水热改性对NiMo/γ-Al2O3加氢脱氮催化剂结构及性能的影响

The influence of hydrothermal modification on the structure and hydrodenitrogenation (HDN) activity of NiMo/γ-Al₂O₃catalyst was studied in the range 140～180 ℃. The experimental results indicated that the hydrodenitrogenation reaction rate of pyridine was accelerated using the NiMo/γ-Al₂O₃catalyst synthesized via hydrothermal route due to the change of the structure, the increase of the amount of Mo and Ni and the rise of the specific surface area. The change of the structure of catalysts was enhanced at higher hydrothermal temperature, producing NiMo/γ-Al₂O₃catalyst with better HDN activity.     

含芳硫基的新三唑类化合物的合成及生物活性研究

许多三唑类化合物具有优良的杀菌和植物生长调节活性 ,如三唑酮、三唑醇、烯效唑、烯唑醇等 ,对常见真菌病害具有很好的防治效果 ,并具有增产、抗倒和生长调节作用 ,已成为重要的杀菌剂类型 [1] .为筛选新型高活性三唑类杀菌剂和探讨其活性与结构间的关系 ,我们利用生物等排体理论以常规三唑类杀菌剂三唑酮为先导物设计合成了 1 6个含芳硫基的新三唑类化合物 ,其合成路线如下 :RCCH2 BrO+HNNNB NRCCH2O NNHAC-Na ACBr2NRCCHOBrNN(1 ) (2 ) (3 )3 +SH 　R′B NRCCHOS　R′NN　 (4 )RCCH2 CH2 NMe2 .HClO+HNNNH2 O…     

Preparation,lithiation and transformation of N-(benzotriazol-1-ylmethyl) heterocycles

Indole, carbazole, pyrrole, imidazole, benzimidazole, 2-methyl- and 2-phenylbenzimidazole, and 1, 2, 4-triazole have each been converted into their N-(benzotriazol-1-ylmethyl) derivatives. The pyrrole, indole, and carbazole adducts undergo smooth lithiation at the inter-ring methylene group and subsequent reaction there with electrophiles. For the imidazole, benzimidazole, and triazole systems, lithiations at other molecular positions competed.     

单分散纳米微粒制备方法研究进展

单分散纳米微粒既可以在严格控制的条件下直接制备，也可以通过对多分散纳米微粒体系进行分级分离获得。本文在总结近年来国内外单分散纳米微粒的研究工作的基础上，介绍了直接制备和分级分离这两种获得单分散纳米微粒的方法。     

Novel hydrogen-bonded three-dimensional network complexes containing cobalt-pyridine-2,6-dicarboxylic acid

The novel complex, Co(H₂O)₅[Co(2,6-pydc)₂] (1) has been prepared in aqueous solution and characterized by single-crystal X-ray diffraction, elemental analyses and i.r. spectra. X-ray structural analysis revealed that three novel compounds each possess both – stacking and hydrogen-bonding interaction three-dimensional (3-D) networks.     

含吡唑啉酮三脚架结构的化合物及其稀土配合物的合成、表征及荧光性能

合成了一种含吡唑啉酮的三脚架结构化合物 1,1,1 三 { 1′ [2′ 氧杂 5′ 氧代 5′ ( 1″ 苯基 3″ 甲基吡唑啉酮 4″ 基 )戊基 ] }丙烷 (H3 L)及其 7个稀土配合物。通过元素分析、摩尔电导、质谱、红外光谱、核磁共振谱、荧光光谱等对H3 L及其稀土配合物的组成及性质进行了表征。分析结果表明 :H3 L的分子式为C45H50 N6O9,配合物的组成比为REL·0 5H2 O (RE =La ,Sm ,Eu ,Gd ,Tb ,Dy ,Yb) ;该三脚架形配体分别以醚氧、烯醇氧及吡唑酮环上的羰基氧与稀土离子进行配位 ,形成内配型配合物。荧光光谱分析表明SmL·0 5H2 O ,EuL·0 5H2 O ,TbL·0 5H2 O ,DyL·0 5H2 O配合物具有三价稀土离子的特征线状荧光 ,其中TbL·0 5H2 O的荧光强度最强 ,表明T(配体 )→5D4(Tb)能级更为匹配 ,从而进行分子内能量有效传递 ;由EuL·0 5H2 O的荧光光谱图形推测 ,Eu3 +离子在该配合物中处于非对称中心     

草酸钙结石形态的红外光谱分析

草酸钙结石主要是以一水草酸钙(COM)、二水草酸钙(COD)的形式存在。在解决缺少COD标样的难题后,将制备的COD样品与COM标样混合,然后采用红外光谱法对混合物进行分析研究,采用谱带比值法,确定了COD和COM在660和610 cm-1处与780和520 cm-1处的吸收度比值(R)与质量分数(w)的关系式,其线性回归方程分别为:R=11.95×10-3wCOD 0.873 61,r=0.983 63;R=4.74×10-3wCOD 0.886 52,r=0.992 44。同时为了减少压片、测定等因素引起的误差,采用零点交叉一阶导数法,测定在1 320 cm-1处吸收度一阶导数与COD质量分数(w)的关系式,其线性回归方程I=5.5×10-5w 9.2×10-5,r=0.996 60。线性良好。     

阿斯美胶囊中四种组分的高效液相色谱分析

建立了反相高效液相色谱法测定阿斯美胶囊中氨茶碱、盐酸甲氧非那明、马来酸氯苯那敏及那可汀四种组分的含量。色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ８，５μｍ，２００ｃｍ×４０ｍｍＩＤ，流动相为体积分数０５％的三乙胺溶液（磷酸调节ｐＨ５５）＋乙腈＋甲醇（５５０＋３６８＋８２），检测波长为２６４ｎｍ，线性范围分别为：氨茶碱３１２５～２５０ｍｇ／Ｌ，γ＝０９９９６，盐酸甲氧非那明１５６２５～１２５０ｍｇ／Ｌ，γ＝１００００，马来酸氯苯那敏２５～２００ｍｇ／Ｌ，γ＝０９９９９，那可汀８７５～７００ｍｇ／Ｌ，γ＝０９９９９；回收率（ｎ＝３）分别为１０１２％，１００８％，９９９％，９９５％；精密度：日内平均ＲＳＤ（ｎ＝６）分别为０７％，０４％，０４％，０６％；日间平均ＲＳＤ（ｎ＝３）分别为１０％，１０％，１１％，１２％。     

模板组装Fe纳米线阵列及其微结构

铝在硫酸溶液中经直流阳极氧化,得到多孔铝阳极氧化膜(AAO). 以AAO膜为模板,通过交流电沉积的方法,在AAO模板孔内成功组装了Fe纳米线.TEM分析表明,Fe纳米线的长度约为2.5 μm,其长度分布十分均匀；粗细均匀,直径约为25 nm. XRD实验分析证实,所制备的Fe纳米线为α-Fe.选区电子衍射（SAED）实验分析表明,α-Fe纳米线具有单晶结构.     

Effects of mixed H2O‐CH3CN solvents on the rate of hydrazinolysis of N‐phenylphthalimide: Spectral and kinetic evidence for the occurrence of N‐aminophthalimide on the reaction path

Kinetic study on the cleavage of N‐phenylphthalimide (NPhPT) in the presence of 0.05 M NH₂NH₂ and mixed H₂O‐CH₃CN solvents reveals the occurrence of reaction scheme where A, B, C, C₁, An, E, and F represent NPhPT, o‐CO^?₂C₆H₄CONHC₆H₅, o‐CONHNH₂C₆H₄‐ CONHC₆H₅, N‐aminophthalimide, aniline, o‐CO^?₂C₆H₄CONHNH₂, and o‐CONHNH₂C₆H₄‐CONHNH₂, respectively. But, in the presence of either nonbuffered ?0.20 M NH₂NH₂ hydrazine buffer of pH ～7.30–8.26 with total buffer concentration ([Buf]_T) of >0.02 M, further conversion of F to 2,3‐dihydrophthalazine‐1,4‐dione (DHPD) has been detected depending upon the length of the reaction time (t), the values of [Buf]_T, and pH. It has been shown that the rate of conversion of C₁ to F is much faster than that of C to C₁ which is much faster than that of F to DHPD. The reaction step A → C involves general base (GB) catalysis, while step C → C₁ seems to involve specific base–general acid (GA) and GB‐GB catalysis. © 2005 Wiley Periodicals, Inc. Int J Chem Kinet 37: 147–161, 2005