何在较低折射率调制量下获得较高衍射效率提供了理论指导     

中心金属或配体刚性调控的α-酮酸酯对硝基烯的不对称共轭加成

通过手性二胺配体与Cu或Ni络合合成了手性金属催化剂,并将其应用于α-酮酸酯对硝基烯的不对称共轭加成反应中,发展了通过改变中心金属或调节配体刚性实现反应对映选择性反转的策略.使用同一手性二胺配体(1S,1'S)-1,1'-联异吲哚啉,与不同的金属前体(Cu(OAc)2·H2O与Ni(OAc)2·4H2O)络合,可以高选择性地得到绝对构型相反的共轭加成产物(ee值高达94%与93%).同样,使用同一金属前体Cu(OAc)2·H2O,与同一手性源出发合成的两种刚性不同的二胺配体络合,也可以在这个反应中实现产物绝对构型的反转(ee值高达94%与94%).     

Size control of gold nanocrystals in citrate reduction: the third role of citrate

Growth kinetics and temporal size/shape evolution of gold nanocrystals by citrate reduction in boiling water were studied systematically and quantitatively. Results reveal that the size variation and overall reaction mechanism were mostly determined by the solution pH that was in turn controlled by the concentration of sodium citrate (Na3Ct) in the traditional Frens's synthesis. This conclusion was further confirmed by the reactions with variable pH but fixed concentrations of the two reactants, HAuCl4 and Na3Ct. Two substantially different reaction pathways were identified, with the switching point at pH = 6.2-6.5. The first pathway is for the low pH range and consists of three overlapping steps: nucleation, random attachment to polycrystalline nanowires, and smoothing of the nanowires via intra-particle ripening to dots. The second pathway that occurred above the pH switching point is consistent with the commonly known nucleation-growth route. Using the second pathway, we demonstrated a new synthetic route for the synthesis of nearly monodisperse gold nanocrystals in the size range from 20 to 40 nm by simply varying the solution pH with fixed concentrations of HAuCl4 and Na3Ct. The switching of the reaction pathways is likely due to the integration nature of water as a reaction medium. In the citrate reduction, the solution pH was varied by changing the initial HAuCl4/Na3Ct ratio. Consequently, when pH was higher than about 6.2, the very reactive [AuCl3(OH)]- would be converted to less reactive [AuCl2(OH)2]- and [AuCl(OH)3]-.