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

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。

Preparation of Sulfonated Chiral Nematic Mesoporous Silicate Solid Acid and Its Catalytic Synthesis of Borneol

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%.