大学化学 >> 2023, Vol. 38 >> Issue (9): 172-178.doi: 10.3866/PKU.DXHX202210077

化学实验 上一篇    下一篇

基于连续流技术的三苯甲醇合成实验

张轩赫1, 蒋小武1, 胡恩铭1, 程景2, 杨雪苹2, 金剑2,*()   

  1. 1 哈尔滨工业大学(深圳)材料科学与工程学院, 广东 深圳 518055
    2 哈尔滨工业大学(深圳)实验与创新实践教育中心, 广东 深圳 518055
  • 收稿日期:2022-10-26 录用日期:2022-12-17 发布日期:2023-09-21
  • 通讯作者: 金剑 E-mail:jianjin@hit.edu.cn
  • 作者简介:第一联系人：

    †三位同学对本研究做出同等贡献，均为本科生

  • 基金资助:
    校级创新实验课(INEP1022)

Continuous-Flow Approach towards the Preparation of Triphenylmethanol

Xuanhe Zhang1, Xiaowu Jiang1, Enming Hu1, Jing Cheng2, Xueping Yang2, Jian Jin2,*()   

  1. 1 School of Materials Science and Engineering, Harbin Institute of Technology (Shenzhen), Shenzhen 518055, Guangdong Province, China
    2 Education Center of Experiments and Innovations, Harbin Institute of Technology (Shenzhen), Shenzhen 518055, Guangdong Province, China
  • Received:2022-10-26 Accepted:2022-12-17 Published:2023-09-21
  • Contact: Jian Jin E-mail:jianjin@hit.edu.cn

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摘要：

三苯甲醇的制备实验是化学相关专业的经典教学实验，是有机化学理论与实践操作重要的结合点。然而，实验装置复杂、格氏试剂引发较为困难、严苛的无水无氧操作等导致实验成功率较低；反复转移溶剂导致师生的溶剂暴露。基于上述问题，本文利用中压柱塞泵和固定床连续流反应器，设计并搭建了格氏试剂连续流动制备装置，实现了三苯甲醇的连续制备。基于连续流的格氏试剂制备装置设备搭建简单，全程避免了师生的有机溶剂暴露，溴苯-格氏试剂转化率重现性好。在本连续流装置内，格式试剂制备反应稳定可控，实验安全性高。过量镁屑无需淬灭，可重复使用。

关键词: 三苯甲醇的制备, 格氏试剂, 连续流动

Abstract:

The preparation of triphenylmethanol is a classic teaching experiment in the field of chemistry and serves as an important combination of organic chemistry theory and practical laboratory skills. However, the experiment has a low success rate due to the complexity of the apparatus, difficulties in handling Grignard reagents, and the strict requirements for anhydrous and oxygen-free conditions. Moreover, repeated solvent transfers result in solvent exposure for both teachers and students. In this study, we designed and constructed a continuous flow apparatus for the preparation of Grignard reagents using a medium-pressure syringe pump and a fixed-bed continuous flow reactor, achieving the continuous production of triphenylmethanol. The continuous flow apparatus for Grignard reagent preparation is simple to assemble, completely eliminates organic solvent exposure for teachers and students, and exhibits good reproducibility in the conversion of bromobenzene to Grignard reagent. Within this continuous flow setup, the preparation of Grignard reagents is stable, controllable, and safe. Excess magnesium turnings do not require quenching and can be reused.

Key words: Preparation of triphenylmethanol, Grignard reagent, Continuous flow