Synthesis,characterization, and crystal structures of organonickel(II) complexes coordinated to novel 1‐bromo‐2,6‐bis{[(λ5‐phosphanylidene)imino]methyl}benzene NCN‐pincer ligands

A novel family of four 1‐bromo‐2,6‐bis{[(λ⁵‐phosphanylidene)imino]methyl}benzene ligands has been synthesized and characterized. The phosphiniminomethyl substituents are decorated with either three phenyl groups, two phenyl and one cyclohexyl group, one phenyl and two cyclohexyl groups, or three cyclohexyl groups. Each ligand was metallated using zero‐valent nickel through an oxidative addition to form a family of organonickel(II) complexes, namely (2,6‐bis{[(triphenyl‐λ⁵‐phosphanylidene)imino]methyl}phenyl‐κ³N,C¹,N′)bromidonickel(II) dichloromethane hemisolvate, [NiBr(C₄₄H₃₇N₂P₂)]·0.5CH₂Cl₂, (2,6‐bis{[(cyclohexyldiphenyl‐λ⁵‐phosphanylidene)imino]methyl}phenyl‐κ³N,C¹,N′)bromidonickel(II) diethyl ether hemisolvate, [NiBr(C₄₄H₄₉N₂P₂)]·0.5C₄H₁₀O, (2,6‐bis{[(dicyclohexylphenyl‐λ⁵‐phosphanylidene)imino]methyl}phenyl‐κ³N,C¹,N′)bromidonickel(II), [NiBr(C₄₄H₆₁N₂P₂)], and (2,6‐bis{[(tricyclohexyl‐λ⁵‐phosphanylidene)imino]methyl}phenyl‐κ³N,C¹,N′)bromidonickel(II), [NiBr(C₄₄H₇₃N₂P₂)]. This family of complexes represents a useful opportunity to investigate the impact of incrementally changing the steric characteristics of a complex on its structure and reactivity.     

γ-Fe2O3/Ag/TiO2的制备与抗菌性能

采用两步法合成了γ-Fe₂O₃/Ag/TiO₂复合光催化剂, 以大肠埃希氏菌(E. coli)为目标菌, 对数去除率为评价指标评价了催化剂的抗菌性能, 优化了催化剂的最佳制备参数. 通过X射线衍射、 扫描电子显微镜、 X射线光电子能谱和紫外-可见漫反射光谱等手段对催化剂进行了表征. 结果表明, 当Ti/Ag摩尔比为1:0.05, 煅烧时间为3 h, 煅烧温度为350 ℃时, γ-Fe₂O₃/Ag/TiO₂表现出最佳抗菌活性. 复合催化剂具有介孔结构, 比表面积为89.1 m²/g; 光吸收边界达690 nm, 有良好的可见光响应能力; 磁性较强, 在水处理应用中可有效分离和重复使用. 反应条件不受光源限制, 在有/无光照下均具有良好的抗菌活性, 且太阳光辐照下对E. coli的对数去除率可达6.28.     

酵母核糖核酸在碳纳米管修饰电极上的电化学行为及其分析测定

研究了酵母核糖核酸（yRNA）在碳纳米管（MWNT）修饰电极上的电化学行为，优化了测定参数，在此基础上建立了一种直接测定yRNA的电分析测试方法。yRNA在碳纳米管修饰电极上于磷酸盐缓冲溶液中在0．758V处产生不可逆的氧化电流峰，峰电流与yRNA的质量浓度在1～10mg／mL之间有良好的线性关系，线性回归方程为：Iρ=0．0813ρ＋0．1807，相关系数r为0．9980，检出限为0．6mg／mL。     

A new anode material LiMoS2 for use in rechargeable Lithium Ion Batteries

The novel applications of molybdenum disulfide in recent research were reviewed, such as in lubricant, catalyst and photoelectrochemical solar cells. Recently, we found that LiMoS2 is a good candidate for new anode materials for lithium ion batteries with high lithium storage capacity.Here, the anode material LiMoS2 was synthesized by a hydrothermal method at 150℃ and the electrochemical characterization as an anode material for lithium ion batteries was examined.put in Teflon-lined stainless steel autoclaves of capacity 40 mL. Distilled water was used to fill the autoclaves to 70 % of the total volume. The autoclaves were maintained at 150℃ for 24 h and then cooled naturally. The resulting dark-gray powders were filled and washed with distilled water,diluted hydrochloric acid and ethanol, successively. The final products were dried at 80℃ for 24 h.The powder X-ray diffraction pattern showed the prepared LiMoS2 was amorphous structure. A test cell using LiMoS2 as the active material was discharged and charged between 3 and 0.01 V with respect to Li metal at a constant current density of C/5 (that is, one lithium per formula unit in 5 hours). During the first discharge, the potential rapidly drops to reach a large plateau at 2.2 V, then slowly drops to the other plateau at 0.8 V, and then continuously decreases down to 0.01V. There is only a plateau at 1.35 V in the subsequent discharge curves. The plateaus of charge potential appear at about 1.9 V.The irreversible loss was 41% in the first cycle. The ratio of discharge and charge is more than 99%in the subsequent cycles. Moreover, the ratio of discharge and charge almost reaches 100% after thedemonstrated that LiMoS2 has a very high capacity and a good cycle-ability as an anode material forlithium ion batteries.     

锌掺杂对TiO2染料敏化电池光阳极中电荷俘获态分布及电子复合过程的影响

基于瞬态光电压和瞬态光电流技术研究了锌掺杂的TiO2染料敏化太阳能电池中电子复合及传输的动力学行为.通过实验获得了不同阳极掺杂条件下的电子复合时间常数与电子收集时间常数,考察了锌掺杂对电池阳极材料导带能级和电子俘获态的影响.研究结果表明,锌的掺杂在提高TiO2导带能级的同时延长了俘获态电子的复合时间常数,从而大大提高了电池的开路电压.     

过碳酸钠-醋酸酐作用下的Baeyer-Villiger反应

在醋酸酐介质中, 过碳酸钠可以与酮进行Baeyer-Villiger反应, 将它们氧化成相应的酯。其中脂环酮的反应结果较好, 环内酯的产率约为80%。芳香酮除芳环被活化的以外, 效果欠佳。当反应施加超声辐射后可显著加快反应速度, 并对过碳酸钠的作用机理进行了讨论。     

基于过程分析技术和设计空间的金银花醇沉加醇过程终点检测

建立了一种新的基于过程分析技术(PAT)和质量源于设计(QbD)设计空间的中药制药过程终点分析与控制方法.以近红外(NIR)光谱技术为PAT工具, 采集正常操作条件下制药过程的多批次NIR光谱; 采用主成分分析结合移动块相对标准偏差(PCA-MBRSD)法, 确定每一批次过程的理想终点样本(DEPs), 由多批DEPs的光谱信息构成过程终点设计空间; 在过程终点设计空间确定的范围内, 建立多变量统计过程控制(MSPC)模型, 利用多变量Hotelling T²和SPE控制图对过程终点进行判断.应用上述方法, 进行了金银花醇沉加醇过程终点检测研究, 结果表明该方法灵敏、准确, 适宜于中药制药过程终点检测.     

Chiral N-phosphonyl imine chemistry:asymmetric additions of glycine enolate to diphenyl diamine-based phosphonyl imines

Diphenyl diamine-based phosphonyl imines attached by the N-isopropyl group in the auxiliary have been synthesized in good yields under convenient reaction conditions.These new chiral N-phosphonyl imines can react with glycine enolate smoothly to give chiral α-β diamino esters in good yields(72%-90%) and up to excellent diastereoselectivity(>99:1 dr).By treatment with HBr,the chiral auxiliary can be readily removed.The absolute structure has been unambiguously determined by converting a product to a known sa...     

多酸含量对无机/高分子复合薄膜结构及光致变色性能的影响

制备了一系列不同浓度的钨磷酸/聚乙烯醇(PWA/PVA)复合薄膜, 通过红外光谱、原子力显微镜、紫外-可见吸收光谱对复合薄膜的结构和光致变色性能进行了研究. 红外光谱分析结果表明, Keggin结构钨磷酸和聚乙烯醇分子的基本结构在复合薄膜中仍然存在, 钨磷酸分子与高分子底物间存在氢键作用, 形成电荷转移桥. 原子力显微镜(AFM)结果表明复合前后PVA薄膜表面形貌发生了显著变化, 复合膜表面形貌随钨磷酸含量的不同而不同. 在紫外光照射下, 复合薄膜由无色变为蓝色. 复合膜的升色速度和褪色速度均随着钨磷酸含量的增加而加快. 这些结果表明钨磷酸含量对复合膜的微结构存在影响, 从而导致了复合膜具有不同的光致变色性能.     

瓯柑石油醚提取物的GC-MS分析

为了研究瓯柑的挥发性成分和脂溶性成分, 采用GC-MS分析法进行分离鉴定, 并用面积归一法确定各成分的质量分数. 从瓯柑果肉石油醚提取物中分离鉴定出11种成分, 占总提取物的97.43%, 其主要成分为(Z, Z)-9, 12-十八碳二烯酸(37.46%)、γ-谷甾醇(22.91%);从瓯柑皮石油醚提取物中分离鉴定出10种成分, 占总提取物的99.79%, 其主要成分为柠檬烯(86.39%).