过氧铌杂多配合物位置异构体的合成、表征及催化性能

合成了6种钨硅杂多配合物异构体α、β_i-M₃H₂[SiW₁₁(NbO₂)O₃₉]·H₂O(M=Me₄N⁺(TMA),Bu₄N⁺(TBA),Et₄N⁺(TEA);β_i=β₁,β₂,β₃)。IR光谱、UV光谱、极谱、I^--S₂O₃^2-滴定证明合成的杂多配合物中有NbO₂基存在, ¹⁸³W NMR光谱证明其阴离子具有Keggin结构,催化实验结果表明,合成的化合物对烯烃环氧化反应具有催化活性,且过氧杂多配合物的催化活性高于非过氧杂多配合物,β异构体的催化活性高于α。     

纳米碳酸锌的制备和热分解动力学参数的测定

Nanosized zinc carbonate was prepared in the droplet of nano-reactor based on microemusion. The influences of the concentration of the surfactant and reactant on the diameter of nanoparticles were studied and the kinetic pa-rameters of thermal decomposition reaction were determined. It can be shown from experimental results， the di-ameter of the droplet in the microemulsion which have dissolved reactant zinc nitrate and sal volatile is between 4.9nm and 7.7nm， 6.2nm and 12.4nm， respectively. Nanosized zinc carbonate prepared by the method of mi-croemusion has shown good dispersion， narrow distribution and light agglomeration. The particle size of nanosized zinc carbonate is between 5nm and 40nm， and its kinetic parameters of thermal decomposition reaction-activation energy E and reaction order n are 110kJ·mol^-1 and 0.9， respectively.     

纳米氧化铜的制备及常温脱硫效能研究

采用硝酸铜为原料、氢氧化钠溶液为沉淀剂、使用体积比为1∶1的乙醇-水溶液为分散剂的直接沉淀法制备，通过改变工艺条件得到了三种纳米氧化铜产品，平均粒径分别为25.63，10.74和7.57 nm。采用TG-DTA、FIR、XRD和TEM等对纳米氧化铜进行表征。对产品的常温脱硫活性进行了穿透试验，并与已开发的其他常温精脱硫产品进行了比较，结果表明纳米氧化铜应用于H₂S脱硫，可在常温条件下具有优异的脱硫活性，对H₂S的脱除精度可以达到0.05 mg·m^-3以下。经过优选，产品在3 000 h^-1空速下穿透硫容达到25.3%，高于同类型的其他脱硫剂产品。     

碲氢化钠与胺烷基化苯并三氮唑的反应

碲氢化钠是一个用途广泛的磁试剂,自作为有用的去溴试剂以来,日益受到化学工作者的关注,不断有文献报道它的合成及应用.例如能有效地还原卤代烃、硝基化合物、叠氮化合物和亚胺等.近年来,Katritzky报道了胺烷基化苯并三氮唑衍生物的合成及应用,此衍生物中的苯并三氮唑基是很好的离去基团,易被各种亲核试剂所取代.我们在前文中对硒氢化钠与胺烷基化苯并三氮唑反应生成二苄基二硒醚的合成进行了报道.本文用碲氢化钠与胺烷基化苯并三氮唑反应,结果生成还原产物N-取代胺.     

ZnO对Ag/SiO2催化剂银的分散作用及对吲哚合成稳定性的影响

将ZnO助剂加到由苯胺和乙二醇一步合成吲哚的Ag/SiO2催化剂中,发现ZnO助剂能大大提高催化剂的稳定性.XRD和TEM表征首次得到:ZnO是结构型助剂,它能使银很好地分散在SiO2表面上,并可有效地抑制反应过程中银粒子的烧结.     

四（五氟化苯基）卟啉氯化铁选择催化氧化超临界丙烷的反应机理

 以BHT为自由基捕捉剂，研究了四（五氟化苯基）卟啉氯化铁（Ⅲ）将超临界丙烷高选择性催化氧化为丙醇的反应机理．通过GC－MS分析发现，反应产物中有PBHT，故可认为在超临界丙烷氧化反应过程中有丙基自由基存在，初步推断反应涉及自由基机理．同时发现高浓度BHT抑制反应，低浓度BHT促进反应的现象，而以戊烷为底物时没有促进作用．这是由于BHT的位阻效应所致．并对BHT存在时超临界丙烷氧化反应机理进行了初步的推断．     

超声波作用下5, 5-二取代乙内酰脲的合成

本文以氰化钠水溶液、碳酸铵和相应的醛或酮为原料, 于25℃~45℃超声波作用3~4h合成八种5, 5-二取代乙内酰脲, 收率30.1~100%。与传统方法比较, 反应时间缩短, 产品收率提高。     

Molecular Spectroscopic Study on the Interaction between Heparin and Neutral Red

The interaction between heparin and neutral red was investigated by molecular spectroscopic methods. The change of all spectra suggested that positively charged neutral red had interacted with negatively charged heparin. The study of influence factors indicated that electrostatic force and hydrophobic bond might be involved in the interaction. The total binding number per disaccharide unit and intrinsic binding constant were obtained using Scatchard model.     

A Novel Green Preparation of a, a''''-Bis (substituted benzylidene)-cycloalkanones Promoted by FeCl_3 6H-2O in Ionic Liquid

a, a'-Bis(substituted benzylidene)cycloalkanones were efficiently prepared from cycloalkanones and benzaldehydes in [bmim][BF4] by using iron(III) chloride hexahydrate as a catalyst. It is shown that [bmim][BF4] and iron(III) chloride hexahydrate can be quantitatively recovered and be reused effectively for many times. Compared with the known methods, this novel process has the advantage of being an envkonmentally benign process together with good yields and mild reaction conditions.     

石墨炉原子吸收光谱法直接测定血样中硒

用石墨炉原子吸收光谱法，以硝酸铜和硝酸铵为基体改进剂，塞曼效应扣背景，采用标准加入法可直接测定血样中硒，回收率为95％～105％，相对标准偏差为5．8％，检出限为96pg，测定结果准确可靠。