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用插层了[Bmim]OH的废钢渣合成水滑石用于碳酸甘油酯的酯交换反应

Synthesis of Hydrotalcites from Waste Steel Slag with [Bmim]OH Intercalated for the Transesterification of Glycerol Carbonate.

作者信息

Liu Guanhao, Yang Jingyi, Xu Xinru

机构信息

International Joint Research Center of Green Energy Chemical Engineering, East China University of Science and Technology, Meilong Road 130, Shanghai 200237, China.

出版信息

Molecules. 2020 Sep 23;25(19):4355. doi: 10.3390/molecules25194355.

Abstract

Ca-Mg-Al hydrotalcites were prepared by coprecipitation from Type S95 steel slag of Shanghai Baosteel Group as supports of ionic liquid in this paper. Five basic ionic liquids [Bmim][CHCOO], [Bmim][HCOO], [Bmim]OH, [Bmim]Br and ChOH were prepared and their catalytic performance on the synthesis of glycerol carbonate by transesterification between dimethyl carbonate and glycerol was investigated. The characterization results indicated that [Bmim]OH is the best ionic liquid (IL) for the transesterification reaction of glycerol carbonate. The hydrotalcites before and after intercalation by ionic liquid were characterized by XRD, FTIR, SEM, EDS and the IL were characterized by FT-IR, C-NMR and basicity determination via the Hammett method. The analysis results implied that the dispersion of [Bmim]OH in hydrotalcites reduced the alkali density appropriately and facilitated the generation of glycerol carbonate. The yield of glycerol carbonate and the conversion rate of glycerol reached 95.0% and 96.1%, respectively, when the molar ratio of dimethyl carbonate and glycerol was 3:1, the catalyst dosage was 3 wt%, the reaction temperature was 75 °C and the reaction time was 120 min. The layered structure of hydrotalcites increased the stability of ionic liquid intercalated in carriers, thus the glycerol conversion and the GC yield still remained 91.9% and 90.5% in the fifth reaction cycle.

摘要

本文以上海宝钢集团的S95型钢渣为原料,通过共沉淀法制备了钙镁铝水滑石,作为离子液体的载体。制备了5种碱性离子液体[Bmim][CHCOO]、[Bmim][HCOO]、[Bmim]OH、[Bmim]Br和ChOH,并研究了它们在碳酸二甲酯与甘油酯交换合成碳酸甘油酯反应中的催化性能。表征结果表明,[Bmim]OH是碳酸甘油酯酯交换反应的最佳离子液体(IL)。采用XRD、FTIR、SEM、EDS对离子液体插层前后的水滑石进行了表征,采用FT-IR、C-NMR和Hammett法测定碱度对离子液体进行了表征。分析结果表明,[Bmim]OH在水滑石中的分散适当降低了碱密度,促进了碳酸甘油酯的生成。当碳酸二甲酯与甘油的摩尔比为3:1、催化剂用量为3 wt%、反应温度为75℃、反应时间为120 min时,碳酸甘油酯的产率和甘油的转化率分别达到95.0%和96.1%。水滑石的层状结构提高了插层在载体中的离子液体的稳定性,因此在第五次反应循环中甘油转化率和碳酸甘油酯产率仍分别保持在91.9%和90.5%。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/7d51/7582532/d34b3aafc69d/molecules-25-04355-g001.jpg

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