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Coordination Polymer of Cobalt (ΙΙ) Nitrate with Imidazole: Synthesis, Properties and Crystal Structure 硝酸钴与咪唑配位聚合物的合成、性能及晶体结构
Pub Date : 2021-01-28 DOI: 10.4236/jcpt.2021.101001
Elmira Alamanova, Nasira Shyytyeva, Zhyldyz Berdalievа, Nurzat Abdyldaeva, Astra Duishonbaeva, Z. Abdullaeva
Layered metal-organic polymer [Co(L)6](NO3)2 was obtained (where, L = C3H4N2) and structurally characterized by X-Ray diffraction (XRD) analysis. Crystals have trigonal structure: a = b = 12.3555(10) Ǻ, c = 14.4833(3) Ǻ; α = β = 90˚; γ = 120˚; V = 1914.78(5) Ǻ; R3, Z = 3. The structure of the complex consists of discrete [Co(L)6]2+ cations and anions. The Co2+ ion has a centrosymmetric octahedron configuration with a coordination site—CoN6. The ligand is coordinated monodentate through the pyridine nitrogen atom (N3) to the Co2+ ion with an average Co-N bond distance of 2.1590 Ǻ. Molecules in the coordination polymer are additionally linked by intermolecular hydrogen bonds through the pyrrole nitrogen atom (-N-H) and oxygen of the nitrate group with the formation of a polymer chain of the type: N-H…O. The chains are linked in layers along the (001) plane.
得到了层状金属有机聚合物[Co(L)6](NO3)2(其中L = C3H4N2),并用x射线衍射(XRD)对其进行了结构表征。晶体具有三角形结构:a = b = 12.3555(10) Ǻ, c = 14.4833(3) Ǻ;α = β = 90˚;γ = 120˚;V = 1914.78(5) Ǻ;R3, z = 3。配合物的结构由离散的[Co(L)6]2+阳离子和阴离子组成。Co2+离子具有中心对称的八面体构型,配位位为con6。配体通过吡啶氮原子(N3)与Co2+离子呈单齿配位,Co-N平均键距为2.1590 Ǻ。配位聚合物中的分子通过吡咯氮原子(-N-H)和硝酸基的氧通过分子间氢键连接,形成了N-H…O型聚合物链。链沿(001)平面分层连接。
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引用次数: 1
Synthesis, Characterization and Crystal Structures of Zwitterionic Triazolato Complexes by Reaction of a Ruthenium Azido Complex with Excess Ethyl Propiolate 钌叠氮配合物与过量丙酸乙酯反应的两性离子三唑啉配合物的合成、表征和晶体结构
Pub Date : 2021-01-01 DOI: 10.4236/jcpt.2021.102002
Chao-Wan Chang, Chi-Rung Lee, Gene-Hsiang Lee
The synthesis and structures of two novel zwitterionic ruthenium triazolato complexes are reported. The treatment of the ruthenium azido complex [Ru]-N 3 (1, [Ru] = (η 5 -C 5 H 5 )(dppe)Ru, dppe = Ph 2 PCH 2 CH 2 PPh 2 ) with an excess of ethyl propiolate in CHCl 3 or CH 2 Cl 2 under ambient conditions for 15 days results in the formation of a mixture of the Z- and E-forms of N(1)-bound ruthenium 3-ethylacryl-4-carboxylate-3H-1,2,3-triazolato complexes [Ru]N 3 (CH=CHCO 2 Et)C 2 H(CO 2 ) (Z-3) and (E-3) in a ratio of ca. 5:2. The structures of E-3 and Z-3 were confirmed by single-crystal X-ray diffraction analysis and fully characterized by 1 H, 31 P, 13 C NMR and IR spectroscopy, mass spectrometry, and elemental analysis. The negatively charged carboxylate moieties of the zwitterionic ruthenium triazolato complexes Z-3 and Z-3 are highly nucleophilic and reactive toward a variety of electrophiles, making Z-3 and Z-3 potential starting materials for the development of biologically active 1,2,3-triazole derivatives.
报道了两种新型两性离子三唑钌配合物的合成及其结构。钌叠氮基的处理复杂[俄文]- N 3(1[俄文]=(η5 - C 5 H 5) (dppe)俄文,dppe Ph值= 2 PCH 2 CH 2、2)与过多的乙基propiolate CHCl 3或CH 2 Cl 2 15天导致环境条件下形成的混合物的Z - N的电子表单(1)绑定钌3-ethylacryl-4-carboxylate-3H-1, 2, 3-triazolato复合物[俄文]N 3 (CH = CHCO - 2等)C 2 H (CO 2) (Z-3)和(e - 3)在ca。5:2的比率。通过单晶x射线衍射分析证实了E-3和Z-3的结构,并通过1h、31p、13c核磁共振、红外光谱、质谱和元素分析对其结构进行了全面表征。阴离子型三唑钌配合物Z-3和Z-3的带负电羧酸部分具有高度亲核性和对多种亲电试剂的反应性,使Z-3和Z-3成为开发具有生物活性的1,2,3-三唑衍生物的潜在起始材料。
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引用次数: 0
Real-Time Characterization of Crystal Shape and Size Distribution Based on Moving Window and 3D Imaging in a Stirred Tank 基于移动窗口和三维成像的搅拌槽晶体形状和尺寸分布实时表征
Pub Date : 2019-12-10 DOI: 10.4236/jcpt.2019.92002
Rui Zhang, Xue-zhong Wang, Yang Zhang, Tao Liu
Crystal shape distribution, i.e. the multidimensional size distribution of crystals, is of great importance to their down-stream processing such as in filtration as well as to the end-use properties including the dissolution rate and bioavailability for crystalline pharmaceuticals. Engineering crystal shape and shape distribution requires knowledge about the growth behavior of different crystal facets under varied operational conditions e.g. supersaturations. Measurement of the facet growth rates and growth kinetics of static crystals in a crystallizer without stirring has been reported previously. Here attention is given to study on real-time characterization of the 3D facet growth behavior of crystals in a stirred tank where crystals are constantly moving and rotating. The measurement technique is stereo imaging and the crystal shape reconstruction is based on a stereo imaging camera model. By reference to a case study on potash alum crystallization, it is demonstrated that the crystal size and shape distributions (CSSD) of moving and rotating potash alum crystals in the solution can be reconstructed. The moving window approach was used to correlate 3D face growth kinetics with supersaturation (in the range 0.04 - 0.12) given by an ATR FTIR probe. It revealed that {100} is the fastest growing face, leading to a rapid reduction of its area, while the {111} face has the slowest growth rate, reflected in its area continuously getting larger.
晶体形状分布,即晶体的多维尺寸分布,对其下游加工(如过滤)以及晶体药物的最终用途特性(如溶出率和生物利用度)非常重要。工程晶体形状和形状分布需要了解不同的晶体面在不同的操作条件下的生长行为,例如过饱和。在没有搅拌的结晶器中测量静态晶体的小面生长速率和生长动力学已经有报道。本文重点研究了晶体在不断运动和旋转的搅拌槽中三维面生长行为的实时表征。测量技术为立体成像,晶体形状重建基于立体成像相机模型。通过对钾明矾结晶的实例研究,证明了可以重构溶液中移动和旋转钾明矾晶体的晶粒尺寸和形状分布(CSSD)。移动窗口方法用于将三维表面生长动力学与ATR FTIR探针给出的过饱和(范围为0.04 - 0.12)相关联。结果表明,{100}是生长最快的面,其面积迅速缩小,{111}面生长速度最慢,其面积不断变大。
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引用次数: 1
Application of Single Scan Differential Scanning Calorimetry Technique for Determination of Kinetic Parameters of Crystallisation in Se-Sb-Ag 应用单扫描差示扫描量热法测定硒锑银结晶动力学参数
Pub Date : 2019-01-30 DOI: 10.4236/JCPT.2019.91001
N. Yaduvanshi, D. Kumar, N. Rastogi, Ashok Kumar
A single scan has been performed in Differential Scanning Calorimetry (DSC) at a heating rate of 15oC/min under non-isothermal conditions to investigate the crystallization kinetics of glassy Se90Sb10-xAgx alloys (where x = 2, 4, 6, 8). For this purpose, Handerson’s theory based on non-isothermal method for thermal analysis of single-scan DSC data has been used. The activation energy of crystallization and order parameter has been determined and composition dependence of these parameters has been discussed.
采用差示扫描量热法(DSC),在非等温条件下,以15oC/min的加热速率进行单次扫描,以研究玻璃态Se90Sb10-xAgx合金(其中x = 2,4,6,8)的结晶动力学。为此,使用了Handerson基于非等温方法的单次扫描DSC数据热分析理论。测定了结晶活化能和有序参数,并讨论了这些参数对组分的依赖关系。
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引用次数: 0
Improved Efficiency of ZnO and Ge Purification 提高氧化锌和锗的净化效率
Pub Date : 2019-01-01 DOI: 10.4236/jcpt.2019.93003
G. S. Pekar, A. F. Singaеvsky, M. M. Lokshin, I. Vasin, O. Dubikovskyi
Unconventional ways to improve the efficiency of purification of two different semiconductor materials of current interest, ZnO and Ge, are described. It is shown that, by using chemically assisted vapour transport of ZnO with carbon as a transporting agent, the degree of chemical purity of ZnO can be increased by more than an order of magnitude. It is also found that heating of the molten Ge in the experimentally determined narrow (about 20˚C wide) temperature range in which an intense evaporation of certain substances is observed, leads to a significant reduction of germanium contamination. As a result, a subsequent deep purification of pre-heat treated germanium by zone refining can be achieved at twice reduced (as compared with “non-treated” Ge) number of passes of a boat with germanium through the melting zones. Thus, the Ge purification process becomes faster, cheaper and more efficient.
本文描述了两种不同半导体材料(ZnO和Ge)净化效率的非常规方法。结果表明,以碳为运输剂进行ZnO的化学辅助气相输运,可以使ZnO的化学纯度提高一个数量级以上。还发现,在实验确定的较窄(约20℃宽)温度范围内加热Ge熔液,观察到某些物质的强烈蒸发,导致锗污染显著减少。因此,随后通过区域精炼对经过热处理的锗进行深度净化,可以实现(与“未经处理”的锗相比)一艘装有锗的船通过熔区的次数减少两倍。因此,锗净化过程变得更快、更便宜、更高效。
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引用次数: 0
Fluorine-Doped Tin Oxide Thin Films Deposition by Sol-Gel Technique 溶胶-凝胶法沉积含氟氧化锡薄膜
Pub Date : 2018-10-31 DOI: 10.4236/jcpt.2018.84006
A. Adjimi, M. L. Zeggar, N. Attaf, M. Aida
In the present work, undoped (SnO2) and fluorine-doped tin oxide (FTO) thin films were prepared by sol-gel process using a solution composed of (SnCl2, H2O), (NH4F), and ethanol mixture. The fluorine concentration effect on structural, optical and electrical properties of SnO2 films is investigated. The electrical properties of FTO films prepared by sol gel remain relatively lower than the ones deposited by other techniques. In present paper, we try to elucidate this difference. Films composition and the FTIR analysis, of films and formed precipitate during film growth, indicate that few amounts of fluorine are incorporated in SnO2 network, most of fluorine atoms remain in the solution. The films resistivity is reduced from 1.1 Ω·cm for undoped films to 3 × 10-2 Ω·cm for 50 wt.% doped FTO, but remains higher than the reported ones in the literature. This high resistivity is explained in terms of fluorine bonding affinity in the solution.
本文以(SnCl2, H2O), (NH4F)和乙醇混合物为溶剂,采用溶胶-凝胶法制备了未掺杂(SnO2)和掺氟氧化锡(FTO)薄膜。研究了氟浓度对SnO2薄膜结构、光学和电学性能的影响。溶胶-凝胶法制备的FTO薄膜的电学性能相对较低。在本文中,我们试图阐明这一区别。薄膜的组成和生长过程中形成的析出物的FTIR分析表明,SnO2网络中含有少量的氟,大部分氟原子留在溶液中。未掺杂FTO时,薄膜的电阻率为1.1 Ω·cm,掺杂50% FTO时,薄膜的电阻率为3 × 10-2 Ω·cm,但仍高于文献报道。这种高电阻率是根据氟在溶液中的键合亲和力来解释的。
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引用次数: 26
Crystallization of Curcumin and Cinnamic Acid from Aqueous Solutions of Hydrotropes 姜黄素和肉桂酸在水溶液中的结晶
Pub Date : 2018-07-31 DOI: 10.4236/jcpt.2018.83005
N. Rathi, V. Gaikar
Batch crystallization studies of curcumin from hydrotropic solutions of sodium cumenesulphonate (NaCS) and of cinnamic acid from a photosensitive hydrotropic medium of sodium cinnamate (Na-CIN) were carried out, in an agitated reactor for the effect of alternate heating and cooling cycles on crystal morphology. The crystal characterization by Scanning electron microscopy (SEM) and crystal size distribution (CSD) showed formation of spheroidal curcumin crystals while cinnamic acid formed porous aggregates when subjected to thermal cycles. The UV irradiation of cinnamic acid however showed no formation of the aggregates. The type of hydrotrope used and the initial crystal morphologies of curcumin and cinnamic acid are shown to be important factors to result in a different behaviour of the crystal morphology upon thermal cycles. The CSD data were effectively used for estimation of nucleation and growth rate parameters.
在搅拌釜中,研究了从亲水的肉桂酸钠(Na-CIN)和肉桂酸(Na-CIN)溶液中提取姜黄素的结晶过程,考察了加热和冷却交替循环对结晶形貌的影响。通过扫描电子显微镜(SEM)和晶体尺寸分布(CSD)表征表明,在热循环作用下,姜黄素形成球状晶体,而肉桂酸形成多孔聚集体。肉桂酸在紫外线照射下未形成聚集体。研究表明,姜黄素和肉桂酸的水同物类型和初始晶体形态是导致晶体形态在热循环中不同行为的重要因素。CSD数据被有效地用于估计成核和生长速率参数。
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引用次数: 3
Effect of Constant Magnetic Field on Convective Heat Transfer through Anisotropic River Beds 恒定磁场对各向异性河床对流换热的影响
Pub Date : 2018-03-21 DOI: 10.4236/JCPT.2018.82004
J. Yovogan, G. Degan, L. Fagbemi
An analytical investigation is conducted to study the effect of magnetic field on convection heat transfer through packed porous beds which consists of a horizontal fluid layer (river bed) and a porous zone with anisotropic permeability and underlined by a surface heated by a constant temperature T1. The free surface of the fluid layer overlying the horizontal porous layer receives solar rays to length of day and is then considered heated isothermally at temperature T2 such as T1 < T2. Flow in porous medium is assumed to be governed by the generalized Brinkman-extended Darcy law and in the fluid layer by the Navier-Stokes model. The Beavers-Joseph condition is applied at the interface between the two layers. The influence of Hartmann number and hydrodynamic anisotropy on the convective phenomenon is investigated analytically. It is found that the magnetic field, the anisotropic permeability and the thickness of the porous lining, e, have a strong influence of the geothermal convective flow and the heat transfer rate.
进行了一项分析研究,以研究磁场对填充多孔床对流换热的影响。填充多孔床由水平流体层(河床)和具有各向异性渗透率的多孔区组成,并以恒定温度T1加热的表面为重点。覆盖在水平多孔层上的流体层的自由表面接收太阳射线至一天的长度,然后被认为在温度T2(例如T1<T2)下被等温加热。假设多孔介质中的流动由广义Brinkman扩展达西定律控制,流体层中的流动则由Navier-Stokes模型控制。Beavers-Josef条件应用于两层之间的界面。分析了哈特曼数和流体力学各向异性对对流现象的影响。研究发现,磁场、各向异性渗透率和多孔衬里厚度e对地热对流和传热速率有很大影响。
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引用次数: 3
Production of High Purity Metals: A Review on Zone Refining Process 高纯金属的生产——区域精炼工艺综述
Pub Date : 2018-01-24 DOI: 10.4236/JCPT.2018.81003
Xiaoxin Zhang, S. Friedrich, B. Friedrich
Purification is a primary application of zone melting, in which the improvement of efficiency, production yield and minimum achievable impurity level are always the research focus due to the increasing demand for high purity metals. This paper has systematically outlined the whole development of related research on zone refining of metals including basic theories, variants of zone refining, parametric optimization, numerical models, and high purity analytical methods. The collection of this information could be of good value to improve the refining efficiency and the production of high purity metals by zone refining.
提纯是区域熔炼的主要应用,由于对高纯度金属的需求不断增加,提高效率、产量和可达到的最低杂质水平一直是研究的重点。本文系统地概述了金属区域精炼的基本理论、区域精炼的变体、参数优化、数值模型和高纯分析方法等相关研究的整个发展过程。这些信息的收集对提高精炼效率和区域精炼生产高纯金属具有一定的参考价值。
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引用次数: 16
Migration of Biodegradable Organic Matter in Underlying Soils of Household Waste Dumpsites: A Case Study in Abomey-Calavi, Benin 可生物降解有机质在生活垃圾填埋场下垫土中的迁移:以贝宁Abomey-Calavi为例
Pub Date : 2018-01-19 DOI: 10.4236/jcpt.2018.81002
M. Djihouessi, S. Onifade, M. Aina, H. Labité, F. P. Codo
This paper presented the first part of the studies about the development of a tool for groundwater contamination prediction, conducted by the Laboratory of Sciences and Technology of Water (UAC/Benin). The investigation made consisted in estimating the combined effect of retardation factor and biodegradation on migration processes of leachate, in the underlying soils of household waste dumpsites, without active safety barrier. Leachate infiltration tests for different initial conditions were made on soil columns and the breakthrough curves were traced for electrical conductivity, the 5 day biochemical oxygen demand (BOD5) and total kjeldahl nitrogen TKN. A mathematical migration model was developed and solved numerically by finite difference method and implemented with Matlab R2013a. Thus, the calibration of the model was made with electric conductivity data by determining the dispersion coefficient of the studied soils (D = 0.96 cm2/min). Simulations for model verification showed that the established model can perfectly predict the migration of biodegradable organic pollution (BOD5) but did not give conclusive results for the monitoring of nitrogenous organic matter (TKN). The influence of the retardation factor on the migration of biodegradable organic pollutants in soils was linear, while the biodegradation rate of the organic material on migration showed an exponential pattern.
本文介绍了水科学与技术实验室(UAC/贝宁)进行的关于开发地下水污染预测工具的第一部分研究。所做的调查包括在没有主动安全屏障的情况下,估计延迟因子和生物降解对生活垃圾倾倒场下层土壤中渗滤液迁移过程的综合影响。在土柱上进行了不同初始条件下的渗滤液渗透试验,并绘制了电导率、5天生化需氧量(BOD5)和总凯氏氮TKN的穿透曲线。建立了偏移数学模型,并用有限差分法对其进行了数值求解,并用Matlab R2013a实现。因此,通过确定所研究土壤的分散系数(D=0.96 cm2/min),利用电导率数据对模型进行了校准。模拟验证表明,所建立的模型可以很好地预测可生物降解有机污染物(BOD5)的迁移,但对含氮有机物(TKN)的监测没有给出结论性的结果。阻滞因子对可生物降解有机污染物在土壤中迁移的影响是线性的,而有机物质的生物降解速率对迁移的影响呈指数型。
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引用次数: 0
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