苯甲醇和苯甲酸制备工艺的改进与创新设计

大学化学 Pub Date : 2020-01-01 DOI:10.3866/pku.dxhx201912001

Xiaosai Quan, Xiuqin Men, Junqing Wang, Ying Zhou, Jun Yao

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引用次数: 0

摘要

以苯甲醛为原料，用Cannizarro反应制苯甲醇和苯甲酸是有机化学实验教学的常见内容。但由于该实验设计耗时长，产率低，分离方法效率低，在教学中效果不理想。对其进行了改进:引入微波辐射法，通过正交试验设计优化合成条件。优化条件为50% KOH, 500 W微波辐照15 min，反应完成。苯甲醇的收率可达82.0%。采用柱层析法分离苯甲醇，避免了蒸馏副产物的产生。采用不分离分光光度法快速、准确地测定了粗产品中苯甲醇的收率。结果表明，改进后的方法可使合成时间缩短99%，产量提高15%。此外，萃取剂的安全性更高。这一改进更符合实验室培训发展日益增长的要求。

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Improvement and Innovative Design on Preparation of Benzyl Alcohol and Benzoic Acid

: The preparation of benzyl alcohol and benzoic acid from benzaldehyde by Cannizarro reaction was the common content of organic chemistry laboratory teaching. Nevertheless, due to its time consuming, low yield and inefficient isolating method, this experimental design was far from satisfactory in teaching. The following improvements have been made: Microwave radiation method was introduced, and the synthesis conditions was optimized by orthogonal test design. Under optimized conditions which was 50% KOH, microwave radiation at 500 W for 15 min, the reaction was completed. The yield of benzyl alcohol could reach 82.0%. Benzyl alcohol was isolated by column chromatography instead of distillation, to avoid the formation of distillation by-products. The yield of benzyl alcohol in crude products was determined quickly and accurately by spectrophotometry without separation. The comparison showed that the improved method could reduce the time by 99% and increase the yield by 15%. In addition, the extraction agent was more safe. The improvement was more responsive to the increasing requirements of laboratory training development.

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来源期刊

大学化学

自引率

0.00%

发文量

5852

期刊介绍： University Chemistry is an educational research academic journal supervised by the Ministry of Education and co-sponsored by Peking University and the Chinese Chemical Society. It was founded in 1986 and changed to a monthly publication in January 2016. Its purpose is to promote and deepen the reform of university chemistry education and serve to improve the level of chemistry teaching in my country. The main columns are: Today's Chemistry, Teaching Research and Reform, Knowledge Introduction, Chemical Experiments, Teacher-Student Chats, Future Chemists, etc. The journal has been included in many databases such as China Journal Network Full-text Database, Wanfang Database, Taiwan Huayi Database, Chinese Science and Technology Journal Database (Full-text Edition), and American Chemical Abstracts.