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Microwave-Assisted Erlenmeyer Synthesis of Azlactones Catalyzed by MgO/Al2O3 Under Solvent-Free Conditions 无溶剂条件下MgO/Al2O3微波辅助Erlenmeyer合成氮唑内酯
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.989575
N. Rostamizadeh, A. Khajeh-Amiri, H. Moghanian
MgO/Al2O3 catalyzes the synthesis of azlactone derivatives from condensation reaction of aldehydes (or ketones) with hippuric acid and acetic anhydride as a dehydrating agent under microwave irradiation. The low toxicity, low cost, ease of handling, and high activity of MgO/Al2O3 make this procedure particularly attractive. Also, this catalyst can be easily recovered by decant and can be reused for this condensation five times in succession without considerable loss of its catalytic activity.
MgO/Al2O3在微波辐射下,以马尿酸和乙酸酐为脱水剂,催化醛(或酮)缩合反应合成氮杂内酯衍生物。MgO/Al2O3的低毒性、低成本、易于处理和高活性使该工艺特别具有吸引力。此外,该催化剂可以很容易地通过滗析回收,并且可以连续重复使用该缩合五次而不会造成相当大的催化活性损失。
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引用次数: 6
Detection of Volatile Organic Compounds Using Langmuir-Blodgett Films of Zinc-Porphyrin and Zinc-Phthalocyanine 锌-卟啉和锌-酞菁Langmuir-Blodgett膜检测挥发性有机化合物
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.989576
Wenyao Yang, Jianhua Xu, Y. Mao, Yajie Yang, Yadong Jiang
Detection of volatile organic compounds (VOCs) by electronic optical nose based on sensing thin films is becoming more interesting in modern industry and daily life. The thin films of zinc-porphyrin and zinc-phthalocyanine fabricated by Langmuir-Blodgett (LB) technique onto quartz substrates have been used as sensing elements for electronic optical nose application. Absorption spectra range of the both organic elements in a chloroform solution and the LB solid state thin films were acquired by using a UV-1700 spectrometer. As an electronic gas sensing test, the optical absorbance performance after the exposure of LB films to different VOCs, and dry air was investigated. The results indicated that the ZnTPP and ZnPc LB films showed different gas sensitivity due to different molecule structure. Besides, a 2 × 1 colorimetric array is fabricated by immobilizing sensing thin film on a silica substrate, and the vapor molecules of pyridine and methanol can be easily detected.
基于传感薄膜的电子鼻检测挥发性有机化合物(VOCs)在现代工业和日常生活中越来越受到关注。利用Langmuir-Blodgett (LB)技术在石英衬底上制备了锌-卟啉和锌-酞菁薄膜,并将其用作电子光学鼻的传感元件。用紫外-1700谱仪测定了有机元素在氯仿溶液和LB固态薄膜中的吸收光谱范围。作为一种电子气敏测试,研究了LB膜暴露于不同VOCs和干燥空气后的光学吸收性能。结果表明,由于分子结构的不同,ZnTPP和ZnPc LB膜表现出不同的气敏性。此外,将传感薄膜固定在二氧化硅衬底上制备了2 × 1比色阵列,可以方便地检测吡啶和甲醇的蒸汽分子。
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引用次数: 17
Synthesis and Structural Properties of Nanoselenium-Supported MCM-41 Material 纳米硒负载MCM-41材料的合成及结构性能研究
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.989579
A. M. Yusof, S. Yusan
The authors describe herein a new process for the synthesis of nanoselenium–supported MCM-41 hybrid material. Selenium nanoparticles were synthesized via chemical reduction method that this method is capable of producing spherical selenium nanoparticles of size 20 to 80 nm, under ambient conditions, and covalently bonded to MCM-41 framework by 3-(triethoxysilyl)-propylamine (APTES). The structures, morphology and size of the products were investigated by several characterization techniques such as XRD, SEM, TEM, FT-IR, UV–vis/DRS, Raman spectroscopy, and N2 adsorption–desorption isotherms method. These results demonstrated that Se-MCM-41 is a promising candidate for biosensor, adsorbent, or catalyst.
本文介绍了一种合成纳米硒负载MCM-41杂化材料的新工艺。采用化学还原法制备了硒纳米粒子,该方法在常温条件下可制得尺寸为20 ~ 80 nm的球形硒纳米粒子,并通过3-(三乙氧基硅基)-丙胺(APTES)与MCM-41骨架共价键合。采用XRD、SEM、TEM、FT-IR、UV-vis /DRS、拉曼光谱、N2吸附-脱附等温线等表征技术对产物的结构、形貌和粒径进行了表征。这些结果表明Se-MCM-41是一种很有前途的生物传感器、吸附剂或催化剂的候选者。
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引用次数: 2
Ultrasonically Assisted Decarboxylative Bromination of α,β-Unsaturated Carboxylic Acids Under Vilsmeier-Haack Conditions 维斯迈耶-哈克条件下α,β-不饱和羧酸的超声辅助脱羧溴化
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.989573
M. Kumar, K. Rajanna, P. Venkanna, M. Venkateswarlu, V. Sudhakar Chary
An efficient method for decarboxylative bromination of cinnamic acids (α,β-unsaturated carboxylic acids or 3-arylpropenoic acids) was achieved under relatively mild conditions using Vilsmeier-Haack reagent and KBr in acetonitrile media. Vilsmeier-Haack reagent is prepared by using 1:1 ratio of oxychloride (SOCl2 or POCl3) and DMF under chilled condition. Ultrasonically assisted reactions underwent smoothly with highly significant rate enhancements and afforded bromostyrenes as products in very good yields even though the reactions were too sluggish.
在相对温和的条件下,以KBr和Vilsmeier-Haack试剂在乙腈介质中实现了肉桂酸(α、β-不饱和羧酸和3-芳基丙烯酸)的脱羧溴化反应。用氯化氧(SOCl2或POCl3)与DMF以1:1的比例在冷冻条件下制备维斯迈耶-哈克试剂。超声辅助反应顺利进行,反应速率显著提高,即使反应太慢,也能以很好的收率生成溴苯乙烯。
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引用次数: 5
Facile Preparation of Fe3O4/Carbon Nanocomposite With High Lithium Storage Capacity 高储锂容量Fe3O4/碳纳米复合材料的制备
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.988824
Shi-Zhao Kang, Lin Bo, Xiangqing Li, A. Mu
In the present work, Fe3O4/carbon nanocomposite was prepared using metal organic framework as a precursor. Meanwhile, the electrochemical performance of the Fe3O4/carbon nanocomposite, as an anode material, was evaluated by galvanostatic discharge-charge tests. The experimental results indicate that the as-prepared sample is a porous aggregation of Fe3O4 nanoparticles interconnected with amorphorous carbon layer, and the mean diameter of Fe3O4 nanoparticles is approximately 30 nm. Moreover, it is also observed that the Fe3O4/carbon nanocomposite possesses a high initial discharge capacity of 1586 mA h g−1.
本文以金属有机骨架为前驱体制备了Fe3O4/碳纳米复合材料。同时,通过恒流充放电试验对Fe3O4/碳纳米复合材料作为负极材料的电化学性能进行了评价。实验结果表明,制备的样品为Fe3O4纳米颗粒与非晶碳层相互连接的多孔聚集体,Fe3O4纳米颗粒的平均直径约为30 nm。此外,还观察到Fe3O4/碳纳米复合材料具有1586 mA h g−1的高初始放电容量。
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引用次数: 3
Investigating the Effect of Ultrasonic and Microwave-Assisted Aging on the Synthesis of Nanosized SAPO-34 Molecular Sieves Using Box–Behnken Experimental Design 采用Box-Behnken实验设计研究超声和微波辅助老化对合成纳米SAPO-34分子筛的影响
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.988827
H. S. Pajaie, M. Taghizadeh
Nanosized SAPO-34 was synthesized by means of ultrasonic and microwave-assisted aging process. Synthesized samples were characterized by BET, XRD, and FE-SEM techniques. Applying the response surface methodology (RSM) based on Box–Behnken statistical design, the effects of microwave (MW), ultrasonic (US) aging time, and hydrothermal time on the preparation of SAPO-34 with respect to crystallinity of final product phase were investigated. The results showed that the interaction between US and MW aging time had the main positive effect on the crystallinity and the crystallization was accomplished in a significantly reduced time.
采用超声和微波辅助时效法制备了纳米SAPO-34。采用BET、XRD、FE-SEM等技术对合成样品进行了表征。采用基于Box-Behnken统计设计的响应面法(RSM),研究了微波(MW)、超声波(US)时效时间和水热时间对SAPO-34制备过程中最终产物相结晶度的影响。结果表明,US和MW时效时间的相互作用对结晶度有主要的积极影响,在显著缩短的时间内完成结晶。
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引用次数: 3
Preparation of N-Doped Mesoporous TiO2 Using Nitromethane as Nitrogen Source and Their High Photocatalytic Performance 硝基甲烷为氮源制备n掺杂介孔TiO2及其高光催化性能
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.989590
Q. Fang, Jianting Tang, Hua Zou, Tiejun Cai, Q. Deng
N-doped mesoporous TiO2 was successfully prepared by using CH3NO2 as the nitrogen source and P123 as template. The materials were characterized by TEM, N2 sorption, XRD, XPS, UV-vis DRS, and TG-DTA techniques. The photocatalytic activity of N-doped TiO2 was tested in elimination of gaseous methanol, formaldehyde, and BTX (benzene, toluene and xylene). The obtained N-doped mesoporous TiO2 materials have better photocatalytic activity than commercial photocatalyst (Degussa P25). Moreover, the N-doped mesoporous TiO2 photocatalysts are easy to prepare and have stable performance, high photocatalytic activity and long lifetime.
以CH3NO2为氮源,P123为模板,成功制备了n掺杂介孔TiO2。采用TEM、N2吸附、XRD、XPS、UV-vis DRS、TG-DTA等技术对材料进行了表征。测试了n掺杂TiO2光催化去除气态甲醇、甲醛和BTX(苯、甲苯和二甲苯)的活性。所制得的n掺杂介孔TiO2材料比市售光催化剂(Degussa P25)具有更好的光催化活性。此外,n掺杂介孔TiO2光催化剂制备简单,性能稳定,光催化活性高,寿命长。
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引用次数: 8
Hydrothermal Synthesis and Structural Characterization of a Three-Dimensional Coordination Polymer on Ag(I) Ag(I)三维配位聚合物的水热合成及结构表征
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.989582
Qi Chen, Huijie Lun, Yong-Hong Li, Shu Li, Bei-Bei Li, Xudong Zhang, Yamin Li
A new coordination polymer [Ag3(1,2,4-btc)]n (1) (1,2,4-H3btc = 1,2,4-benzenetricarboxylate) has been synthesized by hydrothermal method and characterized by X-ray single crystal diffraction, elemental analysis, IR spectrum, and TGA. Compound 1 exhibits a 3D network consisting of the 2D layer connected by the ligand 1,2,4-btc3−, which adopts a new coordination mode. Moreover, blue fluorescence at 480 nm emission was observed under 320 nm excitation.
采用水热法合成了一种新型配位聚合物[Ag3(1,2,4-btc)]n (1) (1,2,4- h3btc = 1,2,4-苯三羧酸盐),并用x射线单晶衍射、元素分析、红外光谱和热重分析对其进行了表征。化合物1呈现由配体1,2,4-btc3−连接的二维层组成的三维网络,采用新的配位模式。在320 nm的激发下,观察到480 nm的蓝色荧光。
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引用次数: 4
Synthesis and Crystal Structures of Co(II) Complexes Derived From Two Unsymmetrical Bis-Heterocyclic Ligands With Benzimidazole Moiety 含苯并咪唑基团的非对称双杂环配体Co(II)配合物的合成及晶体结构
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.989588
Jin Huang, Qin Wei, W. Zhang, Zhong Zhang, Yong-Zhi Liao
Treatment of two kinds of unsymmetrical bis-heterocyclic ligands bearing benzimidazole moiety, 2-[2-(1,2,4-triazole-1-yl)ethyl]-1H-benzimidazole (L1) and 2-[2-(1,2,3-benzotriazole-1-yl)ethyl]-1H-benzimidazole (L2), with Co(II) chloride, resulted in two new complexes, [Co3(L2)4Cl6]·2H2O (1) and [Co(L1)Cl2]2 (2), with different aggregating patterns. Two complexes were characterized by single-crystal X-ray determinations. In the solid state, L1 assumes an anti conformation in compound 1, whereas L2 exists as a gauche conformer in compound 2. Complex 1 reveals a 1-D double-stranded chain structure consisting of both octahedrally and tetrahedrally coordinated Co(II) ions. Complex 2 is a mononuclear tetrahedral Co(II) species, which was hydrogen bonded with each other to give a 1-D linear chain.
含苯并咪唑基团的2-[2-(1,2,4-三唑-1-基)乙基]- 1h -苯并咪唑(L1)和2-[2-(1,2,3-苯并三唑-1-基)乙基]- 1h -苯并咪唑(L2)两种不对称双杂环配体用Co(II)氯处理后,得到了两种具有不同聚集模式的新配合物[Co3(L2)4Cl6]·2H2O(1)和[Co(L1)Cl2]2(2)。两个配合物通过单晶x射线测定进行了表征。在固体状态下,L1在化合物1中呈反构象,而L2在化合物2中呈间扭构象存在。配合物1是由八面体和四面体配位的Co(II)离子组成的一维双链结构。配合物2是一种单核四面体Co(II),相互氢键形成一维线性链。
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引用次数: 0
Hydrothermal Synthesis and Characterization of CaCo3 Nanostructure 纳米碳酸钙的水热合成及表征
Pub Date : 2016-05-03 DOI: 10.1080/15533174.2014.988817
M. Karimi, M. Ranjbar
In this experimental work, the authors synthesized calcium carbonate nanostructures with different morphologies via simple hydrothermal method. Different parameters such as hydrothermal time and surfactant effects were investigated on product size and morphology. SEM images were served for determination of products morphology. XRD pattern was also used for investigation of crystallity and crystal size of as-synthesized product.
在本实验中,作者通过简单的水热法合成了不同形貌的碳酸钙纳米结构。考察了水热时间和表面活性剂对产物尺寸和形貌的影响。用扫描电镜(SEM)图像测定产物形貌。利用XRD谱图对合成产物的结晶度和晶粒尺寸进行了研究。
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引用次数: 14
期刊
Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry
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