Synthesis and Crystal Structure of 4,4＂-Diamino-N,N＇-diethyl Bisbenzenesulfamide

A new compound of 4,4'-diamino-N,N'-diethyl bisbenzenesulfamide (C18H26N4O4S2,Fw = 426.55) has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to the monoclinic system, space group P21/c with a = 10.0623(9), b =13.6759(13), c =15.5309(14) (A),β = 100.482(2)°, V= 2101.6(3)(A)3, Dc = 1.348 g/cm3, F(000) = 904,μ = 0.285 mm-1, Z = 4, the final R = 0.0512 and wR = 0.1363 for 3485 observed reflections with I ＞2σ(Ⅰ). The structure of the title compound is pseudo secondary axisymmetric, and the two sulfamide-groups show distorted tetrahedral configurations.     

聚N,N-双水杨醛乙二胺合钴修饰超微电极的制备及其在一氧化氮测定中应用的研究

通过电化学聚合法制备了聚Ｎ，Ｎ－双水杨醛乙二胺合钴［ｐｏｌｙＣｏ（Ｓａｌｅｎ）］修饰超微电极，研究了该修饰电极的电催化性质及其在一氧化氮（ＮＯ）测定中的应用．实验结果表明，ｐｏｌｙＣｏ（Ｓａｌｅｎ）修饰超微电极对ＮＯ的测定有高的灵敏度，ＮＯ的浓度在２．０×１０－８～２．８×１０－６ｍｏｌ／Ｌ范围内，电流与浓度呈良好的线性关系，线性相关系数为０．９９９８，检出限为１．０×１０－８ｍｏｌ／Ｌ；该电极进一步修饰Ｎａｆｉｏｎ后，生物体中常见的物质如抗坏血酸、儿茶酚胺类神经递质的代谢物、ＮＯ的氧化产物ＮＯ－２等不干扰测定．本传感器可以满足ＮＯ在体分析的需要．     

TiO~2修饰的介孔分子筛MCM-41的合成、表征及光 催化性研究

首次以三种不同的含钛有机物为氧化钛的前驱体,合成了三种TiO~2呈单层分散状态的TiO~2修饰的介孔分子筛MCM-41,并以XRD,FT-IR,液氮温度下N~2吸附-脱附曲线,固体UV-vis漫反射等表征手段对其结构特征和氧化钛分散状态进行了研究。TiO~2在介孔分子筛MCM-41孔道中分散,MCM-41仍能保持骨架结构,没有晶相TiO~2生成;TiO~2与MCM-41孔道表面的≡Si－OH以化学键连接,生成Si－O－Ti键;TiO~2在MCM-41内孔壁呈均匀单层分散状态;TiO~2粒子的减小使其对紫外光的吸收发生明显的蓝移现象。并以苯酚降解反应为模型检验合成的具有光催化性的TiO~2修饰的MCM-41的光催化活性。     

5-阿维菌素B1a酯的合成及生物活性

阿维菌素B_1a(AVB_1a)与羧酸在DMAP/DCC体系中直接酯化,得到10个5-AVB_1a酯衍生物,产率50%～79%;其化学结构由IR,¹H NMR,¹³CNMR和MS谱确证.生物活性测定结果表明,部分5-阿维菌素B_1a酯衍生物具有良好的杀虫、杀螨活性.     

Template‐Free Hydrothermal Synthesis of Mesoporous MgO Nanostructures and Their Applications in Water Treatment

The controlled synthesis of Mg(OH)₂ nanowires and microflowers composed of nanoplates was successfully achieved by a template‐free hydrothermal synthetic method. It was found that the reaction medium played a crucial role in the morphological control of the precursor nanostructures. The high polarity of water molecules favored the polar growth of the precursor, resulting in the formation of nanowires with a diameter of 80 nm, whereas a mixed water/ethanol medium with a lower degree of polarity led to the formation of microflowers. Moreover, mesoporous MgO nanostructures could be obtained by further annealing these as‐prepared precursors in air at 500 °C for 2 h. During thermal treatment, the wire‐ and flower‐like morphologies were retained. Porosity formation was due to thermal decomposition of Mg(OH)₂ and release of H₂O. Both the mesoporous MgO nanowires and microflowers showed superior ability of adsorbing the organic dye methyl orange, and thus they are promising candidates for polluted water treatment.     

Unsymmetrical N and/or O-bridged calixarene derivatives: synthesis,structure and encapsulation of solvent molecules in the solid state

Eight unsymmetrical N and/or O-bridged calixarene derivatives were obtained by 1 (naphthalene-2,7-diol), 2 (bis(4-hydroxyphenyl)methanone), 3 (4,4′-methylenedianiline), 4 (3,3′-methylenedianiline), 5 (4,4′-oxydianiline) and 6 (4,4′-(perfluoropropane-2,2-diyl)dianiline) reacting with fragment a (4,4′-bis(dichloro-s-triazinyloxy)propane-2,2-diyldibenzene) and b (N,N′-bis(dichloro-s-triazinyl)-4,4′-methylenedianiline) under very mild reaction conditions via efficient fragment coupling strategy. We also obtained the crystal structure of 1a (tetraoxocalix[2](propane-2,2-diyldibenzene,naphthalene)[2]triazine) which can form a molecular capsule by two dimers with C–H?N and C–H?O quadruple hydrogen bonds, and it has the encapsulation ability toward solvent molecules.     

高度分散的Pt/TiO2的制备及光催化活性

用柠檬酸作为空穴捕获剂和分散剂,在温和条件下用光催化还原法将3nm金属铂沉积在7nm的锐钛矿相及介孔二氧化钛纳米晶表面,TEM观察显示铂的负载量为w=1．0％时,多数二氧化钛纳米晶表面沉积了岛状的铂团簇,XPS和电子衍射结果表明铂以游离态存在．负载w=1．0％～2．0％铂的TiO2在苯酚光氧化反应中活性显著提高,Pt/TiO2在氨气中经550℃氮化,可制得氮掺杂的Pt／TiO2可见光光催化剂,氮化过程中铂团簇没有烧结和显著长大。     

毛细管电泳法测定桑叶中的黄酮类成分──芦丁和槲皮素

 采用高效毛细管电泳法分离测定了新疆不同地区、不同采集期、不同品种的桑叶中的黄酮类成分芦丁、槲皮素的含量。以含有体积分数为 15 %甲醇的 10mmol/L的磷酸二氢钠 2 0mmol/L的硼砂溶液 (pH 8 6 2 )为电泳缓冲液 ,采用压力进样方式 ,在 2 5℃ ,2 0kV恒压下进行电泳分离 ,并在 2 45nm波长处检测。结果表明 ,桑叶中的两种目标组分在 12min内完全分离 ,且有良好的线性关系 ;芦丁和槲皮素的加样回收率分别为 95 6 4%和99 36 % ,其RSD分别为 2 2 5 %和 1 79% (n =6 )。方法简单、准确、快速。     

藏药蕨麻多糖水解单糖的毛细管区带电泳分离研究

以1-萘基-3-甲基-5-吡唑啉酮(NMP)为柱前衍生试剂,探讨了毛细管区带电泳模式下对藏药蕨麻多糖水解液中单糖的分离条件。实验采用58.5 cm×50μm i.d.毛细管(有效长度50 cm),55 mmol/L硼酸盐缓冲溶液(pH=9.46),柱温20℃,分离电压22 kV,进样10 s。该法不加任何添加剂,9种单糖可高效、快速基线分离,实现了对藏药蕨麻多糖水解液中单糖的分离和定量分析,结果令人满意。     

用于长城等古建筑探测的NMR探测器的磁体设计

以万里长城为代表的古建筑是世界瑰宝,更是中华民族的象征和骄傲.本文提出利用便携式核磁共振（NMR）装置来探测研究这类古建筑的建筑材料,在不对其造成损伤的基础上,发掘其隐含的科学、技术和工程相关的丰富信息.为此,作为第一步,设计了适合于探测这类古建筑的便携式单边NMR探测器组合式磁体.该探测器的磁体结构以semi-Halbach为基础,通过不同磁体模块间的组合得到对应移动探测模式、长距离探测模式和均匀磁场探测模式的磁体结构.随后根据优化结果,设计加工了磁体组件,并采用该磁体进行了流体、长城城砖和现代红砖的NMR实验,实测结果与模拟一致.该组合式磁体的优点在于通过不同磁体模块组合,实现了多种探测方式,适用于探测长城等这类古建筑物需要多种探测模式的科学研究.