磺酸化手性向列型介孔二氧化硅的制备及其催化合成龙脑

doi:10.11944/j.issn.1000-0518.2020.12.200097

摘要/Abstract

摘要： 通过溶胶凝胶法制备了手性向列型介孔二氧化硅(CNMS)和用浸渍法制备了磺酸化手性向列型介孔硅(CNMS-SO₃H)固体酸催化剂。通过比表面积分析(BET)、X射线衍射仪(XRD)、红外吸收光谱分析法(FT-IR)、氨-程序升温脱附(NH₃-TPD)和吡啶吸附红外光谱(Py-FTIR)等技术手段表征催化剂的结构和性质。结果表明,在α-蒎烯与无水草酸物质的量比为1∶0.4,CNMS-SO₃H催化剂用量与松节油的质量比为7∶100。温度为100 ℃,时间为8 h,龙脑的收率最高为49.89%,α-蒎烯转化率为100%,正龙脑的量是异龙脑的4倍。固体酸催化剂具有很好的催化活性和稳定性,在重复使用8次之后,α-蒎烯转化率在99%以上。

关键词: 磺酸化手性向列型介孔二氧化硅, 固体酸, 酯化, 龙脑

Abstract: Chiral nematic mesoporous silicate (CNMS) was prepared by a sol-gel method and sulfonated CNMS-SO₃H solid acid catalyst was prepared by an impregnation method. The structure and properties of the catalysts were characterized by BET, powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy analysis (FT-IR), NH₃-TPD and Py-FTIR. When the molar ratio of amount of substance of α-pinene to oxalic acid is 1∶0.4, the mass ratio of CNMS-SO₃H catalyst to turpentine oil is 7∶100, the temperature is 100 ℃ and the time is 8 h, the conversion of α-pinene is 100% and the yield of borneol is 49.89% and the amount of borneol is 4 times of that of isoborneol. The solid acid catalyst has good catalytic activity and stability. After 8 times of reuse, the conversion of α-pinene is over 99%.

Key words: sulfonated chiral nematic mesoporous silicate, solid acid, esterification, borneol

中图分类号:

O629

郭炜, 王亚明, 蒋丽红, 郑燕娥, 刘壁莹. 磺酸化手性向列型介孔二氧化硅的制备及其催化合成龙脑[J]. 应用化学, 2020, 37(12): 1447-1456.

GUO Wei, WANG Yaming, JIANG Lihong, ZHENG Yan'e, LIU Biying. Preparation of Sulfonated Chiral Nematic Mesoporous Silicate Solid Acid and Its Catalytic Synthesis of Borneol[J]. Chinese Journal of Applied Chemistry, 2020, 37(12): 1447-1456.

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