Li Ruiyun, Song Heyuan, Wang Guoqin, Chen Jing
State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics (LICP), Chinese Academy of Sciences Lanzhou 730000 P. R. China
University of Chinese Academy of Sciences Beijing 100049 P. R. China.
RSC Adv. 2018 Feb 13;8(13):7179-7185. doi: 10.1039/c7ra13385e. eCollection 2018 Feb 9.
Ketalization of cyclohexanone with glycol has been carried out using molecular sieve SBA-15 immobilized Brønsted acidic ionic liquid catalyst. The properties of the heterogeneous catalysts were characterized by elemental analysis, Fourier transform infrared (FT-IR) spectra, scanning electron microscopy (SEM), thermogravimetry/differential scanning calorimetry (TG/DSC), and N adsorption-desorption (BET). The results suggested that Brønsted acidic ionic liquid [BSmim][HSO] had been successfully immobilized on the surface of SBA-15 and the catalytic performance evaluation demonstrated that the catalyst BAIL@SBA-15 exhibited excellent catalytic activities in the ketalization of cyclohexanone with glycol. In addition, the effects of reaction temperature, catalyst loading, reaction time, and reactant molar ratio have also been investigated in detail, and a general reaction mechanism for the ketalization of cyclohexanone with glycol was given. The SBA-15 immobilized ionic liquid can be recovered easily and after reusing for 5 times in the ketalization reaction, the catalyst could still give satisfactory catalytic activity.
已使用负载于分子筛SBA - 15上的布朗斯特酸性离子液体催化剂实现了环己酮与二醇的缩酮化反应。通过元素分析、傅里叶变换红外(FT - IR)光谱、扫描电子显微镜(SEM)、热重/差示扫描量热法(TG/DSC)以及N吸附 - 脱附(BET)对多相催化剂的性质进行了表征。结果表明,布朗斯特酸性离子液体[BSmim][HSO]已成功负载于SBA - 15表面,催化性能评价表明催化剂BAIL@SBA - 15在环己酮与二醇的缩酮化反应中表现出优异的催化活性。此外,还详细研究了反应温度、催化剂用量、反应时间和反应物摩尔比的影响,并给出了环己酮与二醇缩酮化反应的一般反应机理。负载于SBA - 15上的离子液体易于回收,在缩酮化反应中重复使用5次后,该催化剂仍能给出令人满意的催化活性。