摘要
微波加熱相較於一般加熱能更有效的使用能源並縮短反應時間，對於微波相關的研究也越來越多。本研究主要是藉由合成1-甲基-3-丙基氯化咪唑(PMIC)與1-甲基-3-丁基氯化咪唑(BMIC)探討微波室溫離子液體造成的效果，並放大至公斤級製程且將產率提升至90%以上。首先利用CEM Corporation研發的微波反應器Discover Microwave Synthesizer嘗試合成Small-Scale的BMIC 0.025 mole，總重4.56 g，輕物質鹵化烷採1.1過量反應，總反應時間30 min，在加熱區間使用Power to Time模式，功率為300 W，待溫度到達150°C時採用固定溫度模式加熱，最後使用HPLC分析，產率可達95.5%。接下來使用與物理所合作研發的Bio-diesel Microwave Reactor進行Large-scale公斤級研究，總莫耳數分別為5 mole與10 mole，總重為919.6 g與1839.2 g，在反應初期使用1500 W加熱，使溫度保持在150°C，加熱時間為150 min，產率可達96.9%與93.5%。在成功合成BMIC後，以同樣製程方法合成PMIC，Small-Scale產率可達94.7%，Large-scale 反應5 mole的產率為96.8%，10 mole產率則是92.1%。 從實驗結果可以發現:高壓系統下的反應效率高於常壓系統；於加熱初期微波能量使用效率最高，並隨著反應進行下降；計算Small-scale與Large-scale之EFF發現隨著反應總重增加數值減小，代表反應單位反應物所需能量下降，可以推斷微波對於Scale-up製程有顯著的優化效果。
並列摘要
Microwave heating have numerous advantages such as consume less energy than conventional heating and could reduce the reaction time. There are more and more researches on microwave heating. In this study, the effects of microwave synthesis of room temperature ionic liquids were investigated by synthesizing 1-methyl-3-propylimidazole chloride (PMIC) and 1-methyl-3-butylimidazole chloride (BMIC) Moreover, I’ll scale up to the kg-scale and increase the yield to over 90%. Selecting the Discover Microwave Synthesizer, a microwave reactor designed by CEM Corporation to synthesize small-scale BMIC 0.025 mole, with a total weight of 4.56 g, and a light substance with an excess ratio of 1.1. The total reaction time is 30 min. Power to Time mode is used in the heating zone. The power is 300 W, when the temperature reaches 150°C, it is changed to the Fixed Temp mode, and finally analyzed by HPLC. The yield can reach 95.5%. Next, the bio-diesel microwave reactor designed in collaboration with the Institute of Physics was used to manufacture large-scale ionic liquid. The total moles were 5 mole and 10 mole, and the total weight was 919.6 g and 1839.2 g. At the beginning of the reaction, 1500 W heating was set and kept the temperature at 150 °C, reaction time is 150 min. The yield can reach 96.9% and 93.5%. After successfully synthesizing BMIC, PMIC was synthesized by the same process but the reaction temperature decreased from 150°C to 120°C. The small-scale yield was up to 94.7%. The yield of large-scale reaction 5 mole at 96.8% and 10 mole yields at 92.1%. According to the results, it can be found that the reaction efficiency under the high-pressure system is higher than the normal pressure system; the microwave energy efficiency is highest at the initial stage of heating, and decreases as the reaction proceeds; calculating the EFF of different scales found that with the total weight of the reaction increase in the value decreases, which means that the microwave energy required per unit of reactant decreases. It can be concluded that microwave has a significant optimization effect on the scale-up process.
參考文獻
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