微波辐射下活化天然沸石催化合成三乙酸酯

Dzikri Hamzah, T. Rinaldi, M. Marwan, W. Rinaldi
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引用次数: 1

摘要

研究了在活性天然沸石存在下,微波辐射下甘油与乙酸的酯化反应。从Ujung Pancu(Aceh Besar)收集天然沸石,并用盐酸进行化学活化。反应在置于微波炉内的搅拌玻璃烧瓶反应器中进行。实验变量包括微波传输时间、甘油与乙酸的摩尔比和催化剂负载量。活化沸石的XRD图谱显示,Si/Al比增加到6.042,结晶度略有下降12.23%,主要是由于化学处理过程中的脱铝。FTIR定性分析表明,微波加热得到的反应产物在1706.669cm-1波长下含有酯基(三乙酸甘油酯),而酸碱滴定定量分析表明,在摩尔比为1:9、催化剂负载量为3%、微波透射时间为10分钟的反应条件下,甘油转化率最高,为93.033%。本工作表明,微波可以作为甘油酯化制三乙酸甘油酯的有效加热技术。
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Synthesis of Triacetin Catalyzed by Activated Natural Zeolite Under Microwave Irradiation
Esterification of glycerol with acetic acid under microwave irradiation in the presence of activated natural zeolite was investigated. Natural zeolite was collected from Ujung Pancu (Aceh Besar) and chemically activated with hydrochloric acid. The reaction was carried out in a stirred glass flask reactor placed inside microwave oven. Experimental variables include microwave transmission time, molar ratio of glycerol to acetic acid, and catalyst loading. XRD profile of activated zeolite showed an increase of Si/Al ratio to 6.042 and the crystallinity decreased slightly by 12.23%, mainly due to dealumination during chemical treatment. Qualitative analysis by FTIR shows that the reaction product obtained by microwave heating contains ester group (triacetin) at wavelength 1706.669 cm-1, while the quantitative analysis by acidi-alkalimetry titration indicates the highest glycerol conversion of 93.033% at the reaction condition of the molar ratio of 1:9, catalyst loading of 3%, and microwave transmission of 10 minutes. The present work suggests that microwave can be utilized as efficient heating technique in esterification of glycerol to triacetin.
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