两种络合剂对Ce-Sn-O复合氧化物结构与性能的影响

分别以柠檬酸、葡萄糖为络合剂, 用溶胶-凝胶法制备了CeO2和掺杂少量Sn的Ce-Sn-O复合氧化物, 利用XRD、TPR、FT-IR、比表面法、TEM等方法表征了四种催化剂的物理化学性质, 同时以甲烷催化燃烧反应为探针对其进行了活性评价. 结果表明, 以葡萄糖为络合剂合成的掺杂锡后的样品其甲烷完全转化温度较低, 比表面积较大, 通过透射电子显微镜观察, 平均晶粒大小为14 nm 左右, 且分散性良好, 而相比之下柠檬酸为络合剂合成的样品出现明显的团聚现象.     

硝酸铕与二甲基甲酰胺配合物的研究

一、配合物合成及溶解性 配合物按文献[1]的方法合成,为微红色粉末,易溶于水、DMF、DMSO、乙醚、甲醇、乙醇、丙酮、氯仿,不溶于甲苯、二甲苯、CCl_4。 二、分析方法及实验条件 分析方法和实验条件同文献[1];燃烧能的测定仪器、实验条件,量热计当量计算和热交换校正,燃烧焓的换算和生成热的计算同文献[2]。 结果与讨论 一、配合物的性质 1.组成分析 元素分析实验值(％):Eu27.26,C20.07,H3.76,N14.85;计算值(％):Eu27.27,C19.40,H3.80,N15.08。 2.熔点及X-射线粉末衍射分析 配合物熔点为102.0～102.5℃;配合物及硝酸铕水合物     

étude thermodynamique de certains médicaments

Two compounds of sulphamide type:p-amino-benzene sulphonamide (I) and 3,4-dimethylisoxazol 5-sulphanylamide (II) were studied by combustion calorimetry and by differential scanning calorimetry (DSC).The enthalpies in solid state at 298,15 K of combustion, _c H _m ^o (I)=-2788,5±1,6 kJ mol^–1, _c H _m ^o (II)=-5036±3,8 kJ mol^–1 and of formation, _f H _m ^o (I)=-458,3±1,6 kJ mol^–1, _fH _m ^o (II)=-180,1±3,8 kJ mol^–1 were determined.The thermal effects concerning the melting and phase transition of this compounds were also measured.

     

燃烧过程中碱/碱土金属对重金属迁移转化影响的研究进展

碱/碱土金属广泛存在于各种固体燃料中，在燃烧过程中碱/碱土金属与燃料中重金属及其他矿物发生复杂的物理化学反应，从而影响重金属的迁移和转化。本研究主要介绍了碱/碱土金属对As、Se、Pb和Cr四种重金属迁移转化的影响规律，包括碱金属和碱土金属对重金属迁移转化的影响，颗粒物团聚与黏结对重金属排放的影响三个方面。碱/碱土金属能够抑制重金属的挥发：碱金属与Cl元素的结合，降低了PbCl₂的生成；碱金属的存在有利于提升高岭土对Pb的吸附效率；碱/碱土金属可以与As和Se形成稳定的化合物。但同时需要注意碱/碱土金属与Cr的部分结合产物中，Cr以六价态存在，具有较高的毒性。碱/碱土金属对于团聚现象发生，分别起到了促进和抑制作用，适当含量的碱金属有利于减少重金属的释放。通过总结碱/碱土金属对重金属迁移转化的影响规律，以期为降低重金属的危害提供思路。     

Mechanism of coal char burning at a low oxygen content in the feed stream

Evolution of the internal pore structure during the combustion of two different types of coal chars is compared. In this study brown coal char prepared from brown coal (coal-mine Nováky) by drying and devolatilization, and commercial black coal char (provided by U.S. Steel Košice) were used. Particles were combusted to different degrees of burnout at an initial temperature of 800°C in a low oxygen containing atmosphere (5 vol%). It was shown that the combustion of both types of coal chars proceeds via the same shell progressive mechanism, despite differences in their original internal pore structure. The internal surface area of the brown coal char particles mainly belongs to the region of micropores, while for the black coal char is typical its macropore structure. Inside the brown coal particle cores pore structure evolution was observed. This change of the structure was caused by the reaction between solid carbon and carbon dioxide, due to which the specific surface area in the region of micropores significantly increased. This revised version was published online in August 2006 with corrections to the Cover Date.     

Catalytic Combustion of Methane over MnOx／ZrO2-Al2O3 Catalysts

MnOx/Al2O3 and MnOx/ZrO2-Al2O3 catalysts were prepared by incipient wetness impregnation of Mn(CH3COO)2 on the corresponding supports, followed by the characterization using X-ray diffraction (XRD). temperature programmed reduction (TPR) and BET surface area techniques. The result shows the BET surface area of ZrO2-Al2O3 is lower than that of Al2O3 due to the loading of ZrO2.However tile resulted MnOx/ZrO2-Al2O3 catalyst exhibits higher activity for methane combustion than MnOx/Al2O3, because the addition of ZrO2 onto Al2O3 is beneficial for the dispersion of Mn species and the improvement of the lattice oxygen activity in MnOx. subsequently the activation of methane during combustion. The optimum loading of Zr in MnOx/ZrO2-Al2O3 is in the range of 5%-10% correlated with the calcination temperatures of catalyst supports.     

Potentiometric microdetermination of aluminium in organic compounds after combustion in a modified oxygen flask

The microdetermination of aluminium in organic compounds by oxygen flask combustion, a simultaneous fusioncombustion procedure was developed, in which the sample in a mixture with KHSO₄ is burnt in a modified oxygen flask under suitable conditions so that the alumina formed is immediately converted into the corresponding water-soluble sulfate. 2.4 ml of 6M HCl are used as absorption solution, in which the combustion residue is completely dissolved by boiling. The solution is then transferred to a titration cell, neutralized with NaOH in the presence of methyl red, and the Al(III) is finally determined in a buffered 40% (V/V) dioxane solution by potentiometric titration with 0.1 M NaF. The results obtained were accurate within ±0.13%; the recoveries of Al are in the range of 99.00 to 99.90%; the standard deviation amounts to 0.06%. The potentiometric titration of Al(III) with fluoride as well as the conditions of the oxygen flask combustion of organic aluminium compounds are discussed.     

Combustion Derived Ultrafine γ-Fe2O3 Structure,morphology and thermal studies

A novel combustion method of employing poly(ethylene glycol) with the precursor in a fixed ratio for the synthesis of ultrafine γ-Fe₂O₃ through a self-propagating combustion synthesis is reported. Four different precursors viz. ferrous hydroxide, ferrous oxalate dihydrate, ferric 8-hydroxyquinoline and ferric acetylacetonate are employed in this study for the conversion of these precursors to ultrafine g-Fe₂O₃ particles. The as synthesized γ-Fe₂O₃ samples are characterized by XRD, SEM and thermal techniques. A case study for the synthesis of γ-Fe₂O₃ employing ferric acetyl acetonate as precursor is reported. The importance of employing thermal analysis techniques in understanding the combustion synthesis is envisaged. This revised version was published online in July 2006 with corrections to the Cover Date.     

超临界干燥方法对甲烷燃烧催化剂LaMnAl11O19结构及活性的影响

 摘要：用水热合成法制备了锰取代的六铝酸盐催化剂，并比较了超临界干燥法和普通烘箱干燥法对催化剂结构及甲烷燃烧反应活性的影响．DTA－MS结果表明，超临界干燥过程中，催化剂前驱物中的表面铝羟基部分被乙氧基取代．这种表面修饰作用可保持铝分散的均匀性，使催化剂前驱物中碳酸锰和碳酸镧的分解温度明显降低，且氢氧化铝的脱水温度维持在较适宜的范围内；焙烧后，易形成六铝酸盐相．甲烷燃烧反应结果表明，用超临界干燥方法制得的催化剂对甲烷燃烧反应的催化活性明显高于用普通烘箱干燥方法制得的催化剂．     

煤和油页岩燃烧过程的对比

利用改装热重差热仪,对抚顺、茂名油页岩、黄县褐煤和大同烟煤进行了燃烧实验,考察了粒径、燃烧终温、样品种类等因素对燃烧过程的影响。样品粒径范围为2—8mm,升温速率范围为350—600℃/min,燃烧终温为750—900℃。结果表明,在不到2min的升温段,油页岩燃烧转化率可达90%以上,而煤仅为30—50%,其值与煤的挥发份分析值基本一致。