大学化学 >> 2025, Vol. 40 >> Issue (3): 333-341.doi: 10.12461/PKU.DXHX202405177

化学实验 上一篇    下一篇

基于“逆向-逐级优化法”改进经典有机合成实验——以乙酸乙酯合成为例

于娇娇1,2, 孙博3, 李娜2, 文聪2, 李薇1   

  1. 1 兰州石化职业技术大学石油化学工程学院, 兰州 730060;
    2 北京大学化学与分子工程学院, 北京 100871;
    3 中核四零四剂量防护车间, 甘肃 嘉峪关 735100
  • 收稿日期:2024-05-27 录用日期:2024-08-22 发布日期:2025-03-19
  • 通讯作者: 李娜 E-mail:lina@pku.edu.cn
  • 基金资助:
    甘肃省教育科学“十四五”规划2022年度课题(GS[2022]GHB1796)

Improvement of Classical Organic Experiment Based on the “Reverse-Step Optimization Method”: Taking Synthesis of Ethyl Acetate as an Example

Jiaojiao Yu1,2, Bo Sun3, Na Li2, Cong Wen2, Wei Li1   

  1. 1 College of Petrochemical Engineering, Lanzhou Petrochemical University of Vocational Technology, Lanzhou 730060, China;
    2 College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China;
    3 Dose Protection Workshop, CNNC 404, Jiayuguan 735100, Gansu Province, China
  • Received:2024-05-27 Accepted:2024-08-22 Published:2025-03-19
  • Contact: Na Li E-mail:lina@pku.edu.cn

PDF

365

赞

摘要： 经典有机合成教学实验中，学生实验的产率通常不高，且结果不稳定。通过实验，学生通常只能了解到实验原理、实验流程和实验注意事项，对如何提高合成产品的产率和纯度缺乏深层次的探讨。为此，我们提出了高效实用的“逆向-逐级优化法”。本文以乙酸乙酯合成实验为例，采用色谱内标法分析产品的纯度和产率，将乙酸乙酯合成实验分解为反应蒸馏、洗涤干燥和产品蒸馏三个实验阶段，并按照从后向前的方式，对各阶段影响纯度和产率的主要因素进行优化。经过优化后，乙酸乙酯合成实验主要的影响因素和最优条件得以确定，不同学生在不同地区进行实验，均能保证产品纯度稳定在96%–99%之间，产率稳定在72%–75%之间。在经典有机实验中融入“逆向-逐级优化法”，不仅能帮助学生夯实基础，增强对基本操作技能的掌握和对理论知识的理解，还能培养学生的科研思维和解决问题的能力，从而让经典实验焕发新的活力。

关键词: 逆向-逐级优化法, 经典有机实验, 学生培养

Abstract: In classical organic synthesis laboratory teaching experiment, students usually cannot achieve an expected yield and the variation of yield is often big. Students can usually understand the experimental principles, experimental procedures and experimental precautions, but there is a lack of in-depth discussion on how to improve the yield and purity of synthetic products. We propose an efficient “reverse-step optimization method”. The ethyl acetate synthesis experiment is first divided into three experimental stages, including reaction distillation, washing and drying, and product distillation. Then, the main influencing factors of each stage are optimized in a reverse manner by using internal standard chromatography to analyze the purity and yield of the product. After improvement, the product purity and yield remain stable with the former between 96% and 99%, and the latter between 72% and 75%. Integrating the “reverse-step optimization method” into the classic experiment helps to consolidate the foundation, strengthen students’ mastery of basic operation skills and understanding of theoretical knowledge, and also helps to cultivate students’ scientific research thinking, thereby revitalizing the classic experiment.

Key words: Reverse-step optimization method, Classical organic experiment, Student training