甲氧羰基亚甲基三苯基胂与邻羟基芳醛,酮的反应-5,6-苯并-2-吡喃酮的合成

本文报道一种合成烃基取代5,6-苯并-2-吡喃酮的方法。甲氧羰基亚甲基三苯基胂与烃基取代的邻羟基芳醛、酮反应,首先生成α,β-不饱和酸酯,继而发生分子内环化,生成烃基取代的5,6-苯并-2-吡喃酮。     

四硼酸锂水溶液体系的热容及离子相互作用

采用Setaram BT 2.15微量热仪测定了Li₂B₄O₇-H₂O体系(Li₂B₄O₇的浓度为0.00415~0.4208 mol/kg)在298.15, 308.15和323.15 K下的热容, 分别计算了不同温度和浓度下的表观摩尔热容, 并获得了不同温度下表观摩尔热容与浓度的关系式. 基于Li₂B₄O₇-H₂O体系的热容测定结果, 应用Pitzer电解质溶液离子相互作用表观摩尔热容模型, 拟合获得了四硼酸锂在不同温度下的Pitzer单盐参数.     

三门峡虢季墓遗址盐害分析与调查

针对三门峡虢季墓遗址部分区域存在起甲、泛白、疱疹等由可溶盐引起的病害,在其遗址不同部位取样进行土遗址本体含盐分析.取样区域包括虢季墓、梁姬墓和近代墓遗址.采用X射线荧光光谱(XRF)和离子色谱(IC)分析所取样品的可溶盐成分、含量及可溶盐成盐元素在土遗址中的成盐规律.采用电子能谱(XPS)和X射线衍射(XRD)分析样品的物相组成及盐分状态,扫描电子显微镜/能谱(SEM/EDS)进一步考察含盐土质的颗粒组成、微观形貌等.结果表明:虢季墓取样区域所含盐分主要为Na_2SO_4、CaCO_3和少量的其他盐分如CaCl_2、KNO_3和NaCl等.靠近地面部位所取样品盐分含量高于其他部位,盐害表现更为明显.梁姬墓取样区域总盐分含量略高于虢季墓与近代墓,硝酸盐含量较高.而近代墓遗址可溶盐盐分含量略低,盐害不明显.在不同取样点可溶盐含量有所差异,但在邻近区域,其成盐具有一定规律性,这一点对于遗址基体中盐害的深入研究与防治具有重要意义.     

H4PMo11Vo40杂多酸及其镧盐的合成与性质

本文提出主要用~(51)V NMR、CV并辅以IR、XRD、DTG、元素分析等作为有效地核查纯度和表征催化剂的手段。     

MgO•3B2O3-18%MgSO4-H2O过饱和溶液析出固相组成和机理研究

针对青藏高原盐湖卤水析盐过程的特点, 模拟合成MgO•3B₂O_3-18%MgSO_4-H₂O过饱和溶液, 在150 ℃水热条件下对析出固相进行研究. 用化学分析方法、X射线衍射、红外光谱进行物相鉴定. 提出了可能的结晶反应机理, 分析了水热温度对析出物相的影响及MgSO₄对硼酸镁盐的盐溶效应随水热温度的变化.     

经非对映异构盐的外消旋体拆分实用方法

经非对映异构盐拆分外消旋体的经典拆分方法，仍是提供对映纯化合物的有效方法之一。然而对许多外消旋体来讲，获得需要的异构体远小于50%。如何通过经典拆分使需要的异构体获得最大产率？本文阐述了一种外消旋体拆分的实用方法，通过非对映异构盐的形成可得到所需的异构体最大产率。运用该实用策略，在拆分外消旋哌啶甲酸乙酯、Corey内酯和石杉碱甲中间体上都成功实现。该策略的实践基础是著名的Marckwald 原理。     

新型有机盐光引发剂的双光子聚合特性研究

本文运用激光微细加工技术,通过对不同浓度引发剂的甲基丙烯酸类树脂的聚合行为进行评价,研究了1-甲基-2-[2-(9-戊基-咔唑-3-基)-乙烯基]-3,3-二甲基吲哚碘盐(I)作为双光子光引发剂的聚合特性,结果表明该化合物在扫描速度为44μm/s时,双光子聚合阈值为139kJ/cm²;当激光能量密度为286kJ/cm²时,引发聚合的曝光时间阈值为0.7ms.实验结果为进一步作为双光子聚合三维结构的微细加工提供了可靠依据.     

Synthesis and Characterization of Fluoro- and Chloro- bimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal alkoxides was retained to a large extent in 4 ： 1 halogenated alcohol-benzene solution. The heteronuclear NMR spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern. SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.     

Molecular Dynamics Simulation of the Self-assembled Monolayers of 1-Adamantanethiolate and Its Derivatives on Au（111） Surfaces

The self-assembled monolayers （SAMs） of 1-adamantanethiolate and its derivatives on Au（111） surface were investigated. Density functional theory （DFT） calculation indicates that the most stable configuration for absorption is at the face centered cubic （fcc）-bridge site. Canonical ensemble molecular dynamics （MD） simulations were carried out to study the structures and energies of the SAMs. The ordered structures of the SAMs were analyzed by means of radial distribution function and the relative stability of the SAMs was compared. It was concluded by the comparison of various contributions to the SAM formation energy that the formation of the SAMs was determined by the intermolecular nonbonding interaction and the chemical bonding interaction of sulfur and gold.