环丙基砜衍生物的合成研究

在温和的碱性条件下,以TosMIC为砜源,对2-酰基-1-氯环丙烷羧酸酯的区域进行选择性加成,直接合成具有潜在生物活性的环丙基砜类化合物,产率可高达85％,非对映选择性可超过20:1.研究结果首次证明了TosMIC与缺电子环丙烯的亲核加成反应.     

涡流检测技术在宝钢热轧轧辊上的应用

介绍了轧辊涡流检测仪的工作要求、设备组成和使用方法,指出对轧辊进行涡流检测可防止爆辊,减少轧辊磨削量。     

浅谈化工建设项目竣工预验收程序和内容

结合作者的实际工作 ,总结了对工程建设实施“三道质量控制工序”的经验 ,强调了过程质量控制的重要性 ,较为系统地介绍了化工建设项目预验收工作的程序和内容     

高沸点溶剂法合成原乙酸三甲酯

对低沸点溶剂法制备原乙酸三甲酯工艺进行了改进，比较了煤油、2-乙基己醇、氯苯、异佛尔酮、邻苯二甲酸二丁酯、乙二醇二丁醚等高沸点溶剂对反应的影响，筛选出最优高沸点溶剂煤油：研究了新反应体系的醇解pH值、溶剂的循环使用次数对反应的影响及溶剂循环损耗率，结果表明，醇解的最佳pH值为5．6；随着溶剂循环次数增加，原乙酸三甲酯收率从83．6％(1次)逐渐下降到76．7％(16次)；溶剂次平均损耗率4．6％。实现了直接蒸馏产品，溶剂循环使用的新工艺。避免了旧工艺先蒸溶剂，后蒸产品，产品大量分解，收率低等缺点。     

2,6-二乙酰基吡啶合成方法的改进

优化了2，6—二乙酰基吡啶的合成工艺。以2，6—吡啶二羧酸为原料，经过醇化及克莱森酯缩合反应，合成了2，6—二乙酰基吡啶，2，6—吡啶二羧酸二乙醇和2，6—二乙酰基吡啶的分离收率分别为94．1％和88．9％，2，6—二乙酰基毗啶的质量分数大于99％。     

A spectroscopic study of the self-association and inter-molecular aggregation behaviour of pH-responsive poly(l-lysine iso-phthalamide)

The pH mediated intra-molecular association and inter-molecular aggregation of a range of amphiphilic poly(l-lysine iso-phthalamide) polymers have been investigated in aqueous solution over a range of pH values and concentrations. The desired functionality of these novel bioresponsive amphiphilic polymers was achieved by incorporating pendant hydrophilic carboxyl groups along the polymer backbone, via the l-lysine moiety, balanced by a degree of hydrophobicity introduced via the iso-phthaloyl moiety. Incorporation of low levels of bis-functional Cy3 (poly-Cy3) and/or Cy5 dye (poly-Cy3/5 or poly-Cy5) co-monomers in the responsive polymer backbone allowed detailed probing of the pH mediated hydrophobic association using a combination of optical spectroscopic techniques. Both steady-state fluorescence spectroscopy and fluorescence lifetime measurements of poly-Cy3 revealed a conformational transition at pH 4.5. Thus, below a critical pH the polymer collapsed into a compact globular structure (hypercoil) bringing the fluorophore molecules into close proximity with one another. This resulted in a dramatic reduction in fluorescence intensity and fluorescent lifetime in the single fluorophore systems (poly-Cy3) accompanied by a red shift in the maximum emission wavelength. Observed redshifts in the emission maxima and enhancements of fluorescent lifetimes with increasing polymer concentration suggested the formation of polymer aggregates. Fluorescence resonance energy transfer (FRET) was measured in mixtures of single fluorophore containing poly-Cy3 (donor) and poly-Cy5 (acceptor) and dual fluorophore containing poly-Cy3 (donor)/Cy5 (acceptor) in an effort to distinguish between intra-molecular versus inter-molecular association. The relevance of the results with respect to potential in vivo applications (drug delivery and biodiagnostics) is discussed.     

Catalytic activities and properties of mesoporous sulfated Al2O3–ZrO2

Mesoporous sulfated Al₂O₃–ZrO₂ (MSAZ) catalysts with large surface areas and pore volumes after calcination at high temperature (650 °C) and with higher Al₂O₃ content than 20wt% were successfully prepared from a template of block copolymer (P84). The MSAZ catalysts were characterized by X-ray diffraction (XRD), N₂ adsorption, transmission electron microscopy (TEM), ²⁷Al magic-angle spinning nuclear magnetic resonance (MAS NMR), thermogravimetric analysis (TG–DTG), temperature-programmed desorption of ammonia (NH₃-TPD) and infrared spectra (IR) of adsorbed pyridine. It is shown that the resulting mesostructured sulfated Al₂O₃–ZrO₂ samples have a well-developed textural mesoporosity. The number of acid sites present on MSAZ catalysts is higher than that on conventional sulfated zirconia, and the former catalysts are more active than the latter one for various acid-catalyzed reactions.     

半刚性钢-混凝土组合节点受弯承载力的计算

在半刚性钢 -混凝土组合框架中 ,混凝土板中的纵向钢筋增加了节点的强度和刚度 ,但是 ,传统的设计方法往往忽略纵向钢筋的作用而采用简化的计算模型。因此 ,出于经济效益考虑 ,应该根据半刚性组合节点的实际受力性能建立更加准确的计算方法。这里详细介绍了考虑混凝土板纵向钢筋作用的半刚性组合节点受弯承载力的计算方法 ,计算结果表明 ,建议的公式与试验结果吻合良好 ,可供规范制定和工程应用参考。     

高柔韧性聚氨酯丙烯酸酯的合成及应用

选用不同结构的多元醇作骨架，合成一系列高性能的聚氨酯丙烯酸树脂，并通过对聚氨酯丙烯酸树脂性能的对比研究，发现以聚丁二烯二元醇为骨架的聚氨酯丙烯酸酯树脂具有极佳的柔韧性和优异的低温耐曲折性。     

溴虫腈土壤和甘蓝微量残留量的气相色谱法测定

采用气相色谱法定量分析溴虫腈土壤和甘蓝微量残留量。样品经丙酮提取 ,液 液分配及氧化铝柱层析法净化后 ,以GC ECD测定 ,DB 170 1毛细管柱 ,氮气为载气 ,柱温 2 6 0℃ ,汽化室温度 2 5 0℃ ,检测器温度 2 80℃ ,外标法定量。该方法快速、准确 ,在 0 0 1～ 2 0 0mg/L范围内线性相关系数r2 =0 9999,平均回收率 90 0 %～ 10 3 6 7% ,变异系数 4 4 8%～ 5 89% ,最小检测量 2× 10 12 g ,最低检出浓度 3 3× 10 4mg/kg。