Mattia Annatelli, Giacomo Trapasso, Lucrezia Lena, F. Aricò
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引用次数: 3
摘要
市购Purolite CT151是糠醛醇醇解合成乙酰丙酸烷基酯的高效酸催化剂,反应温度较低(80-120℃),反应时间较短(5 h)。首先优化了乙酰丙酸乙酯的合成条件,然后测试了甲基-、丙基-、异丙基-、丁基、中丁基-和乙酰丙酸烯丙酯的制备条件。对大多数乙酰丙酸烷基酯(从5.0 g FA开始)进行了初步的放大试验,所得产品通过蒸馏分离为纯产品,收率很高(高达63%)。此外,对制备乙酰丙酸乙酯的回收实验表明,Purolite CT151和多余的乙醇都可以连续四次回收再利用,而催化剂活性没有明显损失。
Alkyl Levulinates from Furfuryl Alcohol Using CT151 Purolite as Heterogenous Catalyst: Optimization, Purification, and Recycling
Commercially available Purolite CT151 demonstrated to be an efficient acid catalyst for the synthesis of alkyl levulinates via alcoholysis of furfuryl alcohol (FA) at mild temperatures (80–120 °C) and short reaction time (5 h). Reaction conditions were first optimized for the synthesis of ethyl levulinate and then tested for the preparation of methyl-, propyl-, isopropyl-, butyl, sec-butyl- and allyl levulinate. Preliminary scale-up tests were carried out for most of the alkyl levulinates (starting from 5.0 g of FA) and the resulting products were isolated as pure by distillation in good yields (up to 63%). Furthermore, recycling experiments, conducted for the preparation of ethyl levulinate, showed that both the Purolite CT151 and the exceeding ethanol can be recovered and reused for four consecutive runs without any noticeable loss in the catalyst activity.