引用本文:
骆耿耿, 林深, 杨柳艺, 陈杰博, 张燕琼. 多金属氧酸盐纳米粉体室温固相合成、表征及催化性能[J]. 应用化学,
2006, 23(6): 591-596.
Citation: LUO Geng-Geng, LIN Shen, YANG Liu-Yi, CHEN Jie-Bo, ZHANG Yan-Qiong. Preparation,Characterization and Catalytic Activity of Polyoxometalate Nanometer Powders Obtained at Room Temperature by Solid State Reaction[J]. Chinese Journal of Applied Chemistry, 2006, 23(6): 591-596.
Citation: LUO Geng-Geng, LIN Shen, YANG Liu-Yi, CHEN Jie-Bo, ZHANG Yan-Qiong. Preparation,Characterization and Catalytic Activity of Polyoxometalate Nanometer Powders Obtained at Room Temperature by Solid State Reaction[J]. Chinese Journal of Applied Chemistry, 2006, 23(6): 591-596.
多金属氧酸盐纳米粉体室温固相合成、表征及催化性能
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。
English
Preparation,Characterization and Catalytic Activity of Polyoxometalate Nanometer Powders Obtained at Room Temperature by Solid State Reaction
Abstract:
(NH4)4[PMo11VO40]·4H2O nanometer powders were prepared by solid state reaction between H4PMo11VO40·13H2O and(NH4)2C2O4·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 m2/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.
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Key words:
- polyoxometalates
- / nanometer powders
- / solid state reaction
- / catalytic activity
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