A preparation method of defect-state tungsten trioxide for photocatalytic aerobic coupling
A tungsten trioxide, photocatalysis technology, applied in chemical instruments and methods, tungsten oxide/tungsten hydroxide, physical/chemical process catalysts, etc., can solve the problems of complicated steps, high equipment requirements, poor stability, etc., to simplify Difficulty in preparing defects, low cost, mild reaction conditions
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Embodiment 1
[0032] Example 1: Preparation and Characterization of Tungsten Trioxide Nanosheets with Oxygen Defects
[0033] Measure 30mL of deionized water, put it in a beaker with a capacity of 100mL, then weigh 1mmol sodium tungstate dihydrate, 1mmol citric acid and 5mmol glucose, add them to the above beaker, stir for 20min, and disperse and dissolve all the raw materials; Add a 6mol / L hydrochloric acid solution dropwise to the above solution, adjust the pH value to 0.3, and continue to stir for 30 minutes; transfer the reaction solution to a 50mL polytetrafluoroethylene liner, put it into a stainless steel reactor and seal it , the reaction kettle was heated in an oven at 120°C for 24h, and cooled to room temperature naturally; the obtained sample was first washed with deionized water and then centrifuged with ethanol, and then dried in a vacuum oven at 60°C for 12h to obtain Defective tungsten trioxide hydrate nanosheets; the sample of tungsten trioxide hydrate nanosheets with oxygen...
Embodiment 2
[0043] Example 2: Light-driven aerobic coupling reaction
[0044]Take 20 mg of tungsten trioxide nanosheets with oxygen defects prepared in Example 1, ultrasonically disperse them in 4 mL of acetonitrile, add 10 uL of benzylamine; transfer the above reaction solution to a quartz tube with a volume of 30 mL, and replace the reaction atmosphere with oxygen . At room temperature, the light intensity introduced by a xenon lamp is 100mW / cm 2 The incident light is used, and the ultraviolet light is filtered out with a 400nm filter to drive the organic oxidation reaction.
[0045] Figure 7 The conversion efficiencies of the tungsten trioxide nanosheets prepared in Example 1 in the light-driven benzylamine aerobic coupling reaction at different times in this example are given. It can be seen that the trioxide nanosheets with oxygen defects prepared in Example 1 Tungsten oxide nanosheets have good photocatalytic benzylamine aerobic coupling reaction at room temperature.
Embodiment 3
[0047] Measure 30mL of deionized water, put it in a beaker with a capacity of 100mL, then weigh 1mmol of sodium tungstate dihydrate, 1mmol of citric acid and 5mmol of glucose, add them to the above beaker, stir for 20min, and disperse and dissolve all the raw materials; Add 6mol / L hydrochloric acid solution dropwise to the above solution to adjust the pH value to 0, and continue to stir for 30 minutes; transfer the reaction solution to a polytetrafluoroethylene liner with a volume of 50mL, put it into a stainless steel reactor and seal it, and The reaction kettle was heated in an oven at 120°C for 24h. After the reaction was completed, it was naturally cooled to room temperature; the obtained sample was first washed with deionized water and then centrifuged with ethanol, and then dried in a vacuum oven at 60°C for 12h to obtain Oxygen-deficient tungsten trioxide hydrate nanosheets; the sample of tungsten trioxide hydrate nanosheets with oxygen defects was placed in a porcelain ...
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