稀土固体超强酸SO_4~(2-)/TiO_2-Ce~(4 )直接法催化合成聚乳酸及其机理的研究

对稀土固体超强酸SO_4~(2-)/TiO_2-Ce~(4 )催化剂直接法催化合成聚乳酸反应机理进行了研究,实验结果表明:SO_4~(2-)/TiO_2-Ce~(4 )直接法催化剂合成聚乳酸的聚合机理是酸性聚合,酸性越强所合成聚乳酸的分子量越高。     

介孔SO2-4/TiO2固体超强酸的制备与表征

以工业硫酸钛液为原料,分步水解制得吸附硫酸根的介孔偏钛酸,焙烧得到介孔SO2-4/TiO2固体超强酸.用Hammett指示剂法、XRD、BET和FI-IR等多种手段对催化剂进行了表征;以乙酸乙酯的合成为模型反应,考察了催化活性.结果表明所制备的SO2-4/ TiO2催化剂是介孔结构;随着焙烧温度的升高和SO2-4含量的增加,其比表面积和酸强度都先增大后减小,最高酸强度H0=-14.52,最大比表面积为192m2/g;酸强度及硫含量与催化活性都有着密切联系,在500℃下焙烧,硫含量为2.7%时,催化活性最高.     

固体超强酸催化合成丁酸戊酯的研究

以Ti(OC4H9)4为原料,采用溶胶-凝胶法制备固体超强酸SO4 2-/TiO2,并利用XRD、IR及DRS对催化剂进行表征,然后,以SO4 2-/TiO2为催化剂,通过丁酸与戊醇反应合成了丁酸戊酯.探讨了SO4 2-/TiO2催化酯化反应机理及SO4 2-/TiO2的结构,讨论了影响酯化率的主要因素,实验结果表明,当催化剂用量为0.6g,醇酸摩尔比为1.4:1,反应温度为125℃,反应时间为6h时,平行实验的平均酯化率可达96.4%.     

锐钛矿SO42-/TiO2纳米光催化剂的制备及其性能

采用溶胶-凝胶-浸渍法制备了锐钛矿型SO42-/TiO2纳米光催化剂,并通过X射线衍射(XRD)、BET比表面积测量和透射电镜(TEM)对其进行了表征。以对苯二甲酸作为探针分子,结合化学荧光技术研究了光催化剂表面羟基自由基的生成;在紫外和可见光的照射下,以甲基橙为光催化反应的模型化合物,研究了锐钛矿型SO42-/TiO2纳米光催化剂的光催化活性。结果表明:SO42-负载使锐钛矿TiO2的比表面积增加,吸附量增加,光催化活性提高;SO42-/TiO2纳米光催化剂的羟基自由基的生成速率越大,催化剂的催化活性越高;浸渍液H2SO4的浓度对SO42-/TiO2纳米光催化剂的吸附量、羟基自由基的生成速率和催化活性有一定的影响,H2SO4的最佳浓度为0.2mol/L。     

SO_4~(2-)/TiO_2-SiO_2固体超强酸失活原因及再生方法研究

以SO42-/TiO2-SiO2固体超强酸催化剂为例,选择松香与甘油酯化这一高粘度有机反应体系,通过IR、TPD、XRD和BET等检测方法,研究了SO42-/TiO2-SiO2的失活原因。研究表明,催化剂表面吸附有机物、酸中心减少、酸量下降是导致该催化剂失活的主要原因。在此基础上研究了再生方法,优化了再生条件:在500℃焙烧脱去吸附物,再用H2SO4浸渍对失活催化剂进行再生。再生催化剂的催化性能与新鲜催化剂性能基本相同。     

介孔SO_4~(2-)/TiO_2固体超强酸的制备与表征

以工业硫酸钛液为原料,分步水解制得吸附硫酸根的介孔偏钛酸,焙烧得到介孔SO42-/TiO2固体超强酸。用Hammett指示剂法、XRD、BET和FI-IR等多种手段对催化剂进行了表征;以乙酸乙酯的合成为模型反应,考察了催化活性。结果表明所制备的SO42-/TiO2催化剂是介孔结构;随着焙烧温度的升高和SO42-含量的增加,其比表面积和酸强度都先增大后减小,最高酸强度H0=-14.52,最大比表面积为192m2/g;酸强度及硫含量与催化活性都有着密切联系,在500℃下焙烧,硫含量为2.7%时,催化活性最高。     

纳米固体超强酸 SO42- /TiO2的氧敏特性研究

采用溶胶-凝胶法制备了TiO2,再用浸渍法制备纳米固体超强酸SO42-/TiO2,用XRD、TEM、IR、XPS和比表面测量等方法进行表征。结果表明纳米固体超强酸SO42-/TiO2的粒径(≤30nm)比TiO2小,并且具有很大的比表面积,Ti4+离子与SO42-的结合形式为无机双齿螯合型结构,酸强度用乙酸乙脂合成模型实验测定,确定纳米SO42-/TiO2为超强酸(SO42-/TiO2脂产率≥H2SO4脂产率)。利用固体超强酸SO42-/TiO2和纯TiO2纳米粉体分别制作成厚膜型气敏元件,固体超强酸SO42-/TiO2氧敏元件的灵敏度和工作温度等技术指标均优于纯TiO2,还进一步讨论了其氧敏特性和结构之间的关系。     

纳米固体超强酸SO^2—4／TiO2的氧敏特性研究

采用溶胶－凝胶法制备了TiO2,再用浸渍法制备纳米固体超强酸SO^2-4/TiO2,用XRD、TEM、IR、XPS和比表面测量等方法进行表征。结果表明纳米固体超强酸SO^2-4/TiO2的粒径（≤30nm）比TiO2小,并且具有很大的比表面积,Ti^4 离子与SO^2-4的结合形成为无机双齿螯合型结构,酸强度用乙酸乙脂合成模型实验测定,确定纳米SO^2-4/TiO2为超强酸（SO^2-4/TiO2脂产率≥H2SO4脂产率）。利用固体超强酸SO^2-4/TiO2和纯TiO2纳米粉体分别制作成厚膜型气敏元件,固体超强酸SO^2-4/TiO2氧敏元件的灵敏度和工作温度等技术指标均优于纯TiO2,还进一步讨论了其氧敏特性和结构之间的关系。     

SO2-4修饰Co-TiO2光催化剂制备及光解水制氢

采用溶胶-凝胶法制备了Co掺杂TiO2光催化剂,并用浸渍法对其表面进行SO2-4修饰,借助于X射线衍射(XRD)、红外吸收光谱(FT-IR)及紫外-可见吸收光谱(UV-Vis)等分析手段对所制备的催化剂进行表征,并对其光催化分解水制氢性能进行了研究。结果表明,Co掺杂TiO2显示出明显的可见光响应,对其表面进行SO2-4修饰能进一步提升其光催化活性。当Co掺杂量为2.0%(原子分数),SO2-4的修饰量为8.0%(质量分数),焙烧温度为500℃时,所制催化剂催化活性最高,其产氢速率为171.3μmol/h。     

介孔SO4^2-／TiO2固体超强酸的制备与表征

以工业硫酸钛液为原料，分步水解制得吸附硫酸根的介孔偏钛酸，焙烧得到介孔SO4^2-／TiO2固体超强酸。用Hammett指示刑法、XRD、BET和FI—IR等多种手段对催化剂进行了表征；以乙酸乙酯的合成为模型反应，考察了催化活性。结果表明所制备的SO4^2-／TiO2催化剂是介孔结构；随着焙烧温度的升高和SO4^2-含量的增加，其比表面积和酸强度都先增大后减小。最高酸强度H0=14．52，最大比表面积为192m^2／g；酸强度及硫含量与催化活性都有着密切联系。在500℃下焙烧，硫含量为2．7%时，催化活性最高。     

Quaternary system Li2MoO4-Na2MoO4-CaMoO4-BaMoO4

The Li₂MoO₄-Na₂MoO₄-CaMoO₄-BaMoO₄ quaternary system was studied by differential thermal analysis and direct visual observation. Three invariant points, two peritectic and one eutectic, were located.     

Synthesis and Properties of Zn2TiO4–Zn2SnO4–ZnFe2O4 Solid Solutions

Zn₂TiO₄–Zn₂SnO₄–ZnFe₂O₄ mixed oxides are prepared by low-temperature hydrogen–oxygen plasma synthesis and solid-state reactions. Zn_{2 – x} (Ti _a Sn _b )_{1 – x} Fe_2x O₄ (a+ b = 1, x = 0–1.0) solid solutions are shown to have an inverted cubic spinel structure (sp. gr. Fd3m). The lattice parameter, electrical conductivity, band gap, and molar polarizability of about 100 samples are determined. With increasing Fe content, the lattice parameter, degree of spinel inversion, density, activation energy, and polarizability of the solid solutions decrease, while their conductivity rises.     

Synthesis and characterization of Na2Pb2Pr2W2Ti4Ta4O30

A new complex oxide (Na₂Pb₂Pr₂W₂Ti₄Ta₄O₃₀) of tungsten bronze structural family has been synthesized by a high-temperature solid-state reaction (mixed-oxide) route at 1,050 °C. Room temperature structural analysis shows the formation of a single phase new compound. Study of microstructure of the pellet sample, recorded by scanning electron microscope, exhibits the uniform distribution of different size and shape of grains (with a few small voids) on the surface of the sample. Detailed studies of dielectric properties as a function of frequency and temperature show a dielectric anomaly above room temperature suggesting the existence of a ferroelectric phase transition in the material. Impedance spectroscopic analysis and electrical conductivity of the material exhibit a strong correlation between microstructure and electrical parameters. The temperature dependence of dc conductivity of the compound follows Arrhenius equation. The frequency and temperature dependence of ac conductivity (with fittings) shows the signature of Jonscher’s universal power law. The existence of non-exponential-type of conductivity relaxation in the compound was confirmed.     

The spinels CoRh2O4 and Co2RhO4

Polycrystalline CoRh₂O₄ and Co₂RhO₄ are cubic, spinel-type double oxides, S.G. Fd3m (No. 227), Z = 8. For CoRh₂O₄, $\text{a}\text{= 8.4992(1)}\text{A}\text{?}$, $\text{U = 613.95(3)}\text{A}\text{?}{}^3$, D_X = 7.11 Mgm^?3, $\text{x}\text{= 0.257}$, Co in 8(a) positions, R = 0.043. For Co₂RhO₄, $\text{a}\text{= 8.299(2)}\text{A}\text{?}$, $\text{U = 517.6(5)}\text{A}\text{?}{}^3$. D_X = 6.62 Mgm^?3, $\text{x}\text{= 0.261}$, half the Co content in 8(a) positions, R = 0.041. IR absorption band frequencies for both spinels are included.     

硫酸-草酸混合法硬质阳极氧化溶液的分析

1　前　言　　混合酸阳极氧化法是指用含有两种或以上的无机酸或有机酸的混合水溶液对工件进行的阳极氧化。它适用于硬质氧化膜和自然着色法的有机酸电解着色 ,与单一酸阳极氧化法相比有如下优点 :(1)在 10～ 2 0℃下电解 ,能获得耐磨性好的氧化膜和高着色率 ;(2 )实行高电流密度的混合酸电解 ,可防止氧化膜溶解 ,并可在较高温度下有效地形成硬质氧化膜 ;(3)可在较高的温度下实施 ,降低生产成本 ,有利于生产。该法获得的膜层的性能与溶液的成分密切相关 ,因而要求对溶液实行监控分析。然而 ,目前的分析基本上都是沿用单一酸电解液法进行 ,其…     

Large-scale growth of Cu2ZnSnSe4 and Cu2ZnSnSe4/Cu2ZnSnS4 core/shell nanowires

We present a fast and simple protocol for large-scale preparation of quaternary Cu(2)ZnSnSe(4) (CZTSe), as well as CZTSe/Cu(2)ZnSnS(4) (CZTS) core/shell nanowires using CuSe nanowire bundles as self-sacrificial templates. CuSe nanowire bundles were synthesized by reacting Cu(2 - x)Se nanowire bundles with sodium citrate solution. CZTSe nanowires were prepared by reacting CuSe nanowire bundles with Zn(CH(3)COO)(2) and SnCl(2) in triethylene glycol. X-ray diffraction (XRD) and selected area electron diffraction studies show that stannite CZTSe is formed. The formed CZTSe nanowire bundles have diameters of 200-400 nm and lengths of up to hundreds of micrometers. CZTSe/CZTS nanocable bundles with similar morphologies were grown by the addition of some elemental sulfur to the reaction system for growth of CZTSe bundles. The stannite CZTSe/kesterite CZTS core/shell structure of the grown nanocables was confirmed by XRD and high-resolution transmission electron microscope investigation. The influence of S/Se molar ratio in the reaction system on the crystallographic structures and optical properties of CZTSe/CZTS nanocables was studied. The obtained CZTSe/CZTS core/shell nanocable bundles show broad and enhanced optical absorption over the visible and near-infrared region, which is promising for use in photovoltaic applications.     

Liquidus relations in the Li2WO4-Na2WO4-CaWO4 system

Phase relations in the Li₂WO₄-Na₂WO₄-CaWO₄ system were studied by physicochemical analysis. The liquidus surface was mapped out, and the compositions and temperatures of invariant points were determined.