相转移催化合成桂氮酮的动力学

动力学研究表明,以三乙基苄基氯化铵作为固-液相转移催化剂,在甲苯液中有粉状氢氧化钾存在下,己内酰胺的N-正十二烷基化生成桂氮酮为准一级反应,表观速度常数k_(80)=3.39×10~(-3)min~(-1)、k_(100)=4.65×10~(-3)min~(-1)。实验显示,反应温度为80℃及100℃时,反应可于4.5 h及3.5 h完成,转化率分别为74%及67%,实际产率为71%及64%;反应的选择性良好,副反应较少。本文还报道了水分对反应的影响。用动力学方法研究合成反应过程,对指导合成工艺具有普遍意义。     

小花棘豆化学成分分离鉴定

目的：考察小花棘豆（OxytropisglabraDC．）的化学成分。方法：小花棘豆乙醇提取物反复采用硅胶、聚酰胺、SpehadexLH-20柱色谱等多种方法进行分离纯化,利用理化性质及波谱学方法进行鉴定结构。结果：从该药材中分离得到4个化舍物,分别鉴定为己内酰胺（caprolactam,1）,槲皮素-3-O-芸香糖苷（quercetin一3-O-β-D-rutinoside,2）,芹菜素-7-0-新橙皮糖苷（apigenin-7-O-neohesperidoside,3）,山奈酚-3-0-β—D-葡萄糖-7-0-β-D-葡萄糖苷（kaempeferol-3-O-β-D-glucopyranoside-7-0-β-D-glucopyranoside,4）。结论：化合物1、2、3为首次从该植物中得到,其中化合物1同时也是从该属中首次得到。     

NOC的合成方法研究

本文报道用均匀设计方法以正辛醇、氢溴酸、浓硫酸为原料合成正溴辛烷，收率为９１％；以正溴辛烷和己内酰胺，在ＫＯＨ、ＰＴＣ存在下，以甲苯作溶剂，合成１－正辛基氮杂环庚烷－２－酮，收率为９３．２％。反应条件较文献报道的温和，且收率很高。     

Exposure study to examine chemosensory effects of ɛ-caprolactam in healthy men and women

Context: ε-Caprolactam is an important industrial chemical with a relatively low human toxicity; of importance is the irritations that occur after exposure to ε-caprolactam as aerosols or vapors.

Objective: The aim of this study was to examine symptoms and objective effects, which occur on the mucous membranes of the eyes and the upper respiratory tract.

Methods: A total of 52 healthy volunteers (26 women and 26 men, aged between 19 and 50 years) were exposed by random to different ε-caprolactam concentrations (0.05, 0.5 and 5.0?mg/m³) and the control condition (0.0?mg/m³) for 6?h on four consecutive days. Eye blinking frequency, tear film break-up time, eye redness, nasal flows and resistance, olfactory function as well as total protein and interleukin-8 in nasal lavage fluid were determined daily before, during and after exposure. Questionnaires were used to record both subjective symptoms and personality factors.

Results: There were no significant specific effects on the subjective and objective endpoints examined. Statistical analysis yielded no evidence of concentration-response relationships. Evaluation of olfactory symptoms showed that the duration of the stay in the chamber and not the ε-caprolactam concentration was decisive for the perception of “impure air”. Personality factors had no significant influence on the reported symptoms.

Conclusions: Exposure to ε-caprolactam concentrations of 5.0?mg/m³ at maximum for 6?h did not cause chemosensory effects on the upper respiratory tract or eyes of healthy volunteers. Therefore, the concentration of 5.0?mg/m³ corresponds to the No Observed Adverse Effect Level (NOAEL).     

哈克流变仪上模拟ε—己内酰胺反应挤出的试验研究

高温条件下用哈克流变仪进行ε－己内酰胺聚合的模拟性试验，对尼龙６试样进行了常规性能测定；分析讨论了有关工艺参数对己内酰胺阴离子开环聚合的影响，获得了一些可供工程应用的参考数据，为进一步在双螺杆挤出机中进行尼龙６的反应挤出研究提供必要的依据。     

月桂氮堇酮中有关物质测定方法的改进

目的 改进月桂氮革酮中有关物质的测定方法.方法 采用气相色谱法,以甲醇为溶剂、Agilent DB-1毛细管柱(30m ×0.53 mm,3.0 μm)、程序升温、氢火焰离子化检测器进行测定.结果 所用色谱条件可使月桂氮革酮及其强降解杂质得到有效分离,专属性、重复性良好;杂质己内酰胺的检出限为0.13 μg·mL-1,线性方程为:Y=2.3511×103X-0.2742,10.78～269.5 μg·mL-1己内酰胺与峰面积的线性关系良好(r =0.9984).结论 改进后的方法操作简便,准确可靠,可有效地检测月桂氮革酮中的有关物质.