多金属氧酸盐纳米粉体室温固相合成、表征及催化性能  

Preparation,Characterization and Catalytic Activity of Polyoxometalate Nanometer Powders Obtained at Room Temperature by Solid State Reaction

作　　者：骆耿耿[1] 林深[1] 杨柳艺[1] 陈杰博[1] 张燕琼[1] 

机构地区：[1]福建师范大学化学与材料学院,福州350007

出　　处：《应用化学》2006年第6期591-596,共6页Chinese Journal of Applied Chemistry

基　　金：国家教育部科技计划项目(205078);福建省教育厅A类重点项目(JA04167)

摘　　要：以H4[PMo11VO40].13H2O和(NH4)2C2O4.H2O为原料,采用室温固相反应合成出(NH4)4-[PMo11VO40].4H2O纳米粉体。采用元素分析、DRS、FTIR、XRD、TG-DTA和BET等测试技术对其组成、结构和性能进行了表征。结果表明,(NH4)4[PMo11VO40].4H2O粉体平均粒径为25 nm,并保留着杂多阴离子的Keggin结构,比表面积为157.82 m2/g,在390℃以下杂多阴离子有良好的热稳定性。以环己醇分子内脱水生成环己烯为探针反应,测试了该纳米多金属氧酸盐粉体的催化活性。结果表明,当催化剂用量为环己醇的8.31%,反应温度为160℃时,可在0.5 h内完成脱水反应,环己烯产率达77.98%。该纳米粉体可以作为一种新型的固体酸催化剂,且其催化性能优于常规粉体和一般纯杂多酸。（NH4）4 [ PMo11VO40 ] · 4H2O nanometer powders were prepared by solid state reaction between H4 PMo11VO40 · 13H2O and （ NH4 ） 2 C2O4 · H2O at room temperature and characterized by elemental analysis, FTIR, XRD, TEM, TG-DTA and BET techniques. The experimental results indicate that the nanometer powders remain Keggin structure and have a mean grain size of 25 nm and BET specific surface area of 157.82 m^2/g. The heteropolyanion shows good thermal stability up to 390 %. Using so-obtained nanomaterial as catalyst for the dehydration of cyclohexanol, the yield of cyclohexene could reach 77.98%, which is higher than those of currently widely used catalyst as well as its bulk counterpart. The yield was achived under optimized catalytic reaction conditions with the mass ratio （catalyst/cyclohexanol） of 8.31%, 0. 5 h reaction duration and 160 ℃ reaction temperature.

关 键 词：多金属氧酸盐 纳米粉体 固相合成 催化性能 

分 类 号：O613.6[理学—无机化学] O611.4[理学—化学]