Preparation method of titanium dioxide multilevel structure hollow microsphere material

Abstract

The invention relates to a preparation method of a titanium dioxide multilevel structure hollow microsphere material, which comprises the following steps: uniformly stirring and mixing polyethylene glycol, tetrahydrofuran, hydrochloric acid, glacial acetic acid, hydrofluoric acid and butyl titanate; and then transferring into a polytetrafluoroethylene lining of a stainless steel high-pressure kettle, carrying out constant-temperature reaction, cooling, centrifuging, washing and drying to obtain the titanium dioxide hollow microsphere material with the multilevel structure. A one-pot discharging method is adopted, the preparation process is simple, and the obtained multilevel structure material has good photocatalytic degradation capacity.

Description

Technical Field

[0001] The invention relates to a method for preparing a novel catalytic material, in particular to a method for preparing a titanium dioxide multi-level structure hollow microsphere material. Background Art

[0002] Since titanium dioxide has a wide band gap and absorbs large photon energy, about 3.2 eV, it has a better catalytic effect under ultraviolet light, but a poorer catalytic effect under visible light, and a weaker photocatalytic ability under sunlight. At present, some methods for preparing catalysts by modifying titanium dioxide to improve the catalytic effect under visible light have been reported, but the effect is not ideal and the process is relatively complicated. The present invention aims to provide a multi-level structure material composed of nanosheets assembled into microspheres, which can be applied to the fields of photocatalytic degradation of organic pollutants for water pollution prevention and control, industrial catalytic hydrogenation, chemical catalytic oxidation materials, functional materials, etc. Summary of the invention

[0003] The present invention provides a method for preparing a titanium dioxide multi-level structure hollow microsphere material, which has a strong catalytic effect. The technical solution adopted by the present invention to solve the technical problem is: Polyethylene glycol, tetrahydrofuran, hydrochloric acid, glacial acetic acid, hydrofluoric acid and butyl titanate are stirred and mixed evenly, and then transferred to the polytetrafluoroethylene lining of a stainless steel high-pressure reactor, reacted at a constant temperature, cooled, centrifuged, washed and dried to obtain a titanium dioxide multi-level structure hollow microsphere material.

[0004] Photocatalytic test of catalyst: take 20 mg of multi-level structure material, add 25 mL of 10 mg / L rhodamine B, illuminate under 48 W ultraviolet lamp for 1 hour, measure the absorbance A, substitute it into the regression equation of the standard curve, calculate the concentration c, and calculate the degradation rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0005] Figure 1 and Figure 2 This is the SEM photo of titanium dioxide hierarchical structure hollow microsphere material.

[0006] Depend on Figure 1 It can be clearly seen that the microsphere material is assembled from many nanosheets, indicating that the method of the present invention can prepare nanosheet / microsphere multi-level structure materials.

[0007] The nanosheets are nearly square, with a side length of 60~200nm and a thickness of 10~30nm, and the diameter of the microspheres is 0.5~2μm.

[0008] Depend on Figure 2 It can be seen that the microspheres have a hollow structure. DETAILED DESCRIPTION

[0009] In order to make the contents of the present invention easier to understand, the technical solution of the present invention is further described below in conjunction with specific implementation methods, but the present invention is not limited thereto. Embodiment 1

[0010] Weigh 1.5 g of polyethylene glycol, put it into a beaker, add 30 mL of tetrahydrofuran, 2 mL of concentrated hydrochloric acid, and 2.8 mL of glacial acetic acid, and stir to mix well.

[0011] Continue to add 3.6 mL of butyl titanate and 0.6 mL of hydrofluoric acid and stir evenly.

[0012] The solution was transferred to the polytetrafluoroethylene liner of the reactor, kept at a constant temperature of 170°C, and reacted for 12 hours.

[0013] After the reaction, the product is centrifuged, the precipitate is washed with anhydrous ethanol and deionized water respectively, and dried to obtain a titanium dioxide multi-level structure hollow microsphere material.

[0014] Photocatalytic test of the catalyst: Take 20 mg of the multi-stage material, add 25 mL of a 10 mg / L rhodamine B solution, and irradiate under a 48-watt ultraviolet lamp for 1 hour. The degradation rate is: 58.5%. Embodiment 2

[0015] Weigh 0.5 g of polyethylene glycol, put it into a beaker, add 30 mL of tetrahydrofuran, 2 mL of concentrated hydrochloric acid, and 3 mL of glacial acetic acid, and stir to mix well.

[0016] Continue to add 3.6 mL of butyl titanate and 0.6 mL of hydrofluoric acid and stir evenly.

[0017] The solution was transferred to the polytetrafluoroethylene liner of the reactor, kept at a constant temperature of 180°C, and reacted for 6 hours.

[0018] After the reaction, the product is centrifuged, the precipitate is washed with anhydrous ethanol and deionized water respectively, and dried to obtain a titanium dioxide multi-level structure hollow microsphere material.

[0019] Photocatalytic test of the catalyst: Take 20 mg of the multi-stage material, add 25 mL of a 10 mg / L rhodamine B solution, and irradiate under a 48-watt ultraviolet lamp for 1 hour. The degradation rate is: 48.2%. Embodiment 3

[0020] Weigh 1.0 g of polyethylene glycol, put it into a beaker, add 30 mL of tetrahydrofuran, 1 mL of concentrated hydrochloric acid, 2.5 mL of glacial acetic acid, 3.6 mL of butyl titanate, and 0.5 mL of hydrofluoric acid, and stir evenly.

[0021] The solution was transferred to the polytetrafluoroethylene liner of the reactor, kept at a constant temperature of 140°C, and reacted for 24 hours.

[0022] After the reaction, the product is centrifuged, the precipitate is washed with anhydrous ethanol and deionized water respectively, and dried to obtain a titanium dioxide multi-level structure hollow microsphere material.

[0023] Photocatalytic test of the catalyst: Take 20 mg of the multi-stage material, add 25 mL of a 10 mg / L rhodamine B solution, and irradiate under a 48-watt ultraviolet lamp for 1 hour. The degradation rate is: 53.1%.

Claims

1. A method for preparing a titanium dioxide multi-level structure hollow microsphere material, characterized in that: The preparation method comprises the following steps of mixing polyethylene glycol, tetrahydrofuran, hydrochloric acid, glacial acetic acid, hydrofluoric acid and butyl titanate uniformly, and then transferring the reaction solution to the polytetrafluoroethylene lining of a stainless steel autoclave, reacting at a constant temperature, and cooling naturally to room temperature. Centrifugation, washing and drying are performed to obtain titanium dioxide multi-level structure microsphere material.

2. The method for preparing a titanium dioxide multi-level structure hollow microsphere material according to claim 1, characterized in that: The mass ratio of polyethylene glycol to tetrahydrofuran is 1-5%.

3. The method for preparing a titanium dioxide multi-level structure hollow microsphere material according to claim 1, characterized in that: The amount of hydrofluoric acid used is 5% to 25% of the volume of tetrabutyl titanate.

4. The method for preparing a titanium dioxide multi-level structure hollow microsphere material according to claim 1, characterized in that: The amount of hydrochloric acid used is 10% to 70% of the volume of tetrabutyl titanate.

5. The method for preparing a titanium dioxide multi-level structure hollow microsphere material according to claim 1, characterized in that: The amount of glacial acetic acid used is 10% to 100% of the volume of tetrabutyl titanate.

6. A method for preparing a titanium dioxide multi-level structure hollow microsphere material according to claims 1-6, characterized in that: The reaction temperature is 120℃~200℃.

7. A method for preparing a titanium dioxide multi-level structure hollow microsphere material according to claims 1-6, characterized in that: The constant temperature reaction time is 1 hour to 24 hours.

8. A titanium dioxide multi-level structure hollow microsphere material obtained by the method as claimed in claim 1, which is a multi-level structure material in which nanosheets are assembled into microspheres.

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