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The synthesis, structure and physical properties of lanthanide(III) complexes with nicotinic acid 镧系(III)与烟酸配合物的合成、结构和物理性质
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0366-5
Nuša Hojnik, M. Kristl, A. Golobič, Z. Jagličić, M. Drofenik
AbstractThis article reports the synthesis of novel, rare-earth coordination complexes with nicotinic acid. Three compounds with the general formula Ln2[(C5H4NCOO)6(H2O)4] (Ln = Yb, 1; Ln = Gd, 2; Ln = Nd, 3) were prepared from relatively cheap and readily available reactants. Their compositions and structure were characterized by IR spectroscopy and single-crystal X-ray diffraction. The magnetic and thermogravimetric properties were also studied. The complexes consist of centrosymetric, dimeric molecules having all six nicotinato ligands coordinated with the central atom in the bidentate mode. The coordination environment of the Ln3+ for all three compounds is 8. Here we describe the crystal structure of Yb and Gd complexes with nicotinic acid.
摘要本文报道了新型稀土烟酸配位配合物的合成。三种通式为Ln2[(C5H4NCOO)6(H2O)4]的化合物(Ln = Yb, 1;Ln = Gd, 2;Ln = Nd, 3)是由相对便宜和容易获得的反应物制备的。用红外光谱和单晶x射线衍射对其组成和结构进行了表征。并对其磁性和热重性能进行了研究。该配合物由中心对称的二聚体分子组成,其所有六个烟碱配体与中心原子以双齿模式配位。三种化合物的Ln3+配位环境均为8。本文描述了Yb和Gd与烟酸配合物的晶体结构。
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引用次数: 10
Copper-cobalt ferrites as catalysts for methanol decomposition 铜钴铁氧体作为甲醇分解催化剂
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0371-8
N. Velinov, K. Koleva, T. Tsoncheva, D. Paneva, E. Manova, K. Tenchev, B. Kunev, I. Genova, I. Mitov
AbstractCopper-cobalt ferrites with composition Cu1−xCoxFe2O4, where x= 0.2 and 0.8 were prepared by thermal treatment of co-precipitated precursor. The obtained materials were characterized by TG-DSC, XRD, Transmission and Conversion Electron Mössbauer spectroscopy and temperature programmed reduction with hydrogen. The catalytic properties of ferrites were tested in methanol decomposition to CO and hydrogen.
摘要通过对共沉淀前驱体进行热处理,制备了成分为Cu1−xCoxFe2O4, x= 0.2和0.8的铜钴铁氧体。通过TG-DSC、XRD、透射和转换电子Mössbauer能谱和程序升温还原氢对所得材料进行了表征。对铁氧体在甲醇分解制一氧化碳和氢气中的催化性能进行了测试。
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引用次数: 22
Adsorption studies and release of selected dyes from functionalized mesoporous MCM-41 silica 功能化介孔MCM-41二氧化硅对染料的吸附及释放研究
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0361-x
Dawid Lewandowski, A. Olejnik, G. Schroeder
AbstractFunctionalized mesoporous MCM-41 silica was subjected to adsorption and release studies of encapsulated guest molecules of three chosen dyes. These mesoporous systems were composed of three different capping reagents introduced by grafting method on the silica surface to control the release of dye molecules at two different pH values. The amounts of dyes adsorbed on the silica surface were measured using ultraviolet-visible (UV-VIS) spectrophotometry. The efficiency of grafting was calculated on the basis of differential thermal analysis (TG) results and elemental analysis. The release profiles were determined for all obtained systems using USP Dissolution Apparatus 2. Adsorption of the two azo dyes used was the most efficient after the positively charged functionalization and lower after functionalization with neutral and negatively charged capping reagents, while the phthalocyanine dye adsorption was almost functionalization-independent. Grafting efficiency was the highest for neutral capping reagent and much lower for electrically charged molecules of other reagents. Release studies showed clearly that desorption was pH-dependent for azo dyes and pH independent for Alcian Blue. The adsorption and release seem to be connected with the electrical charge of all constituents of these systems. Results obtained can be used for further analysis of different electrically charged molecules.
摘要对功能化介孔二氧化硅MCM-41进行了三种染料包封客体分子的吸附和释放研究。这些介孔体系通过接枝方法在二氧化硅表面引入三种不同的封盖剂来控制染料分子在两种不同pH值下的释放。采用紫外-可见分光光度法测定了二氧化硅表面吸附的染料量。根据差热分析(TG)结果和元素分析计算接枝效率。用USP溶出仪2测定了所有体系的释放曲线。两种偶氮染料在正电荷功能化后的吸附效率最高,而在中性和负电荷封盖剂功能化后的吸附效率较低,而酞菁染料的吸附几乎与功能化无关。接枝效率最高的是中性盖层试剂,接枝效率较低的是其他试剂的带电分子。释放研究清楚地表明,偶氮染料的解吸依赖于pH,而阿利新蓝的解吸不依赖于pH。吸附和释放似乎与这些系统中所有成分的电荷有关。所得结果可用于进一步分析不同的带电分子。
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引用次数: 12
Effect of oxidation of nitride coatings on corrosion properties of Ti-6Al-4V alloy in 0.9% NaCl at 40°C 氮化涂层氧化对Ti-6Al-4V合金在0.9% NaCl中40℃腐蚀性能的影响
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0363-8
I. Pohrelyuk, O. Tkachuk, R. Proskurnyak
AbstractThe corrosion properties of Ti-6Al-4V alloy with oxidized thermodiffusion nitride coatings were investigated in isotonic 0.9% solution of NaCl at temperature of 40°C. It was shown that modification of nitride coatings by oxygen leads to a deterioration of the protective properties of nitrided surface of Ti-6Al-4V alloy. The protective properties of the alloy with nitride coatings modified by oxygen are determined by the composition of formed surface oxynitride film.
摘要研究了Ti-6Al-4V合金氧化热扩散氮化涂层在0.9% NaCl等渗溶液中40℃的腐蚀性能。结果表明,氧对氮化层的改性会导致Ti-6Al-4V合金氮化表面防护性能的下降。采用氧改性氮化涂层的合金的防护性能由表面形成的氮化氧膜的组成决定。
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引用次数: 3
Cooligomerization of dominant monomers of C9 fraction of liquid pyrolysis products: comparison of heterogeneous catalytic approach with common methods 液态热解产物C9馏分优势单体的冷聚反应:多相催化方法与普通方法的比较
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0369-2
T. Voronchak, Irena Nykulyshyn, Z. Pikh, Anna Rypka, Z. Gnativ
AbstractCooligomerization of liquid products of the C9 fraction of diesel fuel pyrolysis to produce cooligomers of wide application is suggested to be carried out with silica-alumina catalysts, among which the activated bentonite clay seems to be optimal. Cooligomerization of the mixture simulating the C9 fraction composition was studied to compare the suggested heterogeneous catalytic method with other methods of cooligomers production. Different methods have been compared in terms of yield of cooligomers and their properties, namely molecular weight and its distribution, density, unsaturation and colour. The ratio of monomer units in cooligomer has been determined and the monomers conversion degrees have been calculated for different cooligomerization methods. Reasons of structure and composition differences of cooligomers obtained by different methods are suggested.
摘要建议用硅-氧化铝催化剂对柴油热解C9馏分液态产物进行冷聚反应,制备应用广泛的冷聚物,其中活化膨润土是最佳的催化剂。研究了模拟C9馏分组成的混合物的冷聚反应,并将所建议的非均相催化方法与其他冷聚物生产方法进行了比较。不同的方法在产率和它们的性质,即分子量及其分布、密度、不饱和度和颜色方面进行了比较。测定了冷聚物中单体单元的比例,计算了不同冷聚方式下单体的转化率。指出了不同方法得到的冷聚物结构和组成差异的原因。
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引用次数: 4
Physical-chemical transformations in the system V2O5/(NH4)2Mo2O7 under hydrothermal conditions 水热条件下V2O5/(NH4)2Mo2O7体系的物理化学转变
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0375-4
S. Khalameida, V. Sydorchuk, R. Leboda, J. Skubiszewska-Zięba, V. Zazhigalov
AbstractModified compositions in the system V2O5/(NH4)2Mo2O7 have been prepared by means of mechanochemical, hydrothermal, microwave and ultrasonic treatments in aqueous medium. Chemical and phase transformations occurring on the stages of modification and following calcinations have been studied with the help of XRD, DTA-TG, FTIR and UV-Vis spectroscopy, nitrogen adsorption, and SEM. It has been established that precursors of catalytically active phases possessing meso-macroporous structure have been formed during modification. The comparison of the properties of compositions prepared via different methods has been carried out. Particularly, precursors modified via various procedures possess different morphology.
摘要在水介质中采用机械化学、水热、微波和超声波等方法制备了V2O5/(NH4)2Mo2O7体系的改性组分。利用XRD、DTA-TG、FTIR、UV-Vis光谱、氮气吸附、SEM等研究了改性和煅烧过程中发生的化学和相变。在改性过程中形成了具有介孔-大孔结构的催化活性相前驱体。对不同方法制备的组合物的性能进行了比较。特别是,通过各种方法修饰的前体具有不同的形态。
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引用次数: 4
Application of NRTL activity coefficient model to describe the kinetics of gas adsorption 应用NRTL活度系数模型描述气体吸附动力学
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0367-4
K. Nieszporek, Tomasz Banach, P. Podkościelny
AbstractThe Non-Random Two-Liquid activity coefficient model is applied to describe the kinetics of pure gas adsorption on energetically heterogeneous solid surfaces. The surface energetic heterogeneity has been represented by the Gaussian-like function of the adsorption energy distribution. Two different kinetic isotherms have been presented. One of them, determined by using the statistical rate theory, has been critically discussed. The applicability of the presented approach has been demonstrated by a quantitative analysis of two sets of experimental data previously reported in the literature.
摘要应用非随机双液活度系数模型描述了纯气体在能量非均相固体表面的吸附动力学。表面能的非均质性用吸附能分布的类高斯函数表示。提出了两种不同的动力学等温线。其中一个是用统计速率理论确定的,已经被批判性地讨论过。所提出的方法的适用性已通过对文献中先前报道的两组实验数据的定量分析得到证明。
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引用次数: 0
Oxygen decorating at the one ring and at the N-mouth of (10, 0) aluminum nitride nanotube: A DFT investigation 氧修饰(10,0)氮化铝纳米管的一环和n口:DFT研究
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0372-7
Ahmad Seif, Lila Torkashavand, F. Mohammadi
AbstractWe have investigated oxygen decorating in the (10, 0) aluminum nitride nanotube (AlNNT) by density functional theory. Band gaps, total (TDOS) and partial (PDOS) densities of state and chemical-shielding isotropic (CSI) and chemical-shielding anisotropic (CSA) have been calculated or determined in three models of the investigated (10, 0) AlNNT: pristine (model.0), O-decorating at the one ring in the middle of AlNNT (Model.1) and O-decorating at the nitrogen mouth of AlNNT (Model.2). The results indicated that the dipole moment does not detect the significant effects of dopant whereas TDOS, PDOS and band gap energies detect notable effects. The CSI and CSA values for the Al and N atoms-contributed to the Al-O bonds or those atoms close to the decorated region, in both models of O-decorated AlNNTs are changed.
摘要应用密度泛函理论研究了氧在(10,0)氮化铝纳米管(AlNNT)中的修饰。在所研究的(10,0)AlNNT的三种模型中计算或确定了带隙、状态和化学屏蔽各向同性(CSI)和化学屏蔽各向异性(CSA)的总(TDOS)和部分(PDOS)密度:原始(模型.0)、AlNNT中间一环的o型装饰(模型1)和AlNNT氮口的o型装饰(模型2)。结果表明,偶极矩对掺杂的影响不显著,而TDOS、PDOS和带隙能对掺杂的影响显著。在两种o修饰的AlNNTs模型中,Al和N原子的CSI和CSA值(对Al- o键或靠近修饰区的原子有贡献)都发生了变化。
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引用次数: 1
The crystal structure of Sm4Ni11In20 and its relation to other indium-rich compounds Sm4Ni11In20的晶体结构及其与其它富铟化合物的关系
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0364-7
Y. Tyvanchuk, V. Svitlyk, Mykola Pustovoychenko, Y. Kalychak
AbstractPolycrystalline Sm4Ni11In20 was obtained by arc-melting of metal ingots. A subsequent high temperature treatment was used for single crystal growth. The Sm4Ni11In20 crystal structure (U4Ni11Ga20 type; C2/m, a = 22.5457(3) Å, b = 4.34929(5) Å, c = 16.5479(2) Å, β = 124.592(2)°, R1 = 0.0358, wR2 = 0.0934) was determined by single crystal synchrotron radiation X-ray diffraction from 2014 independent reflections with I > 2σ(I). Sm4Ni11In20 extends the R4Ni11In20 (R = Y, Gd, Tb, Dy, Ho) series of phases. The R4Ni11In20 and RNi3In6 (LaNi3In6 type; R = La, Ce, Pr, Nd, Eu) series have similar compositions. Their structures share similar fragments; in particular the rare earth atom coordination polyhedra are pentagonal prisms with additional atoms.
摘要采用电弧熔炼法制备了Sm4Ni11In20多晶。随后的高温处理用于单晶生长。Sm4Ni11In20晶体结构(U4Ni11Ga20型;单晶同步辐射x射线衍射测定了2014年I > 2σ(I)独立反射的C2/m, a = 22.5457(3) Å, b = 4.34929(5) Å, c = 16.5479(2) Å, β = 124.592(2)°,R1 = 0.0358, wR2 = 0.0934。Sm4Ni11In20扩展了R4Ni11In20 (R = Y, Gd, Tb, Dy, Ho)系列相。R4Ni11In20和RNi3In6 (LaNi3In6型;R = La, Ce, Pr, Nd, Eu)系列具有相似的成分。它们的结构有相似的片段;稀土原子配位多面体是带有附加原子的五角形多面体。
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引用次数: 1
Promoted ternary CuO-ZrO2-Al2O3 catalysts for methanol synthesis 催化甲醇合成的CuO-ZrO2-Al2O3三元催化剂
Pub Date : 2014-02-01 DOI: 10.2478/s11532-013-0368-3
P. Mierczyński, P. Kaczorowski, A. Ura, W. Maniukiewicz, M. Zaborowski, R. Ciesielski, A. Kedziora, T. Maniecki
AbstractTernary CuO-ZrO2-Al2O3 catalysts promoted by palladium or gold were prepared and tested in CO hydrogenation reaction at 260°C under elevated pressure (4.8 MPa). The promotion effect of palladium or gold addition on the physicochemical and catalytical properties of CuO-ZrO2-Al2O3 catalysts in methanol synthesis (MS) was studied. The catalysts were characterized by BET, XRD, TPR-H2, TPD-NH3 methods. The BET results showed that the ternary system CuO-ZrO2-Al2O3 had the largest specific surface area, cumulative pore volume and average pore size in comparison with the promoted catalysts. The yield of methanol can be given through the following sequence: 5%Pd/CuO-ZrO2-Al2O3 > CuO-ZrO2-Al2O3 > 2%Au/CuO-ZrO2-Al2O3. We also found that the presence of gold or palladium on catalyst surface has strong influence on the reaction selectivity. The high selectivity of gold doped ternary catalyst is explained by the gold-oxide interface sites created on the catalyst surface and the acidity of those systems. The higher selectivity to methanol in the case of the palladium catalyst is explained by the spillover effect between Pd and CuO.
摘要制备了钯或金催化的CuO-ZrO2-Al2O3三元催化剂,并在260℃、4.8 MPa高压下进行了CO加氢反应。研究了钯和金对甲醇合成CuO-ZrO2-Al2O3催化剂理化性能和催化性能的促进作用。采用BET、XRD、TPR-H2、TPD-NH3等方法对催化剂进行了表征。BET结果表明,与促进催化剂相比,CuO-ZrO2-Al2O3三元体系具有最大的比表面积、累积孔体积和平均孔径。甲醇的产率顺序为:5%Pd/CuO-ZrO2-Al2O3 > CuO-ZrO2-Al2O3 > 2%Au/CuO-ZrO2-Al2O3。我们还发现,金或钯在催化剂表面的存在对反应选择性有很大的影响。金掺杂三元催化剂的高选择性是由催化剂表面产生的金氧化物界面位点和这些体系的酸性来解释的。钯催化剂对甲醇有较高的选择性是由于钯和CuO之间的溢出效应。
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引用次数: 7
期刊
Central European Journal of Chemistry
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