Palladium‐Catalyzed Decarboxylative Cycloaddition of Vinylethylene Carbonates with Formaldehyde: Enantioselective Construction of Tertiary Vinylglycols

An efficient method for the enantioselective construction of tertiary vinylglycols through a palladium‐catalyzed asymmetric decarboxylative cycloaddition of vinylethylene carbonates with formaldehyde was developed. By using a palladium complex generated in situ from [Pd₂(dba)₃]?CHCl₃ and a phosphoramidite ligand as a catalyst under mild reaction conditions, the process allows conversion of racemic 4‐substituted 4‐vinyl‐1,3‐dioxolan‐2‐ones into the corresponding 1,3‐dioxolanes, as methylene acetal protected tertiary vinylglycols, in high yields with good to excellent enantioselectivities.     

微波法制备还原氧化石墨烯负载Pt_3Co纳米合金(英文)

微波辐射法可以在数分钟内将高度分散的Pt3Co合金颗粒负载于还原氧化石墨烯表面上.表征结果发现,与传统的溶剂热法和浸渍法相比,微波法制备的催化剂中贵金属的利用率高,合金颗粒的分布均匀,组成可控,同时氧化石墨烯的再石墨化现象也得到有效地抑制.采用微波法制备的Pt3Co/RGO-MW催化剂在肉桂醛加氢反应中具有较高的活性和和产物选择性.Pt3Co/RGO-MW中每一个Pt原子在70℃的转化频率高达23.8 min-1.     

光诱导转化法制备单晶Ag纳米三棱体和立方体

The preparation of Ag nanoparticles with the non-spherical shape has been conducted from aqueous solution by photo induced conversion. Ag nanoprisms (80～120nm) and nanocube s(90～200nm) were respectively obtained in the presence of trisodiumcitrate (TSC) orpolyvinylpirrolidon (PVP). These Ag nanoparticles were single-crystals. The results showed that Ag nanoprisms had apreferential growth direction along the Ag(111) axis and Ag nanocubes had a preferential growth direction along the Ag(100) axis. By means of characterization with TEM, ED and UV-V is Spectra, the fundamental analyses and discussion about the changing causes of nanoparticles shape from spherical tonon-spherical have been carried out in the photo induced process.     

两自由度舵-轴系统振动三维效应修正模型

考虑到小展弦比舵所存在的三维效应,利用附加质量系数ε和环量系数δ对经典Theodorsen两自由度运动方程进行修正,并与经典颤振实验结果进行比较,验证了修正后两自由度运动方程的适用性.质量比μ的不同会引起两自由度舵-轴系统振动V-g曲线形态的差异,故根据V-g曲线形状的不同将系统的振动分为第一类振动和第二类振动,其对应情况下可能发生的颤振为第一类颤振和第二类颤振.利用修正后的两自由度颤振理论模型分析了支撑刚度k_h、扭转刚度k_α、舵弦向重心位置x_α和初始攻角AOA对舵-轴系统颤振特性的影响规律,并通过开展相关实验对理论计算值进行验证,实验结果与计算值吻合良好.计算结果表明,k_h,k_α,x_α和AOA对颤振速度V_F存在显著影响,它们可以分别在一定的取值范围内导致系统发生第二类颤振.并且,V_F随k_h的增大单调增大,随k_α和x_α的增大先增大再减小,随AOA的增大则逐渐减小.其中,令V_F存在非零值的x_α取值范围狭小,反映了系统振动形态对x_α的敏感性.因此,在设计阶段避免将x_α设置在这个狭小的范围内可以降低颤振的发生几率.另一方面,由于V_F对k_h和k_α的反应缓慢,一旦颤振发生就可以通过将刚性轴锁紧来消除颤振效应.     

Fe3+、Ce3+共掺杂γ-LiAlO2的发光性质

采用不同于传统固相反应法的制备方法合成了Fe,Ce 共掺杂γ-LiAlO₂。通过XRD和 SEM分析表明,采用这种方法能够成功获得尺寸小于10 μm的四方相结构γ-LiAlO₂荧光粉。从γ-LiAlO₂ ∶ Fe,Ce 的激发和发射光谱可以看出,通过引入少量的铈离子,我们首先发现了铈离子掺杂对样品的发光效率有明显的影响。并且随着铈离子浓度的增加,其发光效率也出现规律性的变化,而且发射光谱在Ce离子摩尔分数达到1.5%的情况下发光效率最强,当Ce离子摩尔分数达到3％时,发光效率明显下降。这种高效的荧光粉作为转光剂应用于人工植物照明和农用转光膜具有积极的意义。     

光诱导转化法制备单晶Ag纳米三棱体和立方体

分别以柠檬酸三钠 (TSC)及N 聚乙烯吡咯烷酮 (PVP)为稳定剂 ,首先采用KBH4化学还原法制得球形Ag纳米粒子溶胶 (粒径 12～ 18nm) ;再将两种溶胶置于 5 0 0W卤钨灯下进行光诱导转化实验 ,一定转化时间后 ,球形Ag纳米粒子分别转化为单晶Ag纳米三棱体 (边长 80～ 12 0nm)和立方体 (边长 90～ 2 0 0nm) .利用透射电子显微镜 (TEM )、电子衍射 (ED)和紫外 可见吸收光谱 (UV Vis)等手段对单晶Ag纳米三棱体和立方体进行了表征 ,对光转化过程中Ag粒子由球形到三棱体和立方体的转变原因进行了初步的分析和探讨 .认为主要原因在于不同种类稳定剂在Ag的不同晶面吸附作用不同 ,从而形成沿某一晶面取向生长的Ag单晶体 .     

CHARACTERIZATION OF NOVEL POLYMERIC INTERMEDIATE POLY（p-BROMOACETYL STYRENE） CROSSLINKED BY DIVINYLBEZENE

Acetyl crosslinked polystyrene (EPS) and crosslinked bromoacetyl polystyrene (BEPS)beads were synthesized by Fridel-Crafts acetylation of polystyrene (PS) and bromination of EPS respectively. FTIR, XPS, and TG-TDG were employed to characterize their structures. The results revealed there are two types of bromine in the BEPS molecule. One is in the main chain of polystyrene and the other is in the acetyl. The results of TG-DTG showed that the rates of loss weight of PS, EPS, and BEPS were 92.7%, 92.2%, and 81.3% among the 300 ℃～500 ℃; 7.3%, 7.8%, and 18. 7% in 594 ℃, 660 ℃, and 584.8 ℃, respectively.     

HPLC Determination of DCJW in Rat Plasma and Its Application to Pharmacokinetics Studies

A high-performance liquid chromatography–UV method for determining DCJW concentration in rat plasma was developed. The method described was applied to a pharmacokinetics study of intramuscular injection in rats. The plasma samples were deproteinized with acetonitrile in a one-step extraction. The HPLC assay was carried out using a VP-ODS column and the mobile phase consisting of acetonitrile–water (80:20, v/v) was used at a flow rate of 1.0 mL min⁻¹ for the effective eluting DCJW. The detection of the analyte peak area was achieved by setting a UV detector at 314 nm with no interfering plasma peak. The method was fully validated with the following validation parameters: linearity range 0.06–10 μg mL⁻¹ (r > 0.999); absolute recoveries of DCJW were 97.44–103.46% from rat plasma; limit of quantification, 0.06 μg mL⁻¹ and limit of detection, 0.02 μg mL⁻¹. The method was further used to determine the concentration–time profiles of DCJW in the rat plasma following intramuscular injection of DCJW solution at a dose of 1.2 mg kg⁻¹. Maximum plasma concentration (C _max) and area under the plasma concentration–time curve (AUC) for DCJW were 140.20 ng mL⁻¹ and 2405.28 ng h mL⁻¹.     

由M0.02Cu0.4Mg5.6Al1.98(OH)16CO3 (M=Ru,Re)水滑石为前驱体制备的双金属固体碱催化甘油氢解

采用共沉淀法合成了M_0.02Cu_0.4Mg_5.6Al_1.98(OH)₁₆CO₃ (M = Ru,Re)水滑石前驱体,然后经焙烧和还原制备了铜分散度较高的双功能M-Cu/固体碱催化剂.这些双功能催化剂在粗甘油氢解制备丙二醇反应中表现出了很好的催化活性.表征结果证明,M的加入增强了催化剂表面氢的吸附和活化,进而促进了甘油的转化.