摘要
环己酮的合成是一个重要的有机化学教学实验。该文针对利用重铬酸钾替代重铬酸钠作为氧化剂制备环己酮的实验步骤进行了改进。重铬酸钾固体分两次直接加入环己醇的稀硫酸混合液,通过加热或冷却控制反应温度在55~60℃,氧化反应时间在25 min左右,环己酮收率较高。水蒸气蒸馏的馏出液直接用甲基叔丁基醚萃取,合并后的有机相更容易干燥,且易于与干燥剂分离。改进后的实验步骤重复性较好,收率稳定,可在兄弟院校中推广。
The preparation of cyclohexanone is one important organic chemistry teaching experiment.In this paper,we modified the experimental operation to prepare cyclohexanone using K_(2)Cr_(2)O_(7) instead of Na_(2)Cr_(3)O_(7)·2H_(2)O as oxidizing agent.The solids of K_(2)Cr_(2)O_(7) were directly added to the round flask with the mixture of cyclohexanol and diluted sulfuric acid in one/two/three portions,the reaction temperature is controlled between 55~60℃through heating or cooling,the reaction time is controlled in the range of 20~30 min,cyclohexanone can be obtained in good yields.The distillate from the simplified steam distillation can be extracted directedly using methyl tertiary-butyl ether(MTBE).The combined organic phase is easier to dry and easily separated from the drying agent.The modified experiment procedure has a good reproducibility and stable yield and can be promoted in other universities.
作者
郭超
袁琦
熊锐
艾树轩
朱思文
赵昕仪
夏蕾
吕彦莹
王龙胜
GUO Chao;YUAN Qi;XIONG Rui;AI Shuxuan;ZHU Siwen;ZHAO Xinyi;XIA Lei;LYU Yanying;WANG Longsheng(School of Material Science and Chemical Engineering,Hubei University of Technology,Wuhan 430068,China;School of Food and Biological Engineering,Hubei University of Technology,Wuhan 430068,China)
出处
《实验科学与技术》
2023年第2期117-121,共5页
Experiment Science and Technology
基金
湖北省科技厅项目(2014CFB600)
湖北工业大学博士启动金(4032401)
湖北工业大学教研项目(2017008)
绿色轻工材料湖北省重点实验室暨绿色轻质材料与加工湖北工业大学协同创新中心项目(201710A11,201907A09)。
关键词
环己酮
重铬酸钾
氧化
制备
cyclohexanone
potassium dichromate
oxidization
synthesis
