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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

Active Publication Date: 2017-10-31
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the methods that can effectively construct defects on oxides are mainly calcination in reducing atmosphere, argon plasma bombardment, etc. These methods are complicated and cumbersome, require high equipment requirements, and have certain risks.
Although defects can also be introduced by ultraviolet light reduction, its stability is often poor, and it is easy to fill defects in an oxygen environment. Therefore, it is necessary to develop a mild and simple method to prepare stable and Existing defects, to solve many problems and drawbacks in the current preparation process

Method used

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  • A preparation method of defect-state tungsten trioxide for photocatalytic aerobic coupling
  • A preparation method of defect-state tungsten trioxide for photocatalytic aerobic coupling
  • A preparation method of defect-state tungsten trioxide for photocatalytic aerobic coupling

Examples

Experimental program
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Effect test

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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Abstract

The invention discloses a method for preparing defective tungsten trioxide for photocatalytic aerobic coupling, which is characterized by molar ratio 1: (1~2.5): (1~10) taking tungsten source precursor and surface modification Add citric acid and reducing agent glucose to water and stir until dissolved. Use hydrochloric acid to adjust the pH value to 0-1. Place it in a reactor for hydrothermal reaction at 120-180°C for 12-48 hours to obtain tungsten trioxide hydrate with oxygen defects; Then it is calcined at 300-500°C for 1-3 hours under an inert atmosphere, and then cooled to room temperature to obtain tungsten trioxide with oxygen defects. The present invention uses a reducing agent to undergo in-situ reduction during the nucleation process to obtain oxygen defects, which simplifies the difficulty of preparing oxygen defects, has mild conditions and low cost, and can control the concentration of oxygen defects by adjusting the amount of reducing agent and experimental parameters of calcination. . The obtained tungsten trioxide with oxygen defects has good photoresponse and can realize organic catalytic aerobic coupling reaction.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic nanometer materials, and in particular relates to a preparation method of defect-state tungsten trioxide used for photocatalytic aerobic coupling. Background technique [0002] With the continuous development of human society, energy consumption is increasing day by day, and non-renewable energy sources such as oil, coal, and natural gas are gradually exhausted. Therefore, the development of renewable energy is a vital research direction today. At the same time, in today's industrial chemical catalysis, most of the catalytic systems use platinum, palladium, ruthenium and other noble metals as catalysts and use thermal energy to drive catalytic reactions, which greatly increases the required energy consumption and catalyst costs. Therefore, The development of low-energy, low-cost catalysts is also an inevitable direction for future sustainable development. [0003] As a green and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/02B82Y40/00B01J23/30
CPCC01G41/02B01J23/30C01P2002/72C01P2002/01C01P2004/03C01P2002/86C01P2002/84C01P2004/62B01J35/40B01J35/39
Inventor 熊宇杰张宁
Owner UNIV OF SCI & TECH OF CHINA
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