| 双杂原子Ti-V-β沸石的合成、表征及催化性能研究 |
| Synthesis, Characterization and Catalytic Behavior of Bihetero-atom Ti-V-β Zeolite |
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| 摘要: 以白炭黑(二氧化硅)为硅源、四乙基氢氧化铵为模板剂、硫酸钛为钛源、偏钒酸铵为钒源、氟化钠为矿化剂，采用水热法合成了Ti-V-β沸石。探讨了合成条件对Ti-V-β沸石形成的影响。运用XRD、IR、UV-Vis固体漫反射光谱、TG/DTA、SEM+EDS和ICP等测试技术对样品进行了表征并测定了样品中Ti和V的含量。结果表明，按下列化学组成配制初始反应混合物：n(SiO2)∶n(V2O5)∶n(TiO2)∶n[(TEA)2O]∶n(H2O)∶n(NaF)=60∶(0.05～1.2)∶(0.1～2.4)∶(12～18)∶(450～720)∶(4～14)，可制备出Ti-V-β沸石，Ti和V原子进入了沸石骨架。对样品在以H2O2为氧化剂氧化苯乙烯反应中的催化活性作了初步考察，结果表明，Ti-V-β沸石具有很高的催化活性，在下列反应条件下：v(H2O2)/v(ph CH=CH2)=2.6，V(acetone)/v(phCH=CH2)=10，m(cat)/v(phCH=CH2)=0.003 g·mL-1，T=80 ℃，t=6 h，苯乙烯的转化率98.16%。产品的选择性为：苯甲醛68.15%，苯乙醛23.35%，苯乙酮6.61%。 |
| 关键词: 水热合成 沸石 苯乙烯 氧化 |
| 基金项目: |
| Abstract: Ti-V-β zeolite has been hydrothermally synthesized using fumed silica (SiO2) as the silica source，tetraethyl ammonium hydroxide (TEAOH) as the template，titanium sulfate as the titanium source，metavanadic acid ammonium as the Vanadium source and sodium fluoride(NaF) as the mineral agent. The effects of various factors on the synthesis of Ti-V-β zeolite have been investigated. The samples synthesized have been characterized by ICP, XRD, IR, TG/DTA, SEM/EDS and UV-Visible diffuse reflectance spectroscopy to evaluate the structure of the products and measure the contents of vanadium and titanium. The experimental results indicate that Ti-V-β zeolite can be synthesized from the original mixture with the molar ratio of n(SiO2)∶n(V2O5)∶n(TiO2)∶n[(TEA)2O]∶n(H2O)∶n(NaF)=60∶(0.05～1.2)∶(0.1～2.4)∶(12～18)∶(450～720)∶(4～14),and the Ti and V atoms present in the framework of the zeolite. The catalytic behavior of Ti-V-β zeolite in oxidation of styrene using H2O2 as the oxidant has also been explored. The results have shown that Ti-V-β zeolites have high catalytic activity. The conversion of styrene is 98.16% under the following reaction conditions: 80 ℃, 6 h, V(H2O2)/V(styrene)=2.6, V(acetone)/V(styrene)=10, m(cat)/V(styrene)=0.003 g·mL-1. The selectivity for the products is phCHO 68.15%, phCH2CHO 23.35% and phCOMe 6.61% respectively. |
| Keywords: hydrothermal synthesis zeolite styrene oxidation |
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| 李艳凤,喻 铃,何 震,何红运.双杂原子Ti-V-β沸石的合成、表征及催化性能研究[J].无机化学学报,2008,24(1):117-123. |
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