镧系元素的双(九钨二钒)杂多酸钾的合成与表征

报道了镧系元素钨钒杂多配合物的合成方法。元素分析和热重分析确定其通式为：Ｋ１０Ｈ７〔Ｌｎ（Ｖ２Ｗ９Ｏ３７）２〕·ｘＨ２Ｏ（Ｌｎ＝Ｓｍ３＋、Ｅｕ３＋、Ｇｄ３＋）。利用红外（ＩＲ）、紫外（ＵＶ）和Ｘ射线衍射谱对其进行了表征。配合物的热解性质研究表明，其分解温度范围为４００～４５０℃。     

Nitric oxide reduction and carbon monoxide oxidation over carbon-supported copper-chromium catalysts

Carbon supported copper-chromium catalysts are shown to be very active for both the reduction of nitric oxide with carbon monoxide and the oxidation of carbon monoxide with oxygen. Mixed copper-chromium oxide active phases have good activity in the simultaneous removal of nitric oxide and carbon monoxide from exhaust gases. The influence of several catalyst variables has been investigated. The activity per volume of catalyst increases with increasing loading, while the intrinsic activity shows a maximum around C/M=100−50. An optimum catalyst for nitric oxide reduction and carbon monoxide oxidation has a copper/chromium ratio of 2/1. The apparent activation energy for the carbon monoxide oxidation over carbon supported copper-chromium catalysts is 77 kJ/mol, suggesting that the Cu---O bond rupture is the rate-limiting process. The reduction of nitric oxide takes place at higher temperatures. Since all catalysts have a low selectivity for molecular nitrogen formation at lower temperatures, the dissociation of nitric oxide is probably rate determining, resulting in a slightly reduced catalyst system. In an excess of carbon monoxide the reaction is first-order in nitric oxide and zero-order in carbon monoxide. Moisture inhibits the reaction by reversible competitive adsorption, whereas carbon dioxide does not. Oxygen completely inhibits the reduction of nitric oxide due to the more rapid reoxidation of the catalytic sites compared to nitric oxide. Therefore, the reduction of nitric oxide takes place only when all oxygen has been converted and, hence, is shifted to higher temperatures. As a possible consequence, the production of nitrous oxide is reduced. Nitric oxide and molecular oxygen react preferentially with carbon monoxide, so, in an excess of oxidizing component, gasification of the carbon support occurs at higher temperatures after carbon monoxide has been completely consumed.     

JFC磷酸酯的合成和应用

详述了JFC磷酸酯的合成工艺路线，以及它在织物前处理精练工艺中的应用。与其它磷酸酯类精练剂性能对比，证明它可作为一种性能优良的精练剂中的添加剂。     

合成直链烷基苯的锆磷铝固体酸催化剂 I.催化剂合成及其影响因素

合成了一系列用于苯与直链烯烃烷基化反应的含有杂原子的磷铝分子筛固体酸催化剂 (MeZrAPO 5 ) ,同晶取代磷铝分子筛骨架中磷和铝的杂原子包括锆和至少一种选自硅、硼、镓、锗、铁、镁、锡等的元素。考察了晶化温度、晶化时间、杂原子种类、铝源等因素对催化剂合成的影响 ,探索了合成样品中模板剂脱除的最佳条件。结果表明 ,晶化温度高于 15 0℃、n(TEA) /n(Al2 O3 )≥ 1 5以及加入Zr原子都有利于直接生成MeZrAPO 5晶相 ;用小晶粒和高结晶度的铝源合成时 ,分子筛的结晶度高。     

含氯取代基的聚间苯二甲酰间苯二胺的合成与表征

以 2 ,5 -二氯对苯二甲酰氯作为第三单体 ,将其与间苯二甲酰氯、间苯二胺在N ,N -二甲基乙酰胺中进行低温溶液共缩聚反应 ,合成了含氯取代基的聚间苯二甲酰间苯二胺。研究了单体摩尔浓度、反应初始温度、叔胺添加剂种类、第三单体用量等对共聚物相对分子质量的影响 ,并用红外光谱、热重分析等方法对共聚物进行了表征。     

金刚石膜的计算机虚拟制备技术中的分子动力学模拟

综述了近年来金刚石薄膜形成过程的分子动力学（Molecular Dynamics，简称MD）模拟研究，详细地阐述了原子间相互作用势的选取，总结了不同沉积条件下MD的计算模型和几种典型情况下的模拟结果。研究表明：在原子尺度上，MD方法能较全面地提供有关膜生长的信息，对进一步了解金刚石膜形成的微观机制以及为细观层次仿真提供基本信息均具有重要意义。     

由乙腈一步法制备乙酸丁酯的研究

以丁醇和制备丙烯腈的副产物乙腈为原料 ,采用一步法合成了乙酸丁酯。通过正交实验得到了影响反应的 4种因素。确定了最佳的工艺条件为 :催化剂的量为样品质量的 40 % ;n(CH3CN)∶ n(C4 H9OH) =1∶ 1 .0 5 ;反应温度为 1 0 5℃ ;反应时间为 8h。在此反应条件下 ,乙酸丁酯的收率为 88.8% ,纯度可达 99.5 %。并用气相色谱及红外光谱对产品的纯度进行了表征     

The Synthesis of Sulfated Titanium Oxide Nanotubes

TiO₂ nanotubes can be prepared in gram quantities by treating anatase TiO₂ powder with concentrated NaOH solution. These TiO₂ nanotubes acquired strong acidity after being impregnated with sulfuric acid solution and calcined at 300 °C. The anatase TiO₂ powder used to prepare the nanotube did not catalyze the esterification between cyclohexanol and acetic acid, while sulfated TiO₂ nanotubes were very reactive toward the esterification reaction.     

Growth Stresses in the Oxide Scales on TiAl Alloys at 800 and 900°C

In the oxidation of TiAl alloys, the role of scale-growth stresses formed during oxidation has, thus far, been unknown. In the present paper the oxide-growth stresses were investigated by the deflection-test method in monofacial oxidation (DTMO) accompanied by acoustic-emission measurements. On unmodified surfaces the growth stresses are compressive and reach levels of around –100 MPa. At the same time, significant acoustic emission occurs indicating that even under isothermal conditions, stresses are relieved by a scale-cracking mechanism. For oxide scales on TiAl surfaces, which had been ion implanted with chlorine before oxidation, a very thin protective alumina layer is formed which, however, develops growth stresses in the range of several GPa, accompanied by intensive acoustic emission. In all stress–time curves, a dynamic situation is observed. This consists of phases of stress relief by scale microcracking and phases of stresses increase due to crack healing and further oxide growth. As a result, the level of stress as a function of oxidation time, is characterized by an oscillating course.     

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。