微波有機合成反應器之研究

Study of an Organic Synthesis Microwave Reactor

蔡芳宜(Fang-Yi Tsai)

指導教授 ： 寇崇善

國立清華大學/理學院/物理學系/碩士(2013年)

https://doi.org/10.6843/NTHU.2013.00550

摘要

近年來有機合成專用的微波反應器已大量的在學術界和工業界蓬勃的發展，尤其是在合成化學和製藥產業。本實驗自行開發微波有機合成反應器，利用溫度控制加熱有機合成反應。其架構主要分成微波系統(微波加熱腔、磁控管和微波電源供應器)、溫度量測系統、溫度控制系統和介面、壓力閥。主要利用脈衝寬度調變(PWM，Pulse Width Modulation)送入微波電源供應器調控微波的輸出功率。輸入脈衝的工作週期(Duty Cycle)越大，微波輸出的能量越大。本反應器使用熱電偶堆紅外線式感測器(Thermopile sensor)設計類比的溫度量測系統量測反應物的溫度。將初始反應物溫度和預設的化學反應溫度轉為電壓訊號後，利用溫度控制系統讓整個反應過程中的溫度差距變化調變PWM以回饋控制微波輸出的能量，使加熱化學反應，達到溫度控制的效果。
最後實際以有機合成化學反應Knoevenagel condensation和Suzuki reaction做測試，實驗結果發現和使用商用微波有機合成反應器的效果相當。

關鍵字

微波有機合成反應器

並列摘要

Recently there has been a great development of microwave-assisted organic synthesis(MAOS) for use in pharmaceutical industry or synthesis chemistry. In this report it is described how an organic synthesis microwave reactor which uses a temperature control system to heat up organic chemical synthesis reactions was designed and built. The microwave reactor is composed of microwave heating cavity, magnetron, inverter power supply, temperature control system and interface, and pressure valve. The operating principle is inputting PWM (Pulse Width Modulation) signal into the inverter power supply to modulate the output power of microwave. The bigger the duty cycle of input pulse, the stronger the output power of microwave is. The microwave reactor utilizes a thermopile sensor as an analog temperature measurement system to measure the temperature of the reactant. By transforming both the temperature signal of initial reactant and default chemical reaction to voltage signal, the temperature control system use the temperature variation to modulate PWM signal and then feedback control the output power of microwave. This mechanism then heat up the chemical reaction and enable control of the temperature of the chemical reaction.

Finally, two chemical synthesis reactions was used, Knoevenagel condensation and Suzuki reaction, to verify the effect of the microwave reactor. The results of the experiments show that the built microwave reactor has very similar result as commercial microwave reactors.

參考文獻

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