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锐钛矿型纳米TiO2介孔粉体表面织构的研究 总被引:13,自引:0,他引:13
以硫酸钛和尿素为原料,聚乙二醇-1000为空间构造剂,104℃下经尿素水解均匀沉淀法研制颗粒分散均匀、粒径可控的高热稳定性锐钛矿型纳米TiO2介孔粉体,并对其晶相、颗粒大小、比表面积、形貌和孔道结构进行了表征.结果表明,未经任何热处理的TiO2粉体即为锐钛型晶相,颗粒为均匀分散的类球型颗粒,且颗粒间形成直通型的介孔孔道,其孔径在10~30nm之间.控制焙烧温度可以达到控制颗粒大小及形貌的目的,经850℃焙烧5h的样品仍保持锐钛矿型晶相,未出现向金红石型晶相转变的迹象. 相似文献
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低温苯甲醇醇解法制备高活性锐钛矿型纳米晶TiO2光催化剂 总被引:5,自引:0,他引:5
以TiCl4 为钛源,采用低温苯甲醇醇解法制备了不同粒径及晶相组成的大表面TiO2纳米晶,利用X射线衍射、热重-差热分析、透射电子显微镜、拉曼光谱、紫外-可见漫反射光谱和N2物理吸附等方法考察了焙烧温度和焙烧时间对其晶相组成、晶粒尺寸、比表面积及孔体积等微结构性质的影响,并以苯酚的光催化降解为模型反应评价了样品的光催化活性. 结果表明,未经任何热处理的TiO2样品即为锐钛矿晶相,控制焙烧温度及焙烧时间可进一步调控样品的粒径、比表面积、晶相结构及表面氧缺位浓度. 经400 ℃焙烧3 h制备的纳米晶TiO2具有最佳的光催化活性,其活性比商用Degussa P-25 TiO2更高. 相似文献
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采用正交试验方法,调控Ti(SO4)2原料浓度、沉淀剂NH4HCO3浓度、沉淀pH值、焙烧温度和焙烧时间等制备条件制备得到了25个锐钛矿相TiO2光催化剂.对TiO2光催化降解十二烷基苯磺酸钠(SDBS)的催化活性与TiO2锐钛矿相10个晶面的法向粒子尺寸、晶格畸变应力、X射线衍射强度之间的关系进行了分析.发现TiO2光催化SDBS的降解遵循一级反应动力学;其主要影响因素为(101)晶面结晶情况,而与其余晶面的相关性不大;光催化反应需要晶格畸变较少的结晶较完整的(101)晶面;晶粒尺寸减小,比表面积增大有利于提高反应速率;光催化反应过程主要在结晶的锐钛矿相(101)晶面表面上发生,而无定形TiO2催化活性较低. 相似文献
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用TiO2,ZnO及Fe2O3纳米粒子光催化氧化庚烷的反应 总被引:8,自引:0,他引:8
制备了三种n-型半导体氧化物TiO2,ZnO和Fe2O3纳米粒子,用X射线衍射和N2吸附技术分别对它们的结构及比表面积进行了表征.考察了三种氧化物粒子对庚烷的气相光催化氧化反应的催化活性.研究表明,对于同种催化剂,随着焙烧温度的升高,催化剂的粒径增大,比表
面积减小,光催化活性下降.三种催化剂纳米粒子的光催化活性顺序为TiO2(锐钛矿)>ZnO>Fe2O3,金红石型TiO2粒子的催化活性低于ZnO粒子.结合能带理论探讨了三种催化剂光催化活性差异的原因. 相似文献
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超临界流体干燥法制备纳米TiO2-ZnO复合催化剂及其对苯酚降解的光催化性能 总被引:15,自引:0,他引:15
以TiCl4和Zn(NO3)2·6H2O为原料,采用溶胶-凝胶法结合超临界流体干燥法制备了纳米级TiO2-ZnO(7~10nm)复合催化剂,并用XRD和TEM等手段进行了表征.以苯酚光催化降解为模型反应对所制备催化剂的催化性能进行了评价.结果表明,与单组分TiO2及普通干燥法制备的TiO2-ZnO催化剂相比较,纳米TiO2-ZnO复合粒子的光催化活性有较大提高.用超临界干燥法制备的催化剂具有粒径小、分布窄、比表面积大、分散性好和光催化活性高等特点.采用超临界流体干燥法可直接制得纳米TiO2(锐钛矿型)-ZnO(非晶态)复合催化剂,可实现干燥、晶化一步完成.复合催化剂中ZnO的最佳掺入量为x(ZnO)=0.8%.超临界流体干燥法是制备纳米材料的一种新技术,具有产物容易收集和溶剂可回收利用等优点. 相似文献
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吸附相反应技术制备TiO2的结晶过程以及光降解气相甲苯 总被引:1,自引:0,他引:1
研究了吸附相反应技术制备纳米TiO2的结晶过程, 并探讨了该过程对TiO2光催化活性的影响. 利用XRD测定了不同温度和时间焙烧后TiO2的晶型以及晶粒粒径的变化, 发现即使焙烧温度高达900 ℃, TiO2仍维持纯锐钛矿晶型. 随着焙烧温度的增加, TiO2的晶粒粒径变化不大, 均在7 nm以下, 在焙烧温度高于700 ℃时, 锐钛矿结晶峰的峰面积随温度增加, 峰面积保持不变. 改变焙烧时间基本不影响TiO2的晶型和晶粒粒径, 因而其光催化活性变化也较小. 光降解气相甲苯实验表明, 700 ℃焙烧后样品的催化活性最高, 且优于商用P25光催化剂. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
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. 相似文献
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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. 相似文献
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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%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
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. 相似文献
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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. 相似文献
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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. 相似文献
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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. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
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 CuI 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). 相似文献
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George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(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. 相似文献