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Preparation method of Ag/ZnO hierarchical structure microsphere

A hierarchical structure and microsphere technology, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of small nano-photocatalyst particles, reduced catalytic activity of catalysts, and difficulty in separating nano-catalysts , to achieve good photocatalytic degradation performance, cost saving, and mild reaction conditions

Active Publication Date: 2013-06-12
徐州市正峰锌业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although nanoscale Ag / ZnO photocatalysts have high photocatalytic efficiency, from a practical point of view, due to the very large surface energy of nano-ZnO particles, they are easy to coalesce to form large particles during use, which will reduce the photocatalytic efficiency of the catalyst. Catalytic activity
On the other hand, the particle size of the nano-photocatalyst is small, and it is difficult to separate the nano-catalyst from the reaction system after the catalytic reaction is completed, which is not conducive to the recycling of the catalyst.

Method used

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  • Preparation method of Ag/ZnO hierarchical structure microsphere
  • Preparation method of Ag/ZnO hierarchical structure microsphere
  • Preparation method of Ag/ZnO hierarchical structure microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add 0.03 mol zinc sulfate (Zn(SO 4 ) 2 ·7H 2 O), 0.06 mol hexamethylenetetramine and 2 mmol potassium sodium tartrate were dissolved in deionized water, stirred for 10 min to completely dissolve, then added 0.5% (mass ratio) silver nitrate and mixed thoroughly under stirring at room temperature ;

[0022] (2) Put the above mixed solution in an oven at 90 °C for 12 h to obtain a white mixed solution;

[0023] (3) After cooling the above mixture, centrifuge at 2000 r / min for 5 min, pour off the upper liquid, wash the precipitate repeatedly with water and ethanol, and then dry it in a 60 °C drying oven;

[0024] (4) Heat the powder obtained in step (3) to 300 °C in a tube furnace at a heating rate of 1 °C / min, and hold for 0.5 h to obtain Ag / ZnO hierarchical structure microspheres with regular morphology and controllability .

Embodiment 2

[0026] (1) Add 0.03 mol zinc sulfate (Zn(SO 4 ) 2 ·7H 2 O), 0.06 mol hexamethylenetetramine and 2 mmol potassium sodium tartrate were dissolved in deionized water, stirred for 10 min to completely dissolve, and then 2.5% (mass ratio) of silver nitrate was added under stirring at room temperature and mixed thoroughly ;

[0027] (2) Put the above mixed solution in an oven at 90 °C for 12 h to obtain a white mixed solution;

[0028] (3) After cooling the above mixture, centrifuge at 2000 r / min for 5 min, pour off the upper liquid, wash the precipitate repeatedly with water and ethanol, and then dry it in a 60 °C drying oven;

[0029] (4) Heat the powder obtained in step (3) to 300 °C in a tube furnace at a heating rate of 1 °C / min, and hold for 0.5 h to obtain Ag / ZnO hierarchical structure microspheres with regular morphology and controllability .

Embodiment 3

[0031] (1) Add 0.03 mol zinc sulfate (Zn(SO 4 ) 2 ·7H 2 O), 0.2 mol hexamethylenetetramine and 2 mmol potassium sodium tartrate were dissolved in deionized water, stirred for 10 min to completely dissolve, and then 0.5% (mass ratio) silver nitrate was added under stirring at room temperature and mixed thoroughly ;

[0032] (2) Put the above mixed solution in an oven at 90 °C for 12 h to obtain a white mixed solution;

[0033] (3) After cooling the above mixture, centrifuge at 2000 r / min for 5 min, pour off the upper liquid, wash the precipitate repeatedly with water and ethanol, and then dry it in a 60 °C drying oven;

[0034] (4) Heat the powder obtained in step (3) to 300 °C in a tube furnace at a heating rate of 1 °C / min, and hold for 0.5 h to obtain Ag / ZnO hierarchical structure microspheres with regular morphology and controllability .

[0035] The powder X-ray diffraction (XRD) of the sample was carried out on a D / Max-2500 / PC X-ray diffractometer, figure 1 For th...

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Abstract

The invention provides a preparation method of an Ag / ZnO hierarchical structure microsphere. The preparation method comprises the following steps: taking water as a reaction medium, zinc sulfate as a zinc source, silver nitrate as a silver source, sodium potassium tartrate tetrahydrate as a ligand and hexamethylenetetramine as a precipitating agent to react under a certain condition; and centrifugally washing and drying the acquired product Ag / ZnO after the reaction is ended, then roasting and thermally decomposing the Ag / ZnO in a tube furnace to acquire a regularly-shaped and controllable Ag / ZnO hierarchical structure microsphere. The structure form of the microsphere remains complete. The preparation method of the Ag / ZnO hierarchical structure microsphere disclosed by the invention is simple; the size, structure and shape of the product Ag / ZnO microsphere are easily controlled; the yield is high; the problems of poor regularity and easy agglomeration in the using process of the Ag / ZnO structure in the prior art are solved; and the Ag / ZnO hierarchical structure microsphere prepared by the preparation method has excellent photo-catalytic property for organic dyes such as methyl orange and the like.

Description

technical field [0001] The invention belongs to the field of inorganic functional materials, and relates to a preparation method of Ag / ZnO microspheres with hierarchical structure, and further relates to a preparation method of Ag / ZnO hierarchical structure microsphere photocatalysts. Background technique [0002] As a II-VI n-type broadband semiconductor material, ZnO has a forbidden band energy interval of 3.37 eV and an exciton binding energy of 60 meV at room temperature. Due to its cheap price, environmental friendliness, and high catalytic efficiency, nanostructured ZnO has become an important photocatalyst. However, for ZnO, the actual photocatalytic effect of ZnO is greatly reduced due to the rapid recombination of electrons and holes generated by its photoexcitation. Metal Ag can be used as an effective trap for photo-generated electrons, so that the photo-generated electrons on the conduction band of ZnO can be transferred to metal Ag, so the introduction of Ag ca...

Claims

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Application Information

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IPC IPC(8): B01J23/66B01J35/08
Inventor 宋彩霞魏晓星钟洋公国栋王哲王德宝
Owner 徐州市正峰锌业有限公司
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