Preparation method of microspheric ZnO-BiOI composite material

A composite material, spherical technology, applied in chemical instruments and methods, catalyst activation/preparation, water treatment of special compounds, etc., can solve the problems of poor photocatalytic activity, large limitations, complex processes, etc., and achieve a simple and easy preparation process. , Excellent photocatalytic performance, high photocatalytic activity effect

Active Publication Date: 2019-07-12
NORTHEASTERN UNIV
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Problems solved by technology

[0008] In order to solve the technical problems of low safety, high energy consumption, low efficiency, complex process and large limitations in the preparation of microspherical ZnO-BiOI composite materials in the prior art and the microspherical ZnO-BiOI prepared by the prior art Composite materials have problems such as small specific surface area, large band gap, and poor photocatalytic activity. The present invention provides a method for preparing a microspherical ZnO-BiOI composite material, which is used to prepare a microspherical ZnO-BiOI composite material with high catalytic activity. material, the preparation method of the present invention is safe, energy-saving, efficient, simple to operate, green and environmentally friendly, low in cost, the prepared product has a large specific surface area, a narrow band gap and exhibits high photocatalytic activity

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  • Preparation method of microspheric ZnO-BiOI composite material

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Embodiment 1

[0044] This embodiment is about a preparation method of microspherical ZnO-BiOI composite material, which comprises the following steps:

[0045] (1) ZnO with a purity of more than 99.9% is selected as the initial raw material, which is denoted as A-ZnO. Among them: the microscopic appearance of A-ZnO is a rod-like structure with a particle size of 30nm, the macroscopic appearance of A-ZnO is white powder, and its X-ray diffraction diagram is shown in figure 2 .

[0046] (2) Take an appropriate amount of A-ZnO and place it in a crucible, treat it in a muffle furnace at 500°C for 10 minutes, then take it out and cool it to room temperature, and the obtained product is designated as B-ZnO.

[0047] (3) Weigh 12.50g of B-ZnO and 1.25g of NaH respectively 2 PO 4 Disperse them evenly in 500mL of 0.5mL / mL ethanol aqueous solution, stir magnetically and boil and reflux for 8h. Drying at lower temperature for 4h to obtain P-ZnO;

[0048] (4) Weigh 0.26 g of P-ZnO and ultrasonica...

Embodiment 2

[0053] This embodiment is about a preparation method of microspherical ZnO-BiOI composite material, which comprises the following steps:

[0054] (1) ZnO with a purity of more than 99.9% is selected as the initial raw material, which is denoted as A-ZnO. Among them: the microscopic appearance of A-ZnO is a rod-like structure with a particle size of 30nm, the macroscopic appearance of A-ZnO is white powder, and its X-ray diffraction diagram is shown in figure 2 .

[0055] (2) Take an appropriate amount of A-ZnO and place it in a crucible, treat it in a muffle furnace at 450°C for 15 minutes, then take it out and cool it to room temperature, and the obtained product is designated as B-ZnO.

[0056] (3) Weigh 10.00g of B-ZnO and 0.50g of NaH respectively 2 PO 4 And they were uniformly dispersed into 500mL of 0.4mL / mL ethanol aqueous solution, magnetically stirred and boiled and refluxed for 6h. Drying at lower temperature for 5h to obtain P-ZnO;

[0057] (4) Weigh 0.26 g of...

Embodiment 3

[0062] This embodiment is about a preparation method of microspherical ZnO-BiOI composite material, which comprises the following steps:

[0063] (1) ZnO with a purity of more than 99.9% is selected as the initial raw material, which is denoted as A-ZnO. Among them: the microscopic appearance of A-ZnO is a rod-like structure with a particle size of 30nm, the macroscopic appearance of A-ZnO is white powder, and its X-ray diffraction diagram is shown in figure 2 .

[0064](2) Take an appropriate amount of A-ZnO and place it in a crucible, treat it in a muffle furnace at 550°C for 8 minutes, then take it out and cool it to room temperature, and the obtained product is designated as B-ZnO.

[0065] (3) Weigh 11.25g of B-ZnO and 0.84g of NaH respectively 2 PO 4 Disperse them evenly in 500mL of 0.6mL / mL ethanol aqueous solution, stir magnetically and boil and reflux for 7h. Drying at lower temperature for 4h to obtain P-ZnO;

[0066] (4) Weigh 0.26 g of P-ZnO and ultrasonicall...

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Abstract

The invention relates to a preparation method of a microspheric ZnO-BiOI composite material. The preparation method comprises the following steps: S1: pre-treating ZnO at 450 to 550 DEG C, and takingout and cooling the ZnO; S2: dispersing the ZnO treated in Step S1 together with dihydrogen phosphate into an aqueous solution of ethanol, stirring and boiling the solution and performing refluxing for 5 to 8 h to obtain phosphorus-doped ZnO; S3: suspending the phosphorus-doped ZnO in a dispersing agent to obtain a dispersion system A, respectively dissolving water or alcohol-soluble trivalent phosphonium salt and iodized salt in a dispersing agent to obtain a dispersion system B and a dispersion system C respectively; S4: synchronously and continuously dropwise adding the dispersion systems Band C into the dispersion system A, and then transferring the systems into a reaction kettle having the temperature of 75 to 85 DEG C for stirring and reaction for 2 to 5 h, and standing the mixtureafter the reaction is ended; and performing separation, precipitation, washing, drying and grinding to obtain the microspheric ZnO-BiOI composite material. The method disclosed by the invention is simple and environmentally friendly, and the prepared ZnO-BiOI composite material has good regularity and high crystallinity, has an average particle diameter of about 3 mum, a relatively large specificsurface area, a relatively narrow band gap and relatively high photocatalytic activity, and is excellent in photocatalytic performance of photocatalytic degradation of organic pollutants, in particularly benzidine.

Description

technical field [0001] The invention belongs to the technical field of photocatalysis of inorganic materials, and in particular relates to a microspherical ZnO-BiOI composite material and a preparation method and application thereof. Background technique [0002] Due to the rapid advancement of industrialization, waste gas, organic pollutants and other refractory substances have caused serious damage to the environment and endangered the health of humans and other organisms. Among them, the shortage of clean fresh water resources is also becoming more and more serious with the increasing water pollution. [0003] Semiconductor photocatalysis technology is a green, energy-saving and efficient, avant-garde new sewage treatment technology. Due to a series of advantages such as low price, good plasticity and wide application, zinc oxide has attracted widespread attention. However, zinc oxide, as a semiconductor material, has a large band gap, the band gap at room temperature i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/138B01J35/10B01J37/03C02F1/30C02F101/38
CPCB01J27/138B01J35/004B01J35/006B01J35/1014B01J37/031C02F1/30C02F2101/38C02F2305/10
Inventor 王林山杨竹苇张晶晶
Owner NORTHEASTERN UNIV
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