大学化学 >> 2019, Vol. 34 >> Issue (6): 46-52.doi: 10.3866/PKU.DXHX201810023

化学实验 上一篇    下一篇

综合化学实验中空气敏感合成实验的选取和教学

赵晓霞,白银娟,刘晶晶,程河聪,谢钢*()   

  • 收稿日期:2018-10-23 发布日期:2018-12-28
  • 通讯作者: 谢钢 E-mail:xiegang@nwu.edu.cn
  • 基金资助:
    陕西省高校“一流专业”建设项目;国家自然科学基金(21371141);国家自然科学基金(21727805);陕西省自然科学基金(14JS091);陕西省自然科学基金(15JS114)

Selection and Teaching of Synthetic Experiments with Air-Sensitive Substances in Comprehensive Chemical Experiment

Xiaoxia ZHAO,Yinjuan BAI,Jingjing LIU,Hecong CHENG,Gang XIE*()   

  • Received:2018-10-23 Published:2018-12-28
  • Contact: Gang XIE E-mail:xiegang@nwu.edu.cn
  • Supported by:
    陕西省高校“一流专业”建设项目;国家自然科学基金(21371141);国家自然科学基金(21727805);陕西省自然科学基金(14JS091);陕西省自然科学基金(15JS114)

摘要:

选择“硅基芳胺的合成与表征”作为综合化学实验“无水无氧合成技术”的教学内容,实验涉及特殊用途玻璃仪器的干燥与组装、空气敏感物质的操作、惰性气体保护下的化学反应、溶剂浓缩、萃取、少量液体的减压蒸馏以及结构测定等操作。深入分析了无水无氧反应装置的准备、溶剂和物料的转移、正丁基锂的取用、双排管和施伦克玻璃仪器的使用等操作细节问题,并对产物的核磁共振氢谱进行了解析。通过该实验,学生能够实践较高层次的化学实验操作,对拓宽学生专业知识面、提高学生综合实验操作技能有良好的教学效果。

关键词: 正丁基锂, 硅基芳胺, 无水无氧合成技术, 综合化学实验

Abstract:

"Synthesis and characterization of an aryl silylamine" was selected as the teaching content of "Schlenk line technique", which involves drying and assembly of glass instruments for special purposes, operation of air sensitive substances, reactions under inert gas protection, solvent concentration, extraction, distillation under reduced pressure, and molecular structure determination. In this article, the following experimental operations were discussed in detail, including the preparation of experimental devices, the transfer of solvents and reactants, a special method of transferring n-butyllithium, operations of Schlenk line, Schlenk flasks and water-free solvent flasks. The hydrogen spectra of nuclear magnetic resonance (NMR) of the aryl silylamine were analyzed. This experiment enables students to practice the experimental operations at the higher levels. This could have a good teaching effect, in broadening students' professional knowledge and improving their operating skills in comprehensive chemical experiment.

Key words: n-Butyllithium, Aryl silylamine, Schlenk line technique, Comprehensive chemical experiment

MSC2000: 

  • G64