均分散超微细α-Fe2O3水溶胶的制备

均分散微米、亚微米或纳米级α-Fe_2O_3的制备包括静态水解法［1－3］、沸腾回流水解法[4]以及微乳液反应法[5]．随着粒子尺寸的减少,则体系具有明显的表面和体积效应[6]以及光电化学性质[7]．预计均分散超微细α-Fe_2O_3将会在催化、材料等许多新技术领域获得重要的应用．但以FeCl3为原料的水解法,Fb3十浓度一般在0．02－0．04mol·L－1很窄的浓度范围之内,超出该浓度范围将得到足β-FeOOH而不是α-Fe_2O_3[8]．以Fe（NO3）3为原料,虽然Fe3十浓度可增至0．2mol·L－1,但随之而来的不利因素：（1）水解时间增加几倍;（2）产率…     

国家标准方法测定土壤中总砷消解方法的改进

正随着现代工农业的快速发展,城镇和农村生活水平不断提高,土壤中砷的污染日益严重。准确、快捷、有效地测定土壤中砷的含量,成为近年来土壤分析方法研究的重要内容。目前土壤样品中砷前处理方法主要有硝酸-硫酸-高氯酸混合酸电热板消解法[1]、盐酸-硝酸-水(3+1+4)混合液水浴消解法[2-4]、微波消解法[5-7]和程序控温石墨消解法[8]等。     

电化学溶解钛金属直接水解法制备纳米TiO_2

纳米材料是目前材料科学的热点 .TiO2作为一种重要的无机功能材料 ,具有温敏、气敏、光催化等功能 ,广泛用于光电材料、涂料、传感器、介电材料、催化剂及载体等重要领域 .由于其各种应用都与粉体的性能有直接关系 ,因此研究纳米 TiO2的制备方法具有重要的实际意义 [1].近年来 ,纳米 TiO2粉体制备方法有了很大的发展 ,如 TiCl4气相水解沉淀法 [2],乳浊液法和 Ti(OC4H9)4水解沉淀法 [1],喷雾热解法 [3],放电爆炸法 [4],反应电极埋弧法 [5],溶胶凝胶 (Sol gel)法 [6]等 ,其中溶胶凝胶法是制备纳米材料的有效方法 .但这些方法存在…     

2001年全国高中学生化学竞赛(决赛)理论试题

第1题绿矾(化学式FeSO1-7H2O)是硫酸法生产钛白粉的主要副产物,每生产1吨钛白粉,副产4．5～5．0吨绿矾,目前全国每年约副产75万吨,除极少量被用于制备新产品外。绝大部分作为废料弃去,对环境造成污染。因此开发综合利用绿矾的工艺,是一项很有意义的工作。某研究者提出如下图所示的绿色工艺流程。     

反胶束法合成氧化锌微晶及其荧光特性

0引言材料的结构(微结构)、尺寸和形貌等因素对其特性及其实际应用具有重要的影响。对无机材料特别是氧化物半导体进行结构控制的研究近年来引起了人们极大的关注。氧化锌作为一种宽带隙(3.2eV)半导体材料,可广泛应用于压电材料、气体传感器、橡胶添加剂和光学器件等领域,而且还因其在室温下可产生激射现象使其成为纳米光学材料研究领域中的一大热点[1￣6]。目前,除了传统的固相-气相(V S)反应外,用于氧化锌微晶的制备方法主要有共沉淀法[7]、多羟基化合物水解法[8]、有机金属气相沉积法[9￣12]和水热法[13]等。通过选择不同的制备方法和…     

纳米银的电化学合成

纳米颗粒因具有量子尺寸效应、表面效应和宏观量子隧道效应等不同于晶态体材料和单个分子的固有特性 ,显示出体材料不具备的导电特性、光电特性、光催化能力及随粒径变化的吸收或发射光谱 ,已被用于各种发光与显示装置[1] .其制备的化学方法主要有溶胶 -凝胶法、微乳法、化学沉淀法和醇解法等 [2 ] .近年来 ,新发展出一种电化学合成纳米粒子的方法 ,如 Braun等 [3]利用 DNA模板电化学合成了银纳米线 ,Yu等[4 ] 用电化学合成了金纳米棒 ,Zhu等[5] 利用超声电化学合成了半导体 Pb Se纳米粒子 ,Amigo等 [6 ]用电化学方法合成了 Fe-Sr氧化…     

溶剂热法制备钴微球及其表征

<正>0引言过渡金属钴以及它的一些氧化物,以其特殊的电、磁和光学性能被广泛应用到信息存储[1]、催化剂[2]、磁光材料[3]、铁磁流体[4]以及生物医学[5]等诸多领域。前人曾经用羰酰钴热解法[6-7]、γ射线照射法[8]、光刻气相沉积法[9]、电化学沉积法[10]和金属盐溶液的     

高分子保护沉淀法制备超细纳米氧化镁

纳米氧化镁具有不同于本体材料的光、电、磁、化学特性,特别是超细纳米氧化镁由于其颗粒直径小、比表面积大,具有高纯度、高硬度和高熔点,高的反应活性,强吸附性,良好的低温烧结性,高电阻率等优良性质,可用于高绝缘材料,高质量的陶瓷材料,高性能阻燃纤维,环境保护的吸附剂、负载型甲醇和低碳醇合成的催化剂载体等领域,是一种有广泛应用价值的新型无机材料[1￣5]。已见报道的纳米氧化镁的制备方法有电子束蒸发法[6]、化学气相沉积法[7]、金属醇盐水解法,化学沉淀法[8,9],固相法[10],燃烧法[11],溶胶-凝胶法[12,13]等,然而由于氧化镁容易发生…     

纳米ZnO的制备及光催化活性的研究

纳米ZnO由于它的电子结构的特性和潜在的应用受到广泛的关注[1].ZnO既是一个典型的催化材料,又是一类非常有代表性的电化学,光化学半导体材料[2].ZnO的制备国内外有不少报道,如溶胶凝胶法[3]、喷雾干燥法[4]、超声辐射沉淀法[5]等.……     

热处理对SILAR法制备CuInSe_2薄膜性能的影响

0引言铜铟硒(CIS)具有合适的带隙、高光吸收系数、适当的电荷密度和迁移率,是一种用于薄膜太阳能电池的备受关注的吸收材料[1]。目前CuInSe2薄膜已采用多种方法进行制备,如金属前驱体硒化法[2]、共沉积法[3]、溅射法[4]、电沉积法[5]和化学气相沉积法[6]等。这些方法都有各自的     

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.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

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.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.