1-环丙基-7-氯-6-(1-哌嗪基)-4-氧-1,4-二氢-3-喹啉羧酸盐酸盐的熔化与离解性质研究

1－环丙基－7－氯－6－（1－哌嗪基）－4－氧－1，4－二氢－3－喹啉羧酸盐酸盐为环丙沙星合成中主要的杂质之一，研究其物化性质对于改善环丙沙星的结晶分离提纯具有重要意义。本文研究了1－环丙基－7－氯－6－（1－哌嗪基）－4－氧－1，4－二氢－3－喹啉羧酸盐酸盐的熔化，分解特性，溶解度与离子强度，温度和pH值的关系，并测定了该物质的离解常数，估算了该物质在水溶液中的活度积。     

新型缓蚀剂2-炔丙基巯基苯并咪唑的合成

对不锈钢缓蚀剂2-炔丙基巯基苯并咪唑的合成工艺进行了研究。先由邻苯二胺和二硫化碳合成2-巯基苯并咪唑，炔丙醇和三氯化磷合成3-氯丙炔；再由2-巯基苯并咪唑和3-氯丙炔在丙酮溶剂中合成2-炔丙基巯基苯并咪唑。对是否使用相转移催化剂进行了探讨，认为无相转移催化剂可使操作简便，适合于工业化生产。     

Characterization of multiwall carbon nanotubes and influence of surfactant in the nanocomposite processing

Carbon nanotubes prepared by a classical CVD method with a nickel catalyst have been characterized, then used as conducting anisometric objects dispersed into a polymeric matrix. In a first part, these nanotubes are structurally characterized before and after heat treatments (HTT=1500, 2000, 2500 °C). Diffusion Raman experiments and diamagnetic susceptibility experiments demonstrated their limited graphitized structures.Then, in a second step, a well defined processing way to prepare nanocomposites with a standard epoxy resin is presented. In particular, the use or not of a non-ionic surfactant (Tergitol) to disperse these nanotubes is analyzed. The influence of nanotube contents is examined on the bulk nanocomposite density, the glass transition temperature of the nanocomposites, and the d.c. electrical conductivity behavior. These results demonstrated that the interfacial properties are playing a fundamental role. On one hand, the glass transition temperature is increasing with the nanotube content, and on the other hand, the percolation threshold is found for a rather high critical volumic concentration. Finally, it is demonstrated that a pure geometrical model is not sufficient to explain these behaviors and that a wrapping effect of the organic matrix around the nanotubes has to be considered.     

Carbonaceous adsorbents from sewage sludge and their application in a combined activated sludge-powdered activated carbon (AS-PAC) treatment

In this study, waste biological sludge is converted to an adsorbent by chemical activation with sulphuric acid. The adsorbent obtained is then applied to the aerated vessel of an activated sludge process treating glucose and phenol to improve the quality of the treated effluent. The sludge-based carbonaceous adsorbent was found to be mesoporous in nature, with a good adsorption capacity for large molecular weight compounds and limited removal efficiency for smaller molecules such as phenol. The addition of carbon, either sludge-based or commercial, enhanced phenol removal from 58% to 98.7% and from 87% to 93% the organic matter removal as measured by the chemical oxygen demand (COD) when operated with feed concentrations of 100 mg phenol/l and 2500 mg COD/l. No differences were found between the activated sludge-activated carbon bench scale continuous reactors operating with either commercial or sludge-based adsorbents in spite of the higher adsorption capacity of the former. It is suggested that powdered adsorbent bioregeneration in the combined AS-PAC system may be impaired by the obstruction of pores due to bacterial growth, the effect being more important for the commercial activated carbon with a narrower pore size distribution.     

Selective oxidation of ammonia to nitrogen on transition metal containing mixed metal oxides

The selective catalytic oxidation of ammonia to nitrogen (NH₃-SCO) has been studied over hydrotalcite derived mixed metal oxides containing Cu, Co, Fe or Ni. XRD, BET, NH₃-TPD and TPR techniques were used for catalysts characterization. Results of NH₃-SCO were compared with those of selective catalytic reduction of NO with NH₃ (NO-SCR). Reaction mechanism was studied by temperature-programmed surface reaction (TPSR) and activity tests with a various contact time. Catalytic performance of the studied samples depends on both kind and loading of transition metals in the mixed metal oxide system. The Cu-containing samples have been found to be the most active catalysts of the NH₃-SCO process. Transition metal loading strongly influences distribution of ammonia oxidation products. The highest selectivity to N₂ was measured for the catalysts with the lowest transition metal content.     

3-氨基-4-氯苯甲酸十六酯的合成

以3-氨基-4-氯苯甲酸和正十六醇为原料，二甲苯为溶剂，对甲苯磺酸为催化剂酯化合成3-氨基-4-氯苯甲酸十六酯。采用傅里叶红外光谱（FTIR）、核磁共振光谱（NMR）的方法对产品的结构进行表征。考察了醇酸摩尔比、催化剂加量、反应物浓度对酯化率的影响。结果表明：醇酸摩尔比1.2:1，催化剂用量为总质量5%，反应物浓度65%，反应时间7 h，酯化率达96.20%，单程收率为73.91%。研究确立了产物提纯、提高单程收率和滤液去除催化剂后回收、重复使用的最佳系统工艺路线，单程收率提至78.90%，总收率为82.62%，产品的纯度高于使用标准。     

酸性气流脱除物STW-3#对NR硫化性能影响的研究

酸性气流脱除物是净化天然气、合成气、煤气时脱除的物质，STW-3#是由该物质制成的样品之一。就STW-3#对NR硫化性能的影响进行了研究。结果表明，STW-3#对NR有较好的硫化促进特性和一定的软化增塑作用；其用量3.0份以下时，硫化特性较差，3．0份以上时硫化特性较好，但超过4．0份时有粘辊和喷霜现象。它与促进剂M并用时，硫化特性与促进剂D相似。     

Role of La2O3 in Pd-Supported Catalysts for Methanol Decomposition

Systems of Pd supported on various La₂O₃-modified -Al₂O₃ and CeO₂–Al₂O₃ catalysts were tested for catalytic methanol decomposition and characterized by means of XRD, BET, TPR, H₂-chemisorption and CO–FTIR. The addition of lanthanum significantly improved the selectivity of CO and H₂ for all the catalysts but showed a different influence on the catalytic activity in two systems. Methanol conversion decreased on La₂O₃-modified Pd/-Al₂O₃ catalysts, in line with the reduction of Pd dispersion, while the addition of La₂O₃ improved the dispersion of Pd and reinforced Pd–CeO₂ interaction for La₂O₃-modified Pd/CeO₂–Al₂O₃ catalysts, which resulted in a high production rate of CO and H₂. Thus, a synergistic effect between CeO₂ and La₂O₃ was observed on -Al₂O₃-supported Pd catalyst for methanol decomposition.     

The effect of fibre-matrix interactions on structure and property changes during the fabrication of unidirectional carbon/carbon composites

This paper reports the systematic characterisation of changes in the structure and properties of a series of unidirectional carbon-carbon composites at key stages of processing. The composites were fabricated from PAN-based carbon fibres (surface treated and untreated) and two carbon matrix systems (graphitising and non-graphitising). The effects of matrix shrinkage, together with thermal expansion mismatch and interfacial bonding, established the composite structure and hence the composite properties. The morphology and interconnectivity of the shrinkage cracks, the strength and nature of the fibre-matrix interfacial interaction and the development of matrix texture were identified as key structural features. These features were characterised and their effect on subsequent processing stages (densification) and composite properties was determined.     

超重力反应结晶法纳米碳酸钙浆料及粉料的表面处理

研究了脂肪酸盐A、水溶性铁酸酯偶联剂B（B1)以及铁酸酯偶联剂C对新型超重力反应结晶法所得的纳米CaCO3浆料及粉料的湿法表面处理的配方与工艺，确定了A体系的最佳改性时间为30～40min、改性温度为40～50℃、改性剂用量(质量分数)为3%～5％；B(B1)体系搅拌强度必须很高，改性时间30～40min，改性温度80℃左右，改性剂用量(质量分数)3％～5％；C体系的最佳改性时间为30～40min，改性剂用量(质量分数)为3％～5％。同时，采用红外光谱对改性前后的纳米碳酸钙进行了表征，表明改性刑已连接至CaCO3表面。最后，用分散稳定模型简要分析了改性机理。