McDonald Kori D, Bartlett Bart M
Department of Chemistry, University of Michigan 930 North University Avenue Ann Arbor Michigan 48109-1055 USA
RSC Adv. 2019 Sep 11;9(49):28688-28694. doi: 10.1039/c9ra04839a. eCollection 2019 Sep 9.
With the aid of direct heating through microwave irradiation in non-aqueous media, nanocrystalline tungsten(vi) oxide is achievable in 30 minutes at 200 °C, faster and at a lower temperature than conventional synthesis methods. Forming in a platelet morphology, these particles are as small as 20 nm with a BET surface area of 37 m g WO. These nanoplatelets are active for the photocatalytic oxidation of the 1° alcohols benzyl alcohol (rate constant, of 2.6 × 10 h) and 5-(hydroxymethyl)-2-furfural ( of 0.01 h) using 10 mg of WO with 2 mL of 0.250 M substrate in acetonitrile and a 150 mW cm 460 nm blue LED source. As expected, these rate constants are larger than those observed for commercially prepared, micron-sized WO. XPS analysis shows that during catalysis, the concentration of W on the surface increases, but the nanoplatelets are stable under these reaction conditions. The overall morphology and size of the particles are retained through the reactions. Moreover, the nanoplatelets are recyclable-showing no loss in activity for four reaction cycles.
在非水介质中通过微波辐射直接加热的辅助下,纳米晶氧化钨(VI)在200°C下30分钟即可制得,比传统合成方法更快且温度更低。这些颗粒呈片状形态,尺寸小至20nm,BET表面积为37m²/g WO₃。使用10mg WO₃、2mL 0.250M底物在乙腈中以及150mW/cm² 460nm蓝色LED光源,这些纳米片对一级醇苄醇(速率常数为2.6×10⁻⁵ h⁻¹)和5-(羟甲基)-2-糠醛(速率常数为0.01 h⁻¹)的光催化氧化具有活性。正如预期的那样,这些速率常数大于商业制备的微米级WO₃所观察到的速率常数。XPS分析表明,在催化过程中,表面W的浓度增加,但纳米片在这些反应条件下是稳定的。通过反应,颗粒的整体形态和尺寸得以保留。此外,纳米片可回收利用——在四个反应循环中活性没有损失。