功能化的介孔分子筛碱催化性能的研究

以苯甲醛与氰乙酸乙酯的Knoevenagel缩合为模型反应，研究了用γ－氨丙基三乙氧基硅烷或γ－乙二胺丙基三甲氧基硅烷功能化的纯硅介也分子筛HMS（Hexagonal mesoporous silica）的碱催化性能。结果表明，除个别碱基负载量高的样品外，功能化样品对反应显示很高的催化活性，反应的初期活性不仅取决于催化剂上活性中心的密度，而且与载体的孔道结构有关。大孔径载体有利于反应物、产物的扩散，故在高负载量时，大孔径样品比小孔样品有更高的活性。此外，还考察了反应温度、溶剂、反应物配比和催化剂用量等条件的影响以及催化剂的重复使用情况。结果表明，反应可在低于100℃的温和条件下进行，有明显的溶剂效应，反应物配比和催化剂用量存在一最佳值；随使用次数的增加，催化剂逐渐中毒而失活。     

CMS/TiO2杂化材料电流变液的制备及其性能

利用特殊的溶胶凝胶方法原位制备了改性淀粉与无机钛氧化物杂化型电流变材料。实验表明,在强电场下其电流变效应比相同组份的淀粉、二氧化钛混合型电流变液有显著提高,直流电场4 kV/mm,剪切速率5 s-1时,静态剪切屈服强度可达4000 Pa以上。同时,抗沉降性明显改善,静置100 h几乎不沉淀。此外,温度效应也获得一定的优化,在10 ℃~90 ℃的工作温度范围内力学性能保持良好,70 ℃时剪切强度达到最大值。     

A STUDY ON ACIDITY AND CATALYTIC PROPERTY OF [B] ZSM-5 CATALYST MODIFIED WITH SILICON COMPOUND BY CHEMICAL SURFACE DEPOSITION OF LIQUID-PHASE TECHNIQUE

The boron heteroatom zeolite catalyst has been modified with silicon compound by Chemical Surface Deposition of Liquid-phase (CLD) technique and the catalytic property of the modified catalyst is studied. Meanwhile, the acidity of the modified zeolite catalysts is characterized through TPD and IR technique, and the fluid adsorption method is used to determine its pore structure. The relationship between the catalytic property of the zeolite catalyst and its pore structure, its acidity has been found. The results of toluene-ethylene alkylation reaction indicate that the selectivity of p-ethyltoluene on the modified zeolite catalyst is higher than that on the zeolite catalyst before silanizated, reaching 94.14%.     

Intermetallic compounds formed at the interface between liquid indium and copper substrates

The interfacial reactions between liquid In and Cu substrates at temperatures ranging from 175°C to 400°C are investigated for the applications in bonding recycled sputtering targets to their backing plates. Experimental results show that a scallop-shaped Cu₁₆In₉ intermetallic compound is found at the Cu/In interface after solder reactions at temperatures above 300°C. A double-layer structure of intermetallic compounds containing scallop-shaped Cu₁₁In₉ and continuous CuIn is observed after the Cu/In interfacial reaction at temperatures below 300°C. The growth of all these intermetallic compounds follows the parabolic law, which implies that the growth is diffusion-controlled. The activation energies for the growth of Cu₁₆In₉, Cu₁₁In₉, and CuIn intermetallic compounds calculated from the Arrhenius plot of growth reaction constants are 59.5, 16.9, and 23.5 kJ/mole, respectively.     

PEG20000中试放大的工艺研究

在一定温度和催化剂作用下 ,分别利用本体聚合和溶剂聚合的方法 ,在 1L、10 0L不锈钢高压反应釜中合成了相对分子质量为 2 0 0 0 0的聚乙二醇 ,并讨论了聚合反应机理 ,研究了催化剂用量、反应温度、反应时间对聚合反应的影响。经过红外、核磁共振、凝胶色谱、化学分析等方法对产物进行了表征。     

Effect of calcination conditions on phase formation and particle size of nickel niobate powders synthesized by solid-state reaction

The solid-state mixed oxide method via a rapid vibro-milling technique is explored in the preparation of single-phase nickel niobate (NiNb₂O₆) powders. The formation of the NiNb₂O₆ phase in the calcined powders has been investigated as a function of calcination conditions by TG-DTA and XRD techniques. Morphology, particle size and chemical composition have been determined via a combination of SEM and EDX techniques. It has been found that the minor phases of unreacted NiO and Nb₂O₅ precursors and the Ni₄Nb₂O₉ phase tend to form together with the columbite NiNb₂O₆ phase, depending on calcination conditions. More importantly, it is seen that optimization of calcination conditions can lead to a single-phase NiNb₂O₆ in an orthorhombic phase.     

Potential of vibro-milling technique for preparation of electroceramic nanopowders

The potential of the vibro-milling technique as a simple method to obtain usable quantities of single-phase electroceramic powders with nanosized particles was examined. A detailed study considering the role of both milling time and firing condition on phase formation and particle size of the final product was performed. The calcination temperature for the formation of the desired phase was lower when longer milling times have been applied. More importantly, by employing an appropriate choice of the milling time and calcination condition, high purity electroceramic nanopowders have been successfully prepared with a simple solid-state reaction method.     

Formation of composites fabricated by exothermic dispersion reaction in A1-TiO2-B2O3 system

The formation of aluminum matrix composites fabricated by exothermic dispersion reaction in A1-TiO2-B2O3 system was investigated. The thermal analysis results show that the reactions are spontaneous and exothermic. The Gibbs free energy of α-Al2O3 is the lowest among all the combustion products, followed by TiB2 and Al3Ti. It is noted that when the B2O3/TiO2 mole ratio is below 1, the reaction products are composed of particle-like α-Al2O3, TiB2 and rod-like Al3Ti. The α-Al2O3 crystallites, resulting from the reaction between A1 and TiO2 or B2O3, are segregated at the grain boundaries due to a lower wettability with the matrix. SEM micrographs show that rod-like Al3Ti phase distributes uniformly in the matrix. When the BEO3/TiO2 mole ratio is around 1, the Al3Ti phase almost disappears in the composites, and the distribution of α-Al2O3 particulates is improved evidently.     

Hydrothermal Reaction Mechanism and Pathway for the Formation of K2Ti6O13 Nanowires

Calculations and detailed first principle and thermodynamic analyses have been performed to understand the formation mechanism of K₂Ti₆O₁₃ nanowires (NWs) by a hydrothermal reaction between bulk Na₂Ti₃O₇ crystals and a KOH solution. It is found that direct ion exchange between K⁺ and Na⁺ plus H⁺ interactions with [TiO₆] octahedra in Na₂Ti₃O₇ promote the formation of an intermediate H₂K₂Ti₆O₁₄ phase. The large lattice mismatch between this intermediate phase and the bulk Na₂Ti₃O₇ structure, and the large energy reduction associated with the formation of this intermediate phase, drive the splitting of the bulk crystal into H₂K₂Ti₆O₁₄ NWs. However, these NWs are not stable because of large [TiO₆] octahedra distortion and are subject to a dehydration process, which results in uniform K₂Ti₆O₁₃ NWs with narrowly distributed diameters of around 10 nm.     

Research on charge ordering and magnetic properties in La0.3Ca0.7Mn1-xWxO3 system

The perovskite manganite sample La0.3Ca0.7Mn1-xWxO3 （x = 0.08, 0.12） was prepared by the solid-state reaction method. The effect of W doping on the Mn site to La0.3Ca0.7MnO3 charge ordering phase and the changing process of magnetic properties were studied through the measurement of the M-T curve, M-H curves, and ESR curves of the sample. The results showed that when x = 0.08, the charge ordering （CO） phase exists in the system, the transition temperature Tco= 275 K, and the system exhibits PM when T 〉 275 K. The system transforms from spin-disordering paramagnetism to spin-ordering antiferromagnetism in the charge ordering state with the temperature decreasing from 275 K to 230 K. The long-range antiferromagnetism forms and AFM/CO states coexist between 230 K and 5 K. There is a little ferromagnetic component in the AFM/CO background in a low temperature range. When x = 0.12, the CO phase in the system has almost melted completely. There is a little remnant of the CO phase below 150 K. The system exhibits paramagnetism when T 〉 150 K and transforms from paramagnetism to ferromagnetism when T〈 150 K.