Study on microscale chemical expenments for reduction of experiment wastes

减少实验废物的微型化学实验研究

• 批准号: 12680563
• 负责人: OWARI Masanori
• 金额: $ 2.3万
• 依托单位: The University of Tokyo
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 2000
• 资助国家: 日本
• 起止时间: 2000 至 2001
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-12680563/
• 关键词: experiment wastes; microlaboratofy; miniaturized chemical experiment; educationalexperiments; laboratory experiments; Friedel-Crafts acylation; acetylation; organic chemical synthesis; マイクロラポラトリ; 微小規模化学実験; グルコース

This project aimed at development of general purpose miniaturized chemical experiment apparatus system in order to reduce amounts of experiment wastes produced by chemical experiments. Most of the chemical experiments are planned to yield sufficient information, not to yield amount of product material. Therefore, as far as keeping the quality of information obtained from an experiment, amount of material used in the experiment can be reduced.In the first year of this project, downsizing of educational experiments adopted in the specialized course in the chemistry departments in a university. As a model experiment, the Friedel-Crafts acylation of toluene was adopted because this experiment includes several procedures applicable to general organic synthesis reaction, such as refluxing, liquid-liquid extraction, washing, drying, distillation and filtration. By using the smallest commercial apparatus, 1/6-scale experiment was examined. From the results of this examination the following points was understood : Production yield of object material was not degraded within a scale of 1/10 ; Handling easiness was not lost in such scale ; 1/10 was the practical limit of downsizing when commercial apparatus were used.In the second (final) year of this project, original apparatus were designed and manufactured in order to realize 1/25-scale downsizing. The model experiment adopted here was acetylation of glucose hydroxy-groups by acetic acid unhydrate, which is frequently executed in organic synthesis laboratories. This reaction includes dissolving, nitrogen purge, several-hour reaction in water bath, washing-extraction, drying and filtration.Production yield of 72% which is comparable to 76% in full-scale experiment was achieved by using newly designed apparatus, while amount of experiment wastes was reduced down to 1/25 of conventional experiment.

本项目旨在开发通用的小型化化学实验仪器系统，以减少化学实验产生的实验废物。大多数化学实验都是为了获得足够的信息，而不是为了获得大量的产品材料。因此，只要保持从实验中获得的信息的质量，在实验中使用的材料的量可以减少。本项目的第一年，在一所大学的化学系的专业课程中采用了缩小教育实验。采用甲苯的Friedel-Crafts酰化反应作为模型实验，因为该实验包括了几个适用于一般有机合成反应的步骤，如搅拌、液-液萃取、洗涤、干燥、蒸馏和过滤。用最小的商业装置，1/6规模的实验进行了检查。从该检查的结果中了解到以下几点：目标材料的产率在1/10的规模内没有降低; 1/10是使用商业仪器时缩小尺寸的实际极限。在该项目的第二年（最后一年），为了实现1/25规模的小型化，设计并制造了原始装置。这里采用的模型实验是葡萄糖羟基通过乙酸的乙酰化，这是经常在有机合成实验室进行。该反应包括溶解、氮气吹扫、水浴反应、洗涤萃取、干燥、过滤等步骤，采用新设计的实验装置，产品收率达到72%，与工业实验的76%相当，而实验废液量仅为常规实验的1/25。

项目成果

B. Kim, Y Tojo, J. Niu, M. Matsubara, T Sakamoto, M. Owari: "The Study on Miniaturizing the Scale of Chemical Experiments in a University"Joumal of Chemical Education. In press.

B. Kim、Y Tojo、J. Niu、M. Matsubara、T Sakamoto、M. Owari：“大学化学实验规模小型化的研究”化学教育杂志。

B.Kim, Y.Tojo, J.Niu, M.Matsubara, T.Sakamoto, M.Owari: "The Study on Miniaturizing the Scale of Chemical Experiments in a University"Journal of Chemical Education. (in press).

B.Kim、Y.Tojo、J.Niu、M.Matsubara、T.Sakamoto、M.Owari：“大学化学实验规模小型化的研究”化学教育杂志。

B.Kim, Y.Tojo, J.Niu, M. Matsubara, T.Sakamoto, M.Owari: "The study on Miniaturizing the Scale of Chemical Experiments in a University"Journal of Chemical Education. (In press).

B.Kim，Y.Tojo，J.Niu，M.Matsubara，T.Sakamoto，M.Owari：“大学化学实验规模小型化的研究”化学教育杂志。