H_6P_2Mo_9W_9O_(62)/Cu_3(BTC)_2的制备及催化合成缩醛(酮)  

Preparation of H_6P_2Mo_9W_9O_(62)/Cu_3(BTC)_2 and its catalytic performance for synthesis of acetals and ketals

作　　者：向诗银 杨水金 

机构地区：[1]湖北师范大学化学化工学院,湖北黄石435002

出　　处：《日用化学工业》2017年第5期281-285,共5页China Surfactant Detergent & Cosmetics

基　　金：湖北省自然科学基金重点资助项目(2014CFA131)

摘　　要：采用浸渍法制得H_6P_2Mo_9W_9O_(62)/Cu_3(BTC)_2,利用傅里叶变换红外光谱仪(FT-IR)、X射线衍射仪(XRD)、热重分析仪(TG)以及扫描电镜(SEM)表征其组成、结构、热稳定性以及形貌。以H_6P_2Mo_9W_9O_(62)/Cu_3(BTC)_2为催化剂,环己酮和乙二醇合成缩酮的反应为探针,探究出较佳反应条件:环己酮用量为0.2 mol,n(环己酮)∶n(乙二醇)=1∶1.3,催化剂用量占反应物总质量的0.3%,反应时间为60 min,带水剂用量为6 mL。在此条件下,环己酮乙二醇缩酮收率可达83.7%。且以上条件下催化合成苯甲醛乙二醇缩醛、丁酮乙二醇缩酮、丁酮1,2-丙二醇缩酮、苯甲醛1,2-丙二醇缩醛和环己酮1,2-丙二醇缩酮的收率分别为70.1%,66.0%,62.1%,66.3%和75.8%。与分子筛MCM-48负载硅钨酸、活性炭负载对甲苯磺酸和铝交联蒙脱土催化剂相比,H_6P_2Mo_9W_9O_(62)/Cu_3(BTC)_2是一种催化性能较好的催化剂。H6P2Mo9W9O62/Cu3（BTC）2as a new catalyst was prepared by impregnation method. Fourier transformation infrared spectrum （ FT - IR ） , X - ray diffraction （ XRD ） , thermal gravimetry （ TG ） and scanning electron microscope （SEM） were used for characterization and measurement of its composition, structure, thermal stability and morphology. The reaction, with H6P2Mo9W9O62/Cu3（BTC）2 as catalyst, for synthesis of ketal from cyclohexanone and ethylene glycol as starting materials was used as probe reaction, and the optimized synthesis conditions were found by orthogonal experiments as follows： fixing the amount of eyclohexanone as 0. 2 mol ; molar ratio, n （ cyclohexanone ） ： n （ ethylene glycol） = 1 ： 1.3 ; mass ratio of the catalyst to total reactants, 0. 3 % ; the reaction time, 60 min ; and amount of water stripping agent, 6 mL. The yield of the product reaches 83.7%. Under similar reaction conditions, the yield of benzaldehyde ethylene glycol acetal reaches 70. 1% ; butanone glycol ketal, 66.0% ; butanone 1,2 - propylene glycol ketal, 62. 1% ; benzaldehyde 1,2 - propanediol acetal, 66.3% ; and cyclohexanone 1,2 - propylene glycol ketal, 75.8%. Compared with that of catalysts H4SiW12O40/MCM-48, activated carbon supported p- toluene sulfonic acid and A1- cross linked montmorillonite,H6P2Mo9W9O62/Cu3（BTC）2 shows better catalytic performance.

关 键 词：合成香料 缩醛(酮) 催化合成 金属有机骨架 

分 类 号：O643.36[理学—物理化学] TQ224.4[理学—化学]