磷钨钼杂多阴离子柱撑水滑石的制备及催化合成乙酰水杨酸  

Tungstomolybdophosphate heteropolyanions pillared layered double hydroxides(LDHs):preparation and catalytic systhesis of acetylsalicylic acid

作　　者：林文权[1] 王力耕[1] 袁庭[1] 施炜[1] 倪哲明[1] 

机构地区：[1]浙江工业大学化学工程与材料学院,杭州310032

出　　处：《浙江工业大学学报》2011年第6期609-613,634,共6页Journal of Zhejiang University of Technology

摘　　要：以NO3-LDHs水滑石为前躯体,用离子交换法将三种磷钨钼杂多阴离子[PWxMo12-xO403]-(x=1,3,6)柱撑到水滑石层间,用XRD和FT-IR方法对样品进行了表征.并以水杨酸和乙酸酐为原料,考察了催化剂合成乙酰水杨酸的催化活性.结果表明:[PWxMo12-xO403]-(x=1,3,6)已完全取代了前体水滑石中NO3-进入水滑石层间,得到晶相良好的PWxMo12-x-LDHs(x=1,3,6).其中PWMo11-LDHs催化剂具有催化活性高,其最佳催化合成条件:反应时间10min,反应温度75℃,水杨酸与乙酸酐摩尔比为1∶2,催化剂用量为水杨酸质量的10%,乙酰水杨酸收率达82.02%.Three kinds of tungstomolybdophosphate heteropolyanions [PWxMo12-xO40]3-（x=1,3,6） pillared layered double hydroxides （LDHs） were prepared by ion exchange using NO3-- LDHs as a precursor. The materials prepared were characterized by XRD and FT-IR . The catalytic activity were further investigated in the synthesis of acetylsalicylic acid with salicylic acid and acetic anhydride as materials. The results showed that [PWxMo12-xO40]3-（x=1,3,6） could totally replace the original interlayer nitrate anions of the NO3--LDHs, producing [PWxMo12-xO40]3-（x=1,3,6） with good crystallinity. And the PWMou--LDHs catalyst has high catalytic activity. The optimum reaction conditions for the catalytic synthesis of acetylsalicylic acid on the PWMo11-LDHs catalyst were obtained as follows： the reaction time was 10 min, the reaction temperature was 75℃, the molar ratio of salicylic acid to acetic anhydride was 1 ： 2, the amount of catalyst was equal to 10% salicylic acid. Under these conditions, the yield of acetylsalicylic acid reached 82.02 %.

关 键 词：水滑石 磷钨钼杂多阴离子 乙酰水杨酸 催化活性 

分 类 号：O643.321[理学—物理化学]