水溶性染料在PbTiO3体系中的光催化降解

以PbTiO₃为光催化剂,对多种水溶性染料的光催化降解反应进行了研究,结果表明：光降解脱色效率与染料溶液的pH值、光照时间、光源种类及催化剂用量等因素有关.染料溶液浓度为10mg/L,pH=6,催化剂用量为100mg/50mL,直接以太阳光作光源,光照1h以后,脱色率达90%以上,有机染料中硫和氮元素转化为SO₄^2-和NO₃^-的生成率分别为85%和65%.     

钙钛矿型复合氧化物LaFeO3和LaCoO3的光催化活性

采用柠檬酸法合成了钙钛矿复合氧化物ＬａＦｅＯ３和ＬａＣｏＯ３,并以其为光催化剂对水溶性染料进行光催化降解实验,研究了不同光源和不同光照时间对降解脱色率的影响。结果表明ＬａＦｅＯ３和ＬａＣｏＯ３均有较强的光催化活性,而ＬａＣｏＯ３的光催化活性明显高于ＬａＦｅＯ３,这主要与Ｆｅ＾３＋和Ｃｏ＾３＋离子的电子构型以及Ｆｅ－Ｏ间和Ｃｏ－Ｏ间的结合能有关。     

丙醛均相催化加氢制丙醇的研究

系统地研究了在４．０ＭＰａ氢压下，反应温度、催化剂浓度、溶剂等对丙醛均相加氢制正丙醇反应的影响，得出最佳反应条件为：氢压４．０ＭＰａ、温度８０℃，ＲｕＣｌ３·３Ｈ２Ｏ为催化剂前体，用量９８ｍｇ（０．３５ｍｍｏｌ），ＰＰｈ３为３９３ｍｇ（１．５ｍｍｏｌ），Ｒｕ／Ｐ摩尔比为１／４，ＤＭＦ为溶剂．在此条件下，丙醛转化率和正丙醇选择性可分别达９９％和９５％以上．求出了不同反应温度下的反应速度常数．以ＲｕＣｌ３－ＰＰｈ３为催化剂体系，丙醛加氢的活化能为７７．６２ｋＪ／ｍｏｌ     

CaO／La2O3催化剂上的甲烷氧化偶联反应的研究

研究了不同配比的ＣａＯ／Ｌａ_２Ｏ_３催化剂对甲烷氧化偶联反应的催化性能。适当配比的ＣａＯ／Ｌａ_２Ｏ_３催化剂的性能明显优于纯Ｌａ_２Ｏ_３或ＣａＯ，在钙含量为２４％和８１％（Ｃａ／（ｃａ＋Ｌａ））处，Ｃ_２选择性和Ｃ_２收率分别出现两个峰值。同时还发现，１３％ＣａＯ／Ｌａ_２Ｏ_３样品显示出良好的低温催化性能，在５５０℃反应温度下获得了３１．５％的甲烷转化率和４５％的Ｃ_２选择性。并采用ＸＲＤ、ＸＰＳ和Ｃｏ_２ＴＰＤ等技术研究了催化剂的结构。结果表明，ＣａＯ／Ｌａ_２Ｏ_３体系催化剂上没有检测到新物相产生。但是，催化剂中ＣａＯ与Ｌａ_２Ｏ_３两组分之间存在着相互作用，有利于表面活性中心的形成。     

K+-SrO-La2O3/ZnO催化剂上甲烷氧化偶联反应Ⅱ.催化剂碱性和氧物种的表征

Ｋ＾＋－ＳｒＯ－Ｌａ２Ｏ３／ＺｎＯ（ＫＳＬＺ）催化体系具有很好的催化活性。在１０７３Ｋ反应温度下，其Ｃ２产率为１８．２％，用Ｃ２选择性为６８．３％。催化剂抗潮能力明显增加，在室温下经长期主和置后，催化剂活性稳定。     

担载铂催化剂用于硝基苯催化加氢制对氨基苯酚的研究

研究了以活性炭、γＡ１２Ｏ３、γ－Ａ１２Ｏ３－ＴiＯ２为载体,用浸渍法制备的铂含 量为１％的担载铂催化剂,用于硝基苯催化加氢制对氨基苯酚。发现Ｐｔ／γ－Ａ１２Ｏ３－ＴiＯ２催化剂有较高的活性、选择性和较长的寿命,催化剂循环使用１０次后,对氨基酚的率仍高于８０％,优于常用的Ｐt／Ｃ催化剂 。测定了催剂的比表面积、孔结构以 及活性金属铂的分散度,发现孔结构与催化剂性能之间没有规律性的关系;而铂在γ－Ａ１２     

Ce2O—TiO2／SiO2的制备及除氟性能研究

以ＳｉＯ２为基质，ＣｅＯ２ＴｉＯ２为包覆物质，采用溶胶凝胶法制备ＣｅＯ２ＴｉＯ２／ＳｉＯ２表面复合物，并对所制复合物进行除氟测试。用扫描电镜（ＳＥＭ）观察表面形貌，讨论实验环境、试剂用量等因素对ＣｅＯ２ＴｉＯ２／ＳｉＯ２制备及除氟性能的影响，结果表明：ｎＴｉ（ＯＣ４Ｈ９）４／ｎＣｅＣｌ３·７Ｈ２Ｏ＝１、ｎＣＨ３ＣＯＯＨ／ｎＴｉ（ＯＣ４Ｈ９）４＝４５、ｎＣ３Ｈ８Ｏ３／ｎＴｉ（Ｏ４Ｈ９）４＝０３、ＲＨ＝９５％，热处理温度１１０℃时，所制ＣｅＯ２ＴｉＯ２／ＳｉＯ２对Ｆ－的吸附容量（ｑ）为２１４ｍｇ／ｇ，去除率（Ｅ）为８５６％。     

单柱离子色谱法测定痕量草酸根离子

本文采用单柱离子色谱系统测定了Ｃ２Ｏ＾２－４，以１．３ｍｍｏｌ／Ｌ葡萄糖酸钠／１．３ｍｍｏｌ／Ｌ硼砂为淋洗液测定Ｃ２Ｏ＾２－４，８常见阴离子Ｃｌ＾－，ＮＯ＾－３，ＨＰＯ＾２－４，ＳＯ＾２－４不干扰测定，Ｃ２Ｏ＾２－４的检出限为０．５７ｍｇ／Ｌ，相对标准偏差为１．０７％，工作曲线的线性范围为０．５７－５００ｍｇ／Ｌ，应用本方法测定了加Ｃ２Ｏ＾２－４的自来水样，Ｃ２Ｏ＾２－４的回收率为９９．５２％。     

甲烷部分氧化制合成气

对镍铜甲烷部分氧化催化剂的制备化学研究表明，在Ａｌ２Ｏ３、ＳｉＯ２、ｍｇＯ、ＴｉＯ２、Ｙ型分子筛等载体中，具有较好氢溢流功能的Ａｌ２Ｏ３所担载的镍铜催化剂，有最佳的反应性能、载体的产物溢物功能对反应中合成气的生成是有利的，对ＮｉＯ－ＣｕＯ－Ａｌ２Ｏ３催化剂，组分Ｃｕ的最佳含量是Ｃｕ／Ａｌ＝０．２／４（原子比），Ｎｉ／Ａｌ（原子比）在１／４－１．５／４范围内催化剂均保持最佳的反应性能，此时，甲烷转化     

催化动力学光度法测定药物和饮用水中痕量铁的研究

本文利用Ｆｅ＾３＋＋对Ｈ２Ｏ２氧化二苯胺碘酸的反应具有催化作用，且在一定条件下显色反应的速度与催化剂Ｆｅ＾３＋的含量成正比的原理，建立了一种痕量铁的分析方法。本文方法的线性范围为０．００８－０．０６４ｍｇ＝Ｌ，相对标准偏差小于５．０％，标准加入回收率为１０１％－１０３％，检出限为０．００６７３ｍｇ／Ｌ。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp³)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp²)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp²)?H and aliphatic 1,5- and 1,6-C(sp³)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp³)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp²)?H insertion.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y₁ and Y₂. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described.     

正丁胺对激光染料荧光谱影响的研究

用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu⁰ as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than Cu^I in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C₆₀, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine.