A Compendium of the Most Promising Synthesized Organic Compounds against Several Fusarium oxysporum Species: Synthesis,Antifungal Activity,and Perspectives

Vascular wilt caused by F. oxysporum (FOX) is one of the main limitations of producing several agricultural products worldwide, causing economic losses between 40% and 100%. Various methods have been developed to control this phytopathogen, such as the cultural, biological, and chemical controls, the latter being the most widely used in the agricultural sector. The treatment of this fungus through systemic fungicides, although practical, brings problems because the agrochemical agents used have shown mutagenic effects on the fungus, increasing the pathogen’s resistance. The design and the synthesis of novel synthetic antifungal agents used against FOX have been broadly studied in recent years. This review article presents a compendium of the synthetic methodologies during the last ten years as promissory, which can be used to afford novel and potential agrochemical agents. The revision is addressed from the structural core of the most active synthetic compounds against FOX. The synthetic methodologies implemented strategies based on cyclo condensation reactions, radical cyclization, electrocyclic closures, and carbon–carbon couplings by metal–organic catalysis. This revision contributes significantly to the organic chemistry, supplying novel alternatives for the use of more effective agrochemical agents against F. oxysporum.     

Facile Green Synthesis of Ni(OH)2@Mn3O4 Cactus-Type Nanocomposite: Characterization and Cytotoxicity Properties

In the present work, the facile eco-friendly synthesis and evaluation of the anti-tumor activity of Ni(OH)₂@Mn₃O₄ nanocomposite were carried out. The synthesis of Ni(OH)₂@Mn₃O₄ nanocomposite from chia-seed extract was mediated by sonication. The obtained materials were characterized by different spectroscopic techniques such as transmission electron microscopy (TEM), scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible (UV-Vis), and Fourier transform infrared (FT-IR) spectroscopies. The results of XRD, SEM, EDS, TEM, FT-IR, and UV-Vis analysis indicate the successful manufacturing of a crystalline, cactus-type Ni(OH)₂@Mn₃O₄ nanocomposite of 10.10 nm average particle size. XPS analysis confirms that the synthesized materials consist mainly of Ni²⁺, Mn²⁺, and Mn³⁺. The antitumor activity of the nanocomposite was tested against a breast cancer (MCF-7) cell line. The results showed Ni(OH)₂@Mn₃O₄ nanocomposite possesses insignificant cytotoxicity. The cell-death percentage was 34% at a 100 ppm concentration of Ni(OH)₂@Mn₃O₄ nanocomposite. The obtained results imply that the synthesized nanocomposite could be suitable and safe for drug delivery and water treatment.     

钕的氢氧化物和氧化物纳米线的制备及表征

以金属钕为起始原料，采用简单的碱性溶液下水热法制备出氢氧化钕纳米线。所得到的水热产物采用X-射线衍射、扫描电镜和透射电镜等进行了结构与形态表征。研究发现，水热处理的温度、碱液浓度和碱的种类等对水热产物的形貌、长径比和结晶状态有较大影响，提高水热温度和增加碱液浓度有利于氢氧化钕纳米线的生长。在相同水热反应温度(180 ℃)、水热时间(45 h)和碱浓度下，5 mol·L^-1 NaOH溶液体系制备的氢氧化钕纳米线具有较高纯度和较长的长径比，其直径为20～40 nm，长度为2～10 μm。该氢氧化钕纳米线在空气气氛下500 ℃烧结后形成具有体心立方结构的C型Nd₂O₃，该Nd₂O₃仍具有一维纳米线形貌。升高焙烧温度时产物的形貌和相结构都发生了明显变化。     

二氧化铈八面体的水热合成与表征

本文选用硝酸铈和草酸利用水热合成方法合成出二氧化铈八面体。水热产物的形貌与物相可以通过改变反应温度和时间进行调控。基于实验结果,提出了形成二氧化铈八面体的自牺牲模板法机理。     

CaTiO3纳米粉体溶胶-凝胶法合成、表征及介电特性

采用无机盐溶胶-凝胶法制备了CaTiO₃纳米粉体，采用TG-DTA、XRD、TEM等技术进行了表征，并探讨了CaTiO₃纳米粉体烧结特性及介电效应。结果表明，干凝胶800 ℃低温煅烧可获得粒径分布较窄、平均粒径为60～70 nm的单相CaTiO₃纳米粉。纳米CaTiO₃粉具有较大的比表面积，使作为粉体烧结驱动力的表面能剧增，促使CaTiO₃在1 200 ℃实现致密烧结，比固相法制备的微米粉烧结降低100～200 ℃，且具有较宽的烧结温区。与微米级粉体烧结体介电特性相比，纳米粉具有更高的Q_f值。纳米CaTiO₃粉制备的陶瓷在1 250 ℃烧结2 h，获得优良的介电性能：ε_r=172，Q_f=4 239 GHz，τ_f=+7.68 × 10^-4 ℃^-1。     

Synthesis and electrochemical properties of chemically substituted LiMn2O4 prepared by a solution-based gel method

Lithium manganese oxide, LiMn(2)O(4), and its substituted samples LiM(0.05)Mn(1.95)O(4) (M=Al, Co, and Zn) were first prepared by a cost-saving and effective new solution-based gel method using a mixture of acetate and ethanol as the chelating agent. The physical properties of the synthesized samples were investigated by thermogravimetry/differential thermal analysis, X-ray diffraction, and scanning electronic microscopy. The as-prepared powders were used as positive materials for a lithium-ion battery, whose charge/discharge properties and cycle performance were examined. The results revealed that all the substituted samples had better cycle performance than pure LiMn(2)O(4). Among these synthesized materials, the LiCo(0.05)Mn(1.95)O(4) sample had the best cycle performance. After 30 cycles, its capacity loss was only 3%. Therefore, cyclic voltammetry and electrochemical impedance spectroscopy were employed to characterize the reactions of Li ion insertion into and extraction from LiCo(0.05)Mn(1.95)O(4) electrodes.     

多层多孔Co3O4纳米粒子组装体的合成、表征和电化学性能研究

利用十二烷基磺酸钠(SDS)作为表面活性剂,合成了形貌化的CoC₂O₄配合物前驱物,然后在500 ℃下热分解形貌化的前驱物,得到了多层多孔Co₃O₄纳米粒子组装体。采用FESEM、TEM、HRTEM、XRD、N₂吸附脱附和Raman散射等手段对产物进行了分析和表征。低角XRD,TEM和N₂吸附脱附测试表明所得组装体具有多孔结构。常规XRD、HRTEM和Raman结果证明组装体中Co₃O₄纳米粒子建筑块结晶较好。与体相Co₃O₄晶体相比,Co₃O₄纳米粒子组装体的5个拉曼活性峰发生了明显的红移。将Co₃O₄纳米粒子组装体作为锂离子电池的正极材料进行了电化学性能测试,结果表明该组装体电极的首次放电容量为1 115 mAh·g^-1,远高于目前文献报道的Co₃O₄纳米管、纳米粒子和纳米棒电极。但是,该组装体电极的循环性能不好,有待进一步提高。     

Fabrication and Characterization of Nanocomposite Flexible Membranes of PVA and Fe3O4

Composite polymer membranes of poly(vinyl alcohol) (PVA) and iron oxide (Fe₃O₄) nanoparticles were produced in this work. X-ray diffraction measurements demonstrated the formation of Fe₃O₄ nanoparticles of cubic structures. The nanoparticles were synthesized by a coprecipitation technique and added to PVA solutions with different concentrations. The solutions were then used to generate flexible membranes by a solution casting method. The size and shape of the nanoparticles were investigated using scanning electron microscopy (SEM). The average size of the nanoparticles was 20±9 nm. Raman spectroscopy and Fourier-transform infrared spectroscopy (FTIR) were utilized to investigate the structure of the membranes, as well as their vibration modes. Thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) demonstrated the thermal stability of the membranes and the crystallinity degree. Electrical characteristics of the thin membranes were examined using impedance spectroscopy as a function of the nanoparticles’ concentrations and temperatures. The resistivity of the fabricated flexible membranes was possible to adjust by controlled doping with suitable concentrations of nanoparticles. The activation energy decreased with the nanoparticles’ concentrations due to the increase in charge carriers’ concentrations. Therefore, the fabricated membranes may be applied for practical applications that involve the recycling of nanoparticles for multiple application cycles.     

纳米γ-Fe2O3粉体的合成与磁性增强研究

采用微乳法合成出氧化铁的前驱体——纳米β-FeOOH, 分别以β-FeOOH与添加剂壬基酚聚氧乙烯醚(NP-4)以物质量的比(n)为4, 5, 100添加NP-4, 混合煅烧. 采用拉曼光谱分析了样品中炭含量及分布, 并且用透射电镜观测产物的形貌和粒径, 采用磁强计观测产物磁性的变化. 结果得出, 对n＝5或破乳所得凝胶煅烧, 所得样品皆为分散均匀的四方形颗粒状, 且为磁性明显增强的纳米氧化铁γ-Fe₂O₃. 还分别讨论了样品中炭含量以及颗粒形状对比饱和磁化强度σ_s、矫顽力、矩形比的影响.     

钛铁矿型CoTiO3纳米材料的制备及性能表征

以Co(NO3)2·6H2O和TiO2(P-25)为原料,在十六烷基三甲基溴化铵(CTAB)/水形成的胶束溶液中,首先制得纳米氧化钴Co3O4-TiO2复合材料,该复合材料经600和700℃煅烧后制备了钛铁矿型CoTiO3纳米材料.以X射线衍射(XRD)、透射电子显微镜(TEM)、紫外-可见(UV-vis)、拉曼(Raman)光谱和X射线光电子能谱(XPS)对其结构特征和光谱性能进行了研究.用TEM形貌观察,粒子基本为球形;纳米CoTiO3的UV-vis吸收峰明显红移;经Raman光谱和XPS分析,进一步表明600和700℃煅烧后形成了Ti-O-Co键.     

纳米SnO2的非水溶剂溶胶-凝胶法制备与表征

Nanometer SnO₂ powders were successfully prepared by non-hydrolytic sol-gel approach combined with heat treatments using tin tetrachloride as starting material and ethylene glycol as solvent. The reaction mechanism of the sol-gel process is proposed. Results indicate that the -OHCH₂CH₂OH- prevent Cl^- ion from accessing to tin Sn⁴⁺ due to steric effect, and hence increaseing the stability of the sol solution. Ethylene glycol functions not only as a complextion agent to form a polymer network but also as a “spacer” to modulate the distance between metal ions, preventing metal oxide particles from aggregation during desiccation of the sol. The effects of heat treatments on the evolution of structure and morphology of nanosized SnO₂ powders were studied. The powders with narrow size distribution around 15～20 nm could be obtained at 500 ℃ for 4 h.     

Synthesis of prospective disaccharide ligands for Escherichia coli O157 verotoxin

The synthesis of new potential ligands for Escherichia coli 0157 verotoxin is reported, based on disaccharide fragments of the tetrasaccharide glycan portion of Gb₄ glycolipid. Intramolecular aglycone delivery was employed for the high-yielding and stereoselective production of the azidopropyl-tethered α-galactoside building block.     

In-Situ Synthesis and Characterization of Nanocomposites in the Si-Ti-N and Si-Ti-C Systems

The pyrolysis (1000 °C) of a liquid poly(vinylmethyl-co-methyl)silazane modified by tetrakis(dimethylamido)titanium in flowing ammonia, nitrogen and argon followed by the annealing (1000–1800 °C) of as-pyrolyzed ceramic powders have been investigated in detail. We first provide a comprehensive mechanistic study of the polymer-to-ceramic conversion based on TG experiments coupled with in-situ mass spectrometry and ex-situ solid-state NMR and FTIR spectroscopies of both the chemically modified polymer and the pyrolysis intermediates. The pyrolysis leads to X-ray amorphous materials with chemical bonding and ceramic yields controlled by the nature of the atmosphere. Then, the structural evolution of the amorphous network of ammonia-, nitrogen- and argon-treated ceramics has been studied above 1000 °C under nitrogen and argon by X-ray diffraction and electron microscopy. HRTEM images coupled with XRD confirm the formation of nanocomposites after annealing at 1400 °C. Their unique nanostructural feature appears to be the result of both the molecular origin of the materials and the nature of the atmosphere used during pyrolysis. Samples are composed of an amorphous Si-based ceramic matrix in which TiN_xC_y nanocrystals (x + y = 1) are homogeneously formed “in situ” in the matrix during the process and evolve toward fully crystallized compounds as TiN/Si₃N₄, TiN_xC_y (x + y = 1)/SiC and TiC/SiC nanocomposites after annealing to 1800 °C as a function of the atmosphere.     

前驱体法制备Mn_2O_3空心橄榄形结构及形貌演化

利用苹果酸还原高锰酸钾以水热合成方法制备了具有橄榄形貌的纳米结构MnCO3前驱体,通过600℃焙烧MnCO3前驱体得到橄榄形Mn2O3.以扫描电镜(SEM)、透射电镜(TEM)、X射线衍射(XRD)、热重-差热分析(TG-DTA)等方法对产物的形貌和结构进行了表征.考察了MnCO3前驱体微观形貌随水热反应时间的演变:当水热反应时间为2h时得到具有橄榄形形貌的MnCO3前驱体,空心结构的壁比较厚;当水热反应时间延长到6h时得到的MnCO3前驱体仍然具有橄榄形形貌,壁变薄;当反应时间延长到24h时得到的MnCO3前驱体仍然具有橄榄形形貌,并且壁非常薄.我们推测在Ostwald熟化机理作用下,空心橄榄形MnCO3前驱体随着反应时间的延长其壁逐渐由160nm演化为30nm.     

MgFe2O4纳米粉体的水热合成及其表征(英)

MgFe₂O₄ nanoparticles were hydrothermally synthesized at 150 ℃ using iron nitrate [Fe(NO₃)₃·9H₂O], magnesium nitrate [Mg(NO₃)₂·6H₂O] and sodium hydroxide (NaOH) as starting materials by carefully controlling the reaction conditions. The influences of several factors such as presence or absence of Na⁺, molar ratio of Fe³⁺ / Mg²⁺, concentration of mental ions, temperature and reaction time on resultant products were investigated in the hydrothermal process. The sample was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM), and its magnetic properties were measured using vibrating sample magnetometer (VSM).     

新型含N-杂环卡宾二硫化碳配体的锰铼金属双核化合物的合成、表征及电化学性质简

合成了一系列含N-杂环卡宾二硫化碳加合物配体的锰铼金属有机化合物,其中包括3种单核化合物和3种双核化合物,对它们的结构进行了表征,并研究其反应性和电化学性质. 与三烷基膦二硫化碳配体相比,含N-杂环卡宾二硫化碳加合物配体的锰铼金属有机化合物展现出不同的反应特性. 研究结果表明,[MnRe(CO)6(μ-H){μ-CH3SC(S)IMes2}]配合物具有催化质子还原成氢气的能力.     

尖晶石型NiCr2O4的燃烧法合成及表征

通过溶胶-凝胶燃烧法制备了具有立方相的尖晶石型NiCr2O4颜料,并采用TG/DSC、XRD、FTIR和SEM等手段对其进行表征和研究。结果表明:将燃烧后的粉末于900℃下煅烧2 h可以得到单一相的NiCr2O4,温度达不到900℃时所得粉末(包括燃烧后粉末和500和700℃煅烧得到的粉末)为NiO和Cr2O3组成的混合物。利用紫外/可见/近红外分光光度计仔细研究了燃烧后粉末和煅烧后粉末的颜色参数。尽管具有相同的成分,500和700℃下煅烧得到的粉末与燃烧后粉末却具有明显不同的颜色,这可从一氧化镍为非整比化合物的角度加以解释。此外,900和1 000℃下煅烧得到的NiCr2O4粉末呈现出随温度变化的绿色。     

Synthesis of Chitosan-La2O3 Nanocomposite and Its Utility as a Powerful Catalyst in the Synthesis of Pyridines and Pyrazoles

Recently, the development of nanocatalysts based on naturally occurring polysaccharides has received a lot of attention. Chitosan (CS), as a biodegradable and biocompatible polysaccharide, is considered to be an excellent template for the design of a hybrid biopolymer-based metal oxide nanocomposite. In this case, lanthanum oxide nanoparticles doped with chitosan at different weight percentages (5, 10, 15, and 20 wt% CS/La₂O₃) were prepared via a simple solution casting method. The prepared CS/La₂O₃ nanocomposite solutions were cast in a Petri dish in order to produce the developed catalyst, which was shaped as a thin film. The structural features of the hybrid nanocomposite film were studied by FTIR, SEM, and XRD analytical tools. FTIR spectra confirmed the presence of the major characteristic peaks of chitosan, which were modified by interaction with La₂O₃ nanoparticles. Additionally, SEM graphs showed dramatic morphological changes on the surface of chitosan, which is attributed to surface adsorption with La₂O₃ molecules. The prepared CS/La₂O₃ nanocomposite film (15% by weight) was investigated as an effective, recyclable, and heterogeneous base catalyst in the synthesis of pyridines and pyrazoles. The nanocomposite used was sufficiently stable and was collected and reused more than three times without loss of catalytic activity.     

梯度材料LiNi0.8Co0.2O2的合成与表征

The gradient composite LiNi_0.8Co_0.2O₂ was synthesized using spherical Ni(OH)₂ particle coated by a sol-gel containing cobalt and lithium. The precursor was examined by DSC-TG. The gradient composite was characterized by SEM, EDS, XPS, XRD and ICP-AES. The XPS, EDS and ICP-AES results show that content of cobalt in the surface is higher than in the center of the spherical particle of the gradient composite. The first discharge specific capacity of the gradient composite sintered at 700 ℃ is 187.3 mAh·g^-1.     

Synthesis and applications of mesoporous Cu-Zn-Al2O3 catalyst for dehydrogenation of 2-butanol

A series of mesoporous Cu-Zn-Al₂O₃ materials have been synthesized at ambient temperature and their structure was characterized by XRD, N₂ physical adsorption and TPR techniques. Their catalytic applications for the dehydrogenation of 2-butanol to methyl ethyl ketone (MEK) were evaluated in a fixed-bed flow reactor at atmospheric pressure. It is demonstrated from the XRD patterns that both the as-synthesized samples and calcined samples have the typical XRD patterns of meso-structured materials and the results of N₂O chemical adsorption showed that Cu was embedded in the framework of the mesoporous materials and homogeneously dispersed in the mesoporous Cu-Zn-Al₂O₃ materials. The catalytic activity of 2-butanol dehydrogenation was varied in the order of CZA(10)<CZA(CP)<CZA(20)<CZA(30); while the selectivity of MEK was increased in the order of CZA(CP)<CZA(10)<CZA(20)<CZA(30).