7-氨基-6-氰基-5-(3-硝基苯基)吡喃并嘧啶-2,4-二酮的合成

报道了常温、超声辐射、水中、无催化剂条件下，以3-硝基苯甲醛、丙二腈和巴比妥酸为原料合成标题化合物的方法。考察了超声技术、反应时间及反应温度对反应的影响。最佳反应条件为：室温、超声辐射2h，收率为86．2％。     

纳米Fe2O3的制备与气敏性质的研究

报道了纳米氧化铁的制备工艺，采用沉淀法、溶胶凝胶法制备了纳米α-Fe2O3、γ-Fe2O3粉体，用热重－差热分析（TG－DTA）、X射线衍射（XRD）、透射电镜（TEM）和二次粒度分布对粒子进行表征，并制作了气体敏感元件。讨论了纳米氧化铁的制备工艺对气敏性质的影响。     

氯化铜脱除硫化氢气体制硫磺研究

A novel technology of removing H2S with cupric chloride solution was developed in this paper. Cupric as the form of CuS deposition, the CuS produced was then oxidized by excessive cupric ion in another reactor meanwhile cupric ion that has been consumed can be recovered by the oxidization of CuCl2- with oxygen in air,and the solution can be circulated. Moreover, the leaching kinetics of CuS by cupric ion was studied. The removal efficiency of H2S is close to 100%, and the required operating condition is mild. Compared with other wet oxidization methods, no raw material is consumed except O2 in air, the process has no secondary pollution and no problem of degradation and scale, and the absorbent is much stable and reliable.     

SULFUR RECOVERY WITH REDUCED EMISSIONS, LOW CAPITAL INVESTMENT AND HYDROGEN CO-PRODUCTION

The main disadvantage of the Claus process is that by introducing air as oxidant a large volume of tail gas is produced. This must be treated to reduce atmospheric emissions of sulfur-containing gases. The costs of the tail-gas unit are a significant fraction of the total capital and operating costs for sulfur recovery. A new process uses thermal decomposition of hydrogen sulfide in the presence of carbon dioxide instead of air oxidation. The products of this reaction are hydrogen, carbon monoxide, elemental sulfur, water vapor and carbonyl sulfide. Carbonyl sulfide is easily converted to H₂S and C0₂ by liquid- or vapor-phase hydrolysis. Unreacted H₂S and C0₂ are recovered by absorption and recycled to the reactor. Since no air is introduced, there is no tail gas and the tail-gas unit is eliminated, giving a substantial reduction in capital investment. The concentrations of sulfur-containing gases in the product streams depend only on the operation of the absorber and stripper units and can be controlled to very low levels by increasing stripper boil-up. Process operating costs depend on the level of sulfur recovery required and can also be much lower than those of the modified Claus Process.

The process chemistry depends on a shift in the equilibrium of H₂S decomposition caused by reaction of hydrogen with C0₂ by the reverse of the water-gas-shift reaction. Catalysts for this chemistry have been identified. Reactor conversion is further improved by rapid cooling of the reactor effluent gas. Other aspects of process design and operation confer further advantages with respect to the Claus process; however, the process equipment used is similar to that used in a Claus plant. Retrofit of existing plant to the new technology can therefore be considered.     

国外过氧化氢在化学合成中应用研究进展

介绍了近期国外过氧化氢在部分化学品合成中应用研究新进展 ,产品包括过碳酸钠、过碳酰胺、4Na2 SO4·2H2 O2 ·NaCl加合物、叔胺氧化物、水合肼、二羟基苯、季铵盐过氧化氢和甲乙酮肟。内容涉及产品质量 (纯度、安定性、溶解速率、外观等 )、产品收率、催化剂、工艺过程等方面改进。主要介绍专利技术。     

2-苯基-1,2-苯并异硒唑-3-(2H)-酮的合成研究

在N2保护下,采用水合肼的碱性水溶液还原硒粉制备了K2Se2,不经分离直接与邻氨基苯甲酸的重氮盐反应得到了中间体2,2'-二硒化苯甲酸;在环合反应合成2-苯基-1,2-苯并异硒唑-3-(2H)-酮(Ebselen)时改用了乙醚-水为反应体系,K2CO3水溶液作为副产物HCl的吸收剂,促使胺解关环反应顺利进行,产物易分离、纯化得2-苯基-1,2-苯并异硒唑-3-(2H)-酮。     

碳铵化肥发青问题解决小结

探讨了该厂化肥生产中碳铵发青的原因,通过硫化氢含量的测定,分析了系统内外影响因素,提出了解决措施,达到了不停车稳定产品质量的目的。     

从假性紫罗兰酮合成β-紫罗兰酮中主要副产物(I)的分离鉴定

假性紫罗兰酮在浓硫酸及 - 2 0°C低温条件下反应 ,主要生成 β-紫罗兰酮 ,少量的 α-及 γ-紫罗兰酮 ,同时生成副产物 ( I)及 ( II)。用 IR、1H NMR及 MS光谱分析方法 ,对副产物 ( I)进行了结构鉴定 ,结构为 3,4,4a,5 ,8,8a-六氢 - 2 ,5 ,5 ,8a-四甲基 - 2 H - 1 -苯并吡喃     

Investigation of bio-ethanol steam reforming over cobalt-based catalysts

The catalytic performance of cobalt catalysts supported on γ-Al₂O₃, TiO₂, ZrO₂ were studied for bio-ethanol steam reforming (BESR) reaction. The supported catalysts (10 wt%Co) were prepared by impregnation and characterized through Thermogravimetric analysis (TGA), H₂ chemisorption, laser Raman Spectroscopy, Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFTS), and temperature-programmed reaction (TPRxn). The metallic cobalt sites were found to correlate with the BESR reaction activity. The reaction and H₂ chemisorption showed that ZrO₂ supported catalyst showed the best dispersion and best catalytic activity. Over the 10% Co/ZrO₂ catalyst, using a H₂O:EtOH:inert molar ratio of 10:1:75 and a GHSV = 5000 h⁻¹, 100% ethanol conversion and a yield of 5.5 mol H₂/mol EtOH were obtained at 550 °C and atmospheric pressure.     

低(等)压合成氨的最佳H2/N2与催化活性的关系

采用高压催化剂性能评价实验装置，在压力分别为7.0,10.0和15.0MPa，温度分别为350,400和450℃条件下，在H2／N2为1.6-3.0范围内研究了H2／N2对A301，ZA－5和A110－2型催化剂的活性和合成塔出口氨浓度的影响。在压力和空速一定的条件下，最佳H2／N2随反应温度而异。在350，400和450℃下，最佳H2／N2分别为1.8-2.2,2.2-2.5和2.5-3.0。由此可见，合成氨反应的速率达到最大值时的最佳H2／N2值与反应的进程有关。为此提出了催化剂效率K（Catalysis efficiency)的概念来表征在催化剂作用下反应器出口氨浓度趋近平衡的程度，即K＝CNH3／C^*NH3。根据实验结果，得到了最佳H2／N2与催化剂效率的定量关系：（H2／N2）m=1.5(1 CNH3/C^*NH3)=1.5(1 K)。由此可以根据催化剂在不同反应条件下的催化剂效率来确定最佳H2／N2。凡是会降低催化剂效率的因素，都会使最佳H2／N2降低。各种影响因素对最佳H2／N2的影响中，反应温度的影响最大，其次是空速和催化剂的活性，而压力和惰性气体含量的影响相对较小。在低温（低压）下合成氨，宜采用较低的H2／N2。