郑修成, 李宁, 陈耀, 关新新, 刘蒲. 磺化MCM-41介孔固体酸的合成、表征及其催化乙酰丙酸乙酯化性能[J]. 信阳师范学院学报(自然科学版), 2018, 31(1): 73-77. DOI: 10.3969/j.issn.1003-0972.2018.01.014
引用本文: 郑修成, 李宁, 陈耀, 关新新, 刘蒲. 磺化MCM-41介孔固体酸的合成、表征及其催化乙酰丙酸乙酯化性能[J]. 信阳师范学院学报(自然科学版), 2018, 31(1): 73-77. DOI: 10.3969/j.issn.1003-0972.2018.01.014
ZHENG Xiucheng, LI Ning, CHEN Yao, GUAN Xinxin, LIU Pu. Synthesis,Characterization and Catalytic Performance of Sulfonated MCM-41 Mesoporous Solid Acid for Levulinic Acid Esterification with Ethanol[J]. Journal of Xinyang Normal University (Natural Science Edition), 2018, 31(1): 73-77. DOI: 10.3969/j.issn.1003-0972.2018.01.014
Citation: ZHENG Xiucheng, LI Ning, CHEN Yao, GUAN Xinxin, LIU Pu. Synthesis,Characterization and Catalytic Performance of Sulfonated MCM-41 Mesoporous Solid Acid for Levulinic Acid Esterification with Ethanol[J]. Journal of Xinyang Normal University (Natural Science Edition), 2018, 31(1): 73-77. DOI: 10.3969/j.issn.1003-0972.2018.01.014

磺化MCM-41介孔固体酸的合成、表征及其催化乙酰丙酸乙酯化性能

Synthesis,Characterization and Catalytic Performance of Sulfonated MCM-41 Mesoporous Solid Acid for Levulinic Acid Esterification with Ethanol

  • 摘要: 以硅酸乙酯为硅源、十六烷基溴化铵为模板剂,室温常压下便捷地合成了MCM-41介孔分子筛,进而以硫酸为磺化剂,不同水热条件下制得系列磺化介孔固体酸MCM-41-SO3H.利用TG、XRD、FT-IR、TEM-EDX等手段对所得材料进行了表征.采用碱滴定法测定其酸密度,并且以乙酰丙酸乙酯化反应为探针反应,评价其催化性能.结果表明,尽管水热磺化处理在一定程度上降低了MCM-41的介孔规整性,所制备的MCM-41-SO3H介孔固体酸仍较好地保持了MCM-41的介孔结构;水热时间和温度影响其酸密度,进而影响催化活性,其中磺化温度180℃、磺化时间21 h制得的催化剂活性最高,乙酰丙酸转化率达到74.4%,并显示出较好的循环稳定性能.

     

    Abstract: Mesoporous molecular sieves MCM-41 was facilely synthesized at room temperature under normal pressure. Then,it was used to hydrothermally prepare a series of sulfonated MCM-41 mesoporous solid acids with sulfuric acid as sulfonating agent.The samples were characterized by TG,XRD,FT-IR,and TEM-EDX. The acid density was measured by base titration. Furthermore,their catalytic properties were evaluated with the synthesis of ethyl levulinate as a probe reaction. The results showed that the resulting MCM-41-SO3H catalysts maintained the mesoporous structure of MCM-41,although the hydrothermal process reduced the mesoporous regularity to a certain extent. Meanwhile,the hydrothermal time and temperature affected their acid density,which in turn affected the catalytic activity. The catalyst hydrothermally prepared at 180℃ for 21 h exhibited the highest catalytic activity,and the corresponding conversion of levulinic acid as high as 74.4%. In addition,the resulting mesoporous solid acid also displayed satisfactory cyclic stability.

     

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