MIL-101(Fe)高效催化 β-蒎烯与甲醛的Prins缩合制备诺卜醇

通过水热晶化法制备了MIL-101(Fe)金属有机骨架材料, 利用X射线衍射(XRD)、 傅里叶变换红外光谱(FTIR)、 热重分析(TG)、 扫描电子显微镜(SEM)、 透射电子显微镜(TEM)和X射线光电子能谱(XPS)对催化剂的结构和形貌进行了表征. 结果表明, 该材料用于催化β-蒎烯与甲醛的Prins缩合制备诺卜醇反应的效果优异; 催化剂合成温度、 合成时间、 催化剂用量、 反应溶剂、 反应温度和反应时间对β-蒎烯的反应结果均有一定影响. 在相似的反应条件下, 合成的MIL-101(Fe)催化β-蒎烯制备诺卜醇反应的最佳条件为使用150 ℃下反应15 h合成的催化剂MIL-101(Fe), 在90 ℃下反应8 h得到的β-蒎烯转化率高达97.3%, 诺卜醇选择性达到96.7%.

Highly Efficient MIL-101(Fe) Catalyst for the Preparation of Nopol by the Prins Condensation of β-Pinene and Formaldehyde†

Metal organic framework materials MIL-101(Fe) were prepared by hydrothermal synthesis method. All the catalysts were characterized by X-ray diffraction(XRD), Fourier transform infrared spectra(FTIR), thermogravimetric analysis(TG), scanning electron microscopy(SEM), transmission electron microscopy(TEM) and X-ray photoelectron spectroscopy(XPS). Those materials were applied for the catalytic condensation of β-pinene and formaldehyde, and achieved excellent catalytic result. The results indicated that the catalyst synthesis temperature, synthesis time, catalyst amount, solvent, reaction temperature and time have certain effects on the reaction results of condensation reaction. Under similar reaction conditions, MIL-101(Fe)-150-15 catalyst was found to be the most active in the Prins condensation of β-pinene and formaldehyde, for which 97.3% of conversion and 96.7% selectivity are achieved within 8 h at 90 ℃.