苯部分加氢制环己烯的非晶态Ru-M-B/ZrO2催化剂的表征

采用化学还原法，制备了高活性，高选择性非晶态RU-M-B/ZRO2催化剂，并将其用于催化苯部分加氢制环己烯，在140℃、5.0Mpa氢压下，苯转化40%时，环己烯选择性达到85%左右。环己烯最高收率达到52.1%，用XRD、SEM、BET比表面积测定等手段对摧化剂进行表征，XRD和SEM测试表明，RU-U-B/ZRO2属于非晶态，活性组分高度分散，XRD结果证实，在加氢过程中，非晶分解，RU晶化；温度愈高，RU晶化愈快，催化剂的活性、选择性与RU微晶的粒径有关，RU微晶粒径应控制在5nm左右，BET比表面积测定表明，ZRO2的负载提高了催化剂的比表面积，从而有利于活性组分的高度分散，并可阻止RU微晶的长大，讨论了B和ZRO2对提高选择性的作用。     

Iodine catalyzed efficient synthesis of symmetrical diaryl sulfoxides from arenes and thionyl chloride under solvent-free conditions

Synthesis of symmetrical diaryl sulfoxides from arenes and thionyl chloride in the presence of a catalytic amount of iodine at room temperature under solvent-free conditions is described.Mild reaction conditions,easy workup,high yield,and easily available catalyst are important features of this method.     

麻黄中伪麻黄碱在小鼠组织中的分布研究

为了解麻黄(Herba ephedrae,简称HE)中伪麻黄碱(Pseudoephedrine,简称PE)在小鼠脑、肺、心、肝、肾的分布变化,探讨HE的归经,用GC-MS/SIM法,分析了用药后30、60、120 min PE在小鼠脏器分布量。结果表明,PE于不同时间点在小鼠脏器的分布由多到少的顺序是:30 min时,肺脏(肾脏、肝脏、脑),心脏;60 min时,肾脏,心脏(肝脏),脑,肺脏;120 min时,脑,肾脏,心脏,肝脏(肺脏)。本试验从PE在小鼠体内脏器的分布量初步反映了HE的归经趋势。     

N—BOC—8—氨甲基—2—萘甲酸的改进合成法

以２－萘甲酸为原料，经硝化，酯化，重氮化，选择性催化氢化，ＢＯＣ酸酐保护等六步反应，完成了Ｎ－ＢＯＣ－８氨甲基－２－萘甲酸（１ａ）的合成，为化合物１的合成提供了新的合成途径。     

INFLUENCE OF COMPOSITIONAL HETEROGENEITY ON MORPHOLOGY AND PROPERTIES OF SEGMENTED COPOLYMERS

Polyethylene terephthalate(PET)/polycaprolactone(PCL) segmented copolymers with different hard segment contents and a blend of two of them were studied by using DSC, WAXS, TEM and IR techniques and dynamic mechanical, stress-strain and isothermal crystallization measurements. Emphasis was laid on the studies of influence of compositional heterogeneity on the morphology and properties of these segmented copolymers. It was found that the solution cast specimens of the more heterogeneous sample exhibit better segregation of segments, high crystallinity and melting temperature. They have higher thermal stability of mechanical properties at small deformations. However, they are less stable against large deformations and may become softer than the more homogeneous ones.     

丙环唑配合物的合成、缓释性能及生物活性研究

Five propiconazole(L) complexes (ML₂Cl₂, M=Zn(Ⅱ), Cu(Ⅱ), Co(Ⅱ); ML₄Cl₂, M=Ni(Ⅱ), Mn(Ⅱ)) were prepared and characterized by elemental analysis and IR. These complexes exhibited favorable controlled release property, it took 40 to 120 hours to release 85% amount of ligand in the water. The toxicity determination to Botrytis cinera, Rhizoctonia cerealis, Gibberella zeae, Fussrium moniliforme and Colletotrichum orbiculare indicated that the fungicidal activities of the complexes were better than that of the ligand except Mn-complex to Rhizoctonia cereali. The EC50 of Zn-propiconazole were 0.045 2～0.144 1 μg·mL^-1, Co- and Ni-propiconazole were 0.066 3～0.210 4 μg·mL^-1 and 0.183 9～0.340 7 μg·mL^-1, respectively, and Mn-propiconazole were only 0.353 6～0.538 0 μg·mL^-1. The growth regulation experiment to wheat seeding by dressing treating indicated that inhibiting activities of the complexes to root length and stem height were weaker than that of the ligand.     

还原温度对超细K－Co－Mo催化剂合成低碳醇性能的影响

 用溶胶－凝胶法合成了K－Co－Mo催化剂．样品经不同温度还原后，用于低碳醇的合成．XRD和HRTEM结果表明，样品是超细粒子，粒子尺寸为2～5nm．考察了催化剂的还原温度和反应条件对催化剂性能的影响．实验结果表明，还原温度对催化剂的活性有较大的影响，最佳还原温度为500℃．最佳反应温度范围为310～330℃．升高压力和空速可以提高醇的收率和选择性．在空速14400h－1，压力6．0MPa和温度310℃的条件下，醇的选择性为55．8％，收率为520．0g／（kg·h），MeOH／C2＋OH为0．27．催化剂稳定性良好，在200h的寿命实验中，活性基本不变．与文献中催化剂相比，超细K－Co－Mo催化剂对合成醇具有较高的活性和选择性，尤其是对C2＋OH的合成明显高于其他合成醇催化剂体系．     

Analysis of 17β-Estadiol from Sewage in Coastal Marine by Surface Plasmon Resonance Technique

In this study, surface plasmon resonance （SPR） for monitoring 17β-eatradiol （E2） was developed. The small molecule E2 was immobilized on a CM5 sensor chip for an indirect competitive immunoassay to detect E2. The SPR response bahed on the antigen-antibody reaction was measured by injecting the sample solution into the flow system. The limitation of detection was 0.445 μg/L. The developed SPE-SPR system was applied to analyze the seawater samples. Recovery of E2 was 91.6%-93. 1%. Relative standard deviations（RSD） for the E2 assay were between 10.9%-15.1% （n = 3）. The range of determination of E2 samples from the sewage in the coastal marine environ-ment was between ND（lower than detection limit） and ca. 11.78 ng/L.     

毛细管电泳安培检测扑热息痛及其水解物

研究了各种电化学预处理条件下碳纤维电极对扑热息痛及水解物的电化学行为。确定该体系最佳预处理条件为０．２Ｖ电位下阳极化１ｍｉｎ，再于－２．０Ｖ下阴极化１０ｓ。预处理后的碳纤维伏安响应得到明显提高。运用最佳条件并在支持电解中加入添加剂后，扑热息痛及其水解物在毛细管电泳上获得很好的分离和检测。其中扑热息痛的检测下限为２．７８ｐｇ；对氨基酚为１．８４ｐｇ。     

A Two-dimensional Lanthanide Coordination Framework with a New Amide-type Tripodal Ligand, 2,2′,2＂-Nitrilotris{[（2′- benzylaminoformyl）phenoxy]ethyl}amine

The La(III) complex with a new amide‐type tripodal ligand,2,2′.2″‐nitrilotris{[(2′‐benzylaminofomyl)‐phenoxylethyl)amine (L), was synthesized and characterized by X‐ray crystallographic analysis. Crystal data: C₄₈H_55.50LaN₇O_18.75, M_r=1169.40, monoclinic. space group, P2₁/n, a= 1.0644(3) nm. b=2.3889(5) nm, c= 2.1917(5) nm, β=90.65°, V=5.573(2) nm³, Z=1, D_c=1.394 g°cm^?3, R₁=0.0487, wR [1>2s?(I)]=0.1266. The results reveal that each La(III) ion binds to 9 oxygen atoms, three of which belong to carbonyl groups from three tripodal ligands and six to three bidentate nitrate groups and a two‐dimensional sheet of 4.8² networks is assembled by metal‐ligand coordination interaction. L, a heptadentate compound, merely acts as a tridentate bridging spacer due to its steric hindrance and links the La(III) ions as three‐connected nodes.