A Triformylphloroglucinol-based Covalent Organic Polymer: Synthesis,Characterization and Its Application in Visible-light-driven Oxidative Coupling Reactions of Primary Amines

A triformylphloroglucinol-based A₃B₂-typed covalent organic polymer(TFG-BPTH) was successfully constructed by the condensation reaction of triformylphloroglucinol(TFG) and 2,5-bis(2-propynyloxy)terephthalo-hydrazide(BPTH) under solvothermal conditions. The structure of the TFG-BPTH was confirmed by spectra techniques including FTIR and solid-state ¹³C CP/MAS NMR spectroscopy. The mophological features of TFG-BPTH were analyzed using scanning electron microscopy(SEM) and transmission electron microscopy(TEM). The TFG-BPTH possessed good thermal and chemical stability, and exhibited good photocatalytic activity as a metal-free heterogeneous catalyst for oxidation of amines to valuable imines under visible light irradiation using O₂ as green oxidant. In addition, the catalyst could be readily recovered from the reaction mixture by simple filtration and reused for at least five cycles without any observable change in structure and catalytic activity.     

多级孔道钛硅分子筛HTS-1的制备、表征及其氧化脱硫性能

以吐温40（T-40）为碳源,通过两步溶胶-凝胶法制得SiO₂/T-40干凝胶;干凝胶经温和炭化处理制得C-SiO₂复合物;以C-SiO₂复合物为介孔模板和硅源,四丙基氢氧化铵（TPAOH）为微孔模板,钛酸四丁酯为钛源,成功制备出多级孔道钛硅分子筛（HTS-1）,其结构和性能经FT-IR、 XRD、 UV-Vis、 SEM、 ICP-OES和N₂吸附-脱附表征。结果表明：HTS-1具有有序的微孔结构,以及相互连接的介孔以及大孔结构,且其介孔/大孔尺寸可通过T-40的加量调节;HTS-1在大分子有机硫化物的选择氧化反应中,表现出较高的催化活性。      

Synthesis and Characterization of a Novel One-dimensional Metal Organic Compound

1 INTRODUCTION Metal-organic compounds with open-frameworks are of intense interest due to their potential appli- ciations in the fields of molecular sieving, optical materials, zeolitic catalyses and so forth[1～9]. Addi- tionally, their functionality can be modified by chan- ging either the inorganic species or the organic li- gands in the structures. In the past decade, one di- mensional (1-D) infinite sructure with specific topo- logies has been obtained by assembly of suitable metal …     

新型无机/有机复合柱撑粘土材料的合成与表征

以无机TiCl4／HCl制成的钛基柱撑液和十六烷基三甲基溴化胺(CTAB)为有机改性液,通过控制两种柱撑液的加入顺序以及相对含量,利用蒙脱石粘土矿物层间域的特殊化学反应场所的特性,合成得到三类复合柱撑蒙脱石材料．X射线衍射结果表明,d001晶面由于CTAB与钛基水合离子的相互作用形成粒度不同的柱撑空间而表现为两个峰值．与FT-IR光谱相比,FT-Raman光谱能够更加有效地表征和鉴定复合柱撑粘土的结构差别．采用原土无机柱撑后再有机柱撑,可以合成层间距更大的复合柱撑粘土材料．经热处理后得到锐钛型氧化钛的改性粘土材料,并且可以重新合成得到无机／有机复合柱撑的新型改性粘土材料．这些合成手段为制备新型改性粘土材料应用于环保以及化工等方面提供了借鉴．     

用氧化偶联聚合法合成新型电活性聚酰胺及其结构表征

使用氧化偶联聚合的方法, 合成了一种新的电活性聚酰胺, 使其同时具有聚酰胺和聚苯胺性质. 该反应操作简便易行, 室温下即可进行. 通过红外光谱和核磁共振谱对其结构进行了表征, 用紫外-可见光谱和循环伏安法研究了氧化还原性质和电活性, 并测试了导电率.     

低价钛在有机合成中的应用新进展

主要综述了近年来低价钛诱导的McMurry反应在有机合成中的应用新进展.     

Synthesis and Characterization of Novel Polyamines Containing Different Substitute Groups Via Chemical Oxidative Polymerization

In this study, polymers of substitute aromatic amine compounds were synthesized by chemical oxidative polycondensation in aqueous alkaline medium using NaOCl as oxidant. The structures of synthesized compounds were confirmed by FT‐IR, UV‐Vis and NMR analyses. The characterizations of synthesized compounds were made by fluorescence, TG‐DTA, DSC, scanning electron microscopy (SEM) and Brunauer‐Emmett‐Teller (BET) surface area measurements. In addition, electrochemical and electrical conductivity values of compounds were carried out with cyclic voltammetry (CV) and four points probe technique measurements, respectively. Synthesized polymers viewed structural change, optical, electrochemical and thermal differences.     

新型烟酰胺-铕配合物的合成及性能研究

以烟酰胺和硝酸铕为原料,采用热溶剂法合成了烟酰胺-铕配合物的微纳米球。其结构和性能经红外光谱(IR)、热重(TG)、扫描电镜(SEM)、X-射线衍射(XRD)、元素分析(EDS)和荧光检测等表征。研究结果表明：配合物含有碳、氧、氮和铕等元素,其红外光谱图与烟酰胺配体有明显的差异;配合物的质量在250℃和550℃条件下出现了明显的下降,下降率分别为15%和19%; SEM照片显示配合物为大小不均一的微纳米球,且具有较好的荧光发光性能,发射峰位于579 nm, 591 nm, 612 nm, 618 nm, 693 nm和699 nm。烟酰胺配体和烟酰胺-铕配合物对肺癌人肺泡基底上皮细胞(A549细胞)的活性影响趋势一致,随着药物浓度升高,该细胞活性没有发生明显变化。     

Synthesis and Characterization of Novel Organic／Inorganic Hybrid Polymers Containing Polyhedral Oligosilsesquioxanes

Hybrid polymers, poly(vinyl pyrrolidone-co-isobutyl styryl polyhedral oligomeric silsesquioxanes)s (PVP-POSS) were synthesized by one step polymerization and characterized using GPC and DSC. Addition of POSS significantly increases the Tg of polyvinylpyrrolidone at a fair high POSS content and obtained high molecular weight polymers with very narrow molecular distribution. The POSS content in the resulted hybrids can be controlled by varying the POSS feed ratio.     

Synthesis and Characterization of Novel Poly-thiophene-nanoporous Silica and its Application for Mercury Removal from Waste Waters

In this work, MCM-41 (Mobil Composition of Matter number 41) nanoporous silica has been synthesized and characterized by X-ray powder diffraction and IR spectroscopy. In the next step, poly-thiophene was coated on the nanoporous silica in order to increase its surface area. This composite was characterized by X-Ray powder diffraction, High resolution transmission electronic microscopy micrograph (HRTEM), elemental analysis (CHNS) and Thermal analysis (TG/DTA). The application of this composite was investigated in mercury ions removal from waste water prior to determination by inductively coupled plasma atomic emission spectroscopy (ICP-OES). In order to investigate the effect of nanoporous structure on the efficiency of this composite, the same composite without porous structure has been synthesized and the results were compared.     

氧化偶联聚合的方法合成新型电活性聚醚砜及其结构表征

通过氧化偶联聚合的方法我们制备了一种新型电活性聚芳醚砜,这种聚合物主链上含有苯基封端的苯胺四聚体齐聚物单元。我们通红外、核磁和XRD对其结构进行了表征。在1.0M的硫酸水溶液介质中我们对其电活性进行了研究,聚合物展现出两对氧化还原峰。此外,我们使用TGA测试手段对其热稳定性也做了研究。在室温质子酸掺杂的条件下聚合物的导电率为1.37 × 10-7 S·cm-1。     

Synthesis and Characterization of a Novel Phosphonate Metal Organic Framework Starting from Copper Salts

Abstract

Increased interest in the area of metal phosphonate inorganic–organic frameworks is exemplified with a high range of applications and a rich synthetic and structural chemistry of these compounds. The synthesis and potential applications of a novel metal phosphonate, namely Cu(II) phenylvinylphosphonate (PVP) is described in this paper. Syntheses were performed starting from a 1:1 molar ratio of a Cu(NO₃)₂·6H₂O or CuSO₄·5H₂O and 1-phenylvinylphosphonic acid under hydrothermal conditions at pH values ranging between 2.8 and 3.1. The influence of different counterion for the copper salt used as the Cu(II) source on the structure and crystallinity of the final product was studied. The obtained copper(II) phenylvinylphosphonate compounds were characterized by X-ray powder diffraction, FT-IR spectroscopy, scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and energy-dispersive X-ray spectrometry (EDAX). A possible crystal structure for the copper (II) phenylvinylphosphonate products is proposed using semiempirical approaches.     

Synthesis and Characterization of Mesoporous Titanium Dioxide Spheres

Mesoporous titanium dioxide spheres were synthesized by a convenient solvothermal method at room temperature with tetraethyl titanate as a precursor. Investigation by means of X-ray diffraction(XRD), transmission electron microscopy(TEM), scanning electron microscopy(SEM), and N2 adsorption-desorption isotherms confirms that the sample has a mesostructure with a higher specific surface area and shows that the mesoporous TiO2 spheres have a diameter of 2 μm, the average pore size is about 5.9 nm, and the BET...     

Naphthochromenones: Organic Bimodal Photocatalysts Engaging in Both Oxidative and Reductive Quenching Processes

Twelve naphthochromenone photocatalysts (PCs) were synthesized on gram scale. They absorb across the UV/Vis range and feature an extremely wide redox window (up to 3.22 eV) that is accessible using simple visible light irradiation sources (CFL or LED). Their excited‐state redox potentials, PC*/PC^.? (up to 1.65 V) and PC^.+/PC* (up to ?1.77 V vs. SCE), are such that these novel PCs can engage in both oxidative and reductive quenching mechanisms with strong thermodynamic requirements. The potential of these bimodal PCs was benchmarked in synthetically relevant photocatalytic processes with extreme thermodynamic requirements. Their ability to efficiently catalyze mechanistically opposite oxidative/reductive photoreactions is a unique feature of these organic photocatalysts, thus representing a decisive advance towards generality, sustainability, and cost efficiency in photocatalysis.     

Octahedral Titanium(IV)-Reagents in Organic Synthesis

Abstract

As part of our studies directed toward the use of organotitanium chemistry in organic synthesis^1,2 we wish to report that stable hexa-coordinate octahedral complexes³ of methyltitaniumtrichloride (1) are diastereoand enantioselective methylating reagents. The reaction of tetramethylethylene diamine³ (TMEDA), glyme³ tetrahydrofuran³ or (?)-sparteine with the equivalent amount of 1 in CH₂Cl₂ yields compounds 2, 3, 4 and 5 respectively. These were allowed to react in situ with 2-phenylpropionaldehyde at ?50 °C in CH₂Cl₂ for two hours.     

新型含二茂铁有机配合物的合成及其电化学性质

以二茂铁为起始原料,经氯汞化反应、溴代反应、Suzuki偶联反应、水解反应和取代反应等5步反应合成了一种新型的含二茂铁结构单元的有机配合物(7),其结构经1H NMR、13C NMR、IR和HR-MS(ESI-TOF)表征。电化学研究结果表明:化合物6的E1/2小于化合物7,具有较高的氧化还原活性。     

Synthesis and Initial Thermal Characterization of Titanium Polyferrocene Ethers

Titanium polyferrocene ethers were synthesized by the inter-facial technique. Reaction is rapid and general. Synthesis can be effected by utilizing either NaOH or Et₃N but not without added base. Reactant molar ratio yield trends vary with the nature of the diol, indicative of the sensitivity of the system, at least to this variable. Decomposition to ca. 150°C occurs via a nonoxidative mode(s). Above 150°C, degradation occurs through an oxidative route(s) in air.     

介孔二氧化钛的非有机模板剂法合成

 采用硫酸钛水解法在不使用有机模板剂的条件下合成了高热稳定的锐钛矿型介孔TiO2. 以工业硫酸钛溶液为原料,经两步水解得到介孔结构的偏钛酸, 500 ℃下焙烧后得到比表面积为202.2 m2/g、 平均孔径为2.8 nm并具有超强酸特性的介孔TiO2. 使用X射线衍射、 N2吸附、扫描电镜、 X射线能谱和红外光谱对该样品进行了表征,初步讨论了介孔的形成机理. 吸附在偏钛酸孔壁上的硫酸分子和孔壁上的自由羟基键合,起到了孔结构的导向作用及支撑作用.     

Synthesis,Characterization and Antibacterial Activity of a Novel Photoluminescent Nb-Substituted Lindqvist Polyoxotungstate Based Organic Cation

A novel heteropolyoxometalate, Nb-substituted hexatungstate compound; (C₉H₈N)₃[NbW₅O₁₉]·3H₂O triquinolinium μ₆-oxido-dodeca-μ₂-oxidohexaoxido[niobium(V)pentatungsten(VI)]ate trihydrate (QNbW5) has been grown by slow evaporation method and characterized by powder X-ray and single-crystal XRD methods, NMR, IR, UV–Vis and photoluminescence spectroscopy measurements, elemental analysis and thermogravimetric analysis. Single-crystal XRD analyses show that QNbW5 crystallizes in the triclinic space group \({\text{P}}\overline{ 1}\) and its crystal structure consists of 3D grid-like network of components in a close connection through N–H···O, C–H···O and offset π···π stacking interactions between neighboring rings of quinolinium moieties. Moreover, the spectroscopic and electronic properties of QNbW5 have also been investigated showing a considerable important gap energy well confirming the semiconductor behavior and the blue photoluminescent property of reported material. In addition, the complex shows promising antimicrobial activity against four pathogenic microbes in comparison with its components alone.