CN116351383B - Preparation and application of graphite carbon nitride/titanate nanocomposite adsorption material - Google Patents

Preparation and application of graphite carbon nitride/titanate nanocomposite adsorption material Download PDF

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CN116351383B
CN116351383B CN202310523101.6A CN202310523101A CN116351383B CN 116351383 B CN116351383 B CN 116351383B CN 202310523101 A CN202310523101 A CN 202310523101A CN 116351383 B CN116351383 B CN 116351383B
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carbon nitride
graphite carbon
titanate
adsorption material
nanocomposite
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CN116351383A (en
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马骏
郝晨丽
李康宁
马静慧
秦荔妍
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Taiyuan University of Science and Technology
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Abstract

The invention discloses preparation and application of a graphite carbon nitride/titanate nanocomposite adsorption material, and belongs to the technical field of preparation of semiconductor photocatalytic materials. Aiming at the problems of low photocatalytic performance caused by the defects of wider forbidden band, high coincidence rate of photons and holes and the like of the traditional photocatalytic material, the graphite carbon nitride/titanic acid nanotube composite material prepared by the two-step synthesis of a high-temperature polycondensation method and a hydrothermal method effectively improves the photocatalytic activity of titanium dioxide compared with other traditional photocatalytic materials; and secondly, the multi-layer structure of the material has larger specific surface area, is favorable for exposing more photocatalytic active sites and adsorbing more organic pollutants such as Methylene Blue (MB) in aqueous solution, has higher activity in the aspect of photocatalytic degradation of the Methylene Blue (MB), and has potential application prospect in the field of sewage treatment.

Description

Preparation and application of graphite carbon nitride/titanate nanocomposite adsorption material
Technical Field
The invention belongs to the technical field of preparation of semiconductor photocatalytic materials, and particularly relates to preparation and application of a graphite carbon nitride/titanate nanocomposite adsorption material.
Background
Methylene Blue (MB) is an organic dye widely used in the textile industry and is also an important organic contaminant in the environment, and how to treat Methylene Blue (MB) retained in the environment has become an increasing concern.
In recent years, a semiconductor photocatalysis technology is taken as an emerging technology, a method for degrading methylene blue through photocatalysis in the environmental field is widely applied, the core of the photocatalysis is a photocatalysis material, however, the conventional photocatalysis material commonly used has the defects of wider forbidden band, high coincidence rate of photons and holes and the like, so that the photocatalysis material is limited in photocatalysis. Therefore, how to design and synthesize a high-efficiency photocatalyst to further improve the photocatalytic performance has important research significance.
Disclosure of Invention
Aiming at the problem of low photocatalytic performance caused by the defects of wider forbidden band, high coincidence rate of photons and holes and the like of the traditional photocatalytic material, the invention provides a graphite carbon nitride/titanate nanocomposite adsorption material and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The preparation method of the graphite carbon nitride/titanate nanocomposite adsorption material comprises the following steps:
Step 1, heating urea to 500 ℃ at a heating rate of 2 ℃/min under a weak oxygen environment, maintaining the temperature for 2 hours, then heating to 520 ℃ again, maintaining the temperature for 2 hours, cooling to room temperature, and grinding to obtain pale yellow powder g-C 3N4 blocks (CNB);
Step 2, fully contacting pale yellow powder g-C 3N4 blocks with oxygen, heating to 520 ℃ at a heating rate of 2 ℃/min, then maintaining for 2 hours, cooling to room temperature, grinding, and collecting to obtain white flocculent g-C 3N4 sheets (CNS);
Dispersing TiO 2 in NaOH solution, adding g-C 3N4 tablets, performing ultrasonic dispersion for 30min, magnetically stirring for 5h, fully mixing, and transferring the mixture into a reaction kettle with polytetrafluoroethylene lining for hydrothermal reaction; and then filtering and washing the reactant with deionized water to neutrality, and drying to obtain the graphite carbon nitride/titanate nano composite adsorption material (g-C 3N4/TNTs).
Further, the mass ratio of urea to pale yellow powder g-C 3N4 blocks in the step 1 is 20:1.
Further, the dosage ratio of TiO 2 to NaOH in step 2 is 0.1g:66mL.
Further, the dosage ratio of TiO 2 to g-C 3N4 sheets in the step 3 is 1:6.
Further, the concentration of the NaOH solution in the step 3 is 10mol/L.
Further, the hydrothermal reaction condition in the step 3 is that the reaction is carried out for 72 hours at the temperature of 130 ℃.
Further, the drying condition in the step 3 is specifically that the drying is performed at 80 ℃ for 8 hours.
Further, the mass ratio of the graphite carbon nitride to the titanate in the graphite carbon nitride/titanate nano composite adsorption material is 6:1.
The photocatalytic material is in a multi-layer sheet shape, the sheets are corroded to form holes with different sizes, and TNTs nano particles in irregular spherical shapes are wrapped around the sheet graphite carbon nitride.
The graphite carbon nitride/titanate nano composite adsorbing material prepared by the preparation method of the graphite carbon nitride/titanate nano composite adsorbing material is used for photocatalytic degradation of photocatalytic methylene blue.
Compared with the prior art, the invention has the following advantages:
Compared with other traditional photocatalysis materials, the graphite carbon nitride/titanic acid nanotube composite material prepared by the invention effectively improves the photocatalysis activity of titanium dioxide; and secondly, the multi-layer structure of the material has larger specific surface area, is favorable for exposing more photocatalytic active sites and adsorbing more organic pollutants such as Methylene Blue (MB) in aqueous solution, has higher activity in the aspect of photocatalytic degradation of the Methylene Blue (MB), and has potential application prospect in the field of sewage treatment.
Drawings
FIG. 1 is a flow chart of the preparation of example 1;
FIG. 2 is an SEM image of a graphitic carbon nitride/titanate nanotube composite material prepared in example 1;
FIG. 3 is a TEM image of the graphite carbon nitride/titanate nanotube composite material prepared in example 1;
FIG. 4 is a graph showing MB degradation rates of the composite materials prepared in experimental examples 1 to 3 and comparative examples 1 and 2.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples, which are only for illustrating the present invention and not for limiting the scope of applicability of the present invention.
Example 1
And 1, accurately weighing 10g of urea in a 25mL alumina crucible with a cover, transferring the urea into a muffle furnace, heating to 500 ℃ at a heating rate of 2 ℃/min under a weak oxygen environment, maintaining the temperature for 2h, and then heating to 520 ℃ again and maintaining the temperature for 2h. After cooling to room temperature, milling to give g-C 3N4 pieces (CNB) as pale yellow powder for use.
And 2, taking 0.5g of standby yellow powder, uniformly spreading the powder in a 300mL aluminum oxide crucible in a net shape to ensure sufficient contact with oxygen, and heating to 520 ℃ at a heating rate of 2 ℃/min to maintain the temperature for 2h. Cooled to room temperature, milled and collected to obtain white flocculent g-C 3N4 tablets (CNS) for later use.
Step 3, dispersing 0.1g of TiO 2 in 66mL of 10mol/LNaOH solution, adding 0.8gg-C 3N4, performing ultrasonic dispersion for 30 minutes, magnetically stirring for 5 hours, fully mixing, transferring the mixture into a 50mL reaction kettle lined with polytetrafluoroethylene, and performing hydrothermal reaction at 130 ℃ for 72 hours. And then filtering and washing the reactant with deionized water to neutrality, and drying to obtain g-C 3N4/TNTs.
Example 2
And 1, accurately weighing 10g of urea in a 25mL alumina crucible with a cover, transferring the urea into a muffle furnace, heating to 500 ℃ at a heating rate of 2 ℃/min under a weak oxygen environment, maintaining the temperature for 2h, and then heating to 520 ℃ again and maintaining the temperature for 2h. After cooling to room temperature, milling to give g-C 3N4 pieces (CNB) as pale yellow powder for use.
And 2, taking 0.5g of standby yellow powder, uniformly spreading the powder in a 300mL aluminum oxide crucible in a net shape to ensure sufficient contact with oxygen, and heating to 520 ℃ at a heating rate of 2 ℃/min to maintain the temperature for 2h. Cooled to room temperature, milled and collected to obtain white flocculent g-C 3N4 tablets (CNS) for later use.
Step 3, dispersing 0.1g of TiO 2 in 66mL of 10mol/LNaOH solution, adding 0.6gg-C 3N4, performing ultrasonic dispersion for 30 minutes, magnetically stirring for 5 hours, fully mixing, transferring the mixture into a 50mL reaction kettle lined with polytetrafluoroethylene, and performing hydrothermal reaction at 130 ℃ for 72 hours. And then filtering and washing the reactant with deionized water to neutrality, and drying to obtain g-C 3N4/TNTs.
Example 3
And 1, accurately weighing 10g of urea in a 25mL alumina crucible with a cover, transferring the urea into a muffle furnace, heating to 500 ℃ at a heating rate of 2 ℃/min under a weak oxygen environment, maintaining the temperature for 2h, and then heating to 520 ℃ again and maintaining the temperature for 2h. After cooling to room temperature, milling to give g-C 3N4 pieces (CNB) as pale yellow powder for use.
And 2, taking 0.5g of standby yellow powder, uniformly spreading the powder in a 300mL aluminum oxide crucible in a net shape to ensure sufficient contact with oxygen, and heating to 520 ℃ at a heating rate of 2 ℃/min to maintain the temperature for 2h. Cooled to room temperature, milled and collected to obtain white flocculent g-C 3N4 tablets (CNS) for later use.
Step 3, dispersing 0.1g of TiO 2 in 66mL of 10mol/LNaOH solution, adding 0.3gg-C 3N4, performing ultrasonic dispersion for 30 minutes, magnetically stirring for 5 hours, fully mixing, transferring the mixture into a 50mL reaction kettle lined with polytetrafluoroethylene, and performing hydrothermal reaction at 130 ℃ for 72 hours. And then filtering and washing the reactant with deionized water to neutrality, and drying to obtain g-C 3N4/TNTs.
Comparative example 1
And 1, accurately weighing 10g of urea in a 25mL alumina crucible with a cover, transferring the urea into a muffle furnace, heating to 500 ℃ at a heating rate of 2 ℃/min under a weak oxygen environment, maintaining the temperature for 2h, and then heating to 520 ℃ again and maintaining the temperature for 2h. After cooling to room temperature, milling to give g-C 3N4 pieces (CNB) as pale yellow powder for use.
And 2, taking 0.5g of standby yellow powder, uniformly spreading the powder in a 300mL aluminum oxide crucible in a net shape to ensure sufficient contact with oxygen, and heating to 520 ℃ at a heating rate of 2 ℃/min to maintain the temperature for 2h. Cooled to room temperature, milled and collected to obtain white flocculent g-C 3N4 tablets (CNS) for later use.
Comparative example 2
Pure titanium dioxide P25.
Experiment of Material application
The composite materials prepared in examples 1 to 3 and the graphite carbon nitride of comparative example 1 and the titanium dioxide P25 of comparative example 2 were each subjected to degradation effect detection of methylene blue.
The detection method specifically comprises the following steps:
1. Dispersing 10mg of sample in 100mL MB solution with the concentration of 50mg/L, and placing the sample in a photocatalytic reactor;
2. Firstly, stirring for 30min in dark or shading environment by ultrasonic, allowing the mixed solution to reach adsorption balance among the photocatalyst, MB and water, then adopting a xenon lamp with the distance of 300W as a visible light source to irradiate at the position 11cm away from the reaction solution, triggering the photocatalytic reaction, and simultaneously introducing circulating water for cooling;
3. Filtering all ultraviolet light with wavelength less than 420nm with ultraviolet filter, measuring MB absorbance with ultraviolet-visible spectrophotometer (SP-756, shanghai spectrometer Co., ltd.), and obtaining corresponding concentration according to standard curve;
4. The pipette samples at intervals during the irradiation of visible light, the absorbance of the reaction solution is measured after centrifugation, and the degradation efficiency of MB is calculated, and the result is shown in FIG. 4. As can be seen from FIG. 4, the degradation efficiency of the 6:1 graphite carbon nitride/titanate nanocomposite adsorption material prepared by the invention on MB is highest; whereas the degradation efficiency of MB in example 1 and example 3 was relatively low, the degradation efficiency of MB in the materials prepared in comparative examples 1 and 2 was the lowest. The photocatalytic activity of the 6:1 graphite carbon nitride/titanate nano composite adsorption material is obviously improved, the degradation rate is twice as high as that of the raw material, and the optimal photocatalytic performance is shown.
What is not described in detail in the present specification belongs to the prior art known to those skilled in the art. While the foregoing describes illustrative embodiments of the present invention to facilitate an understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, but is to be construed as protected by the accompanying claims insofar as various changes are within the spirit and scope of the present invention as defined and defined by the appended claims.

Claims (10)

1. A preparation method of a graphite carbon nitride/titanate nanocomposite adsorption material is characterized by comprising the following steps: the method comprises the following steps:
Step 1, heating urea to 500 ℃ at a heating rate of 2 ℃/min under a weak oxygen environment, keeping the temperature at 2h ℃, then heating to 520 ℃ again, keeping the temperature for 2 hours, cooling to room temperature, and grinding to obtain pale yellow powder g-C 3N4 blocks;
Step2, fully contacting pale yellow powder g-C 3N4 blocks with oxygen, keeping 2h after the temperature is raised to 520 ℃ at a heating rate of 2 ℃/min, cooling to room temperature, grinding, and collecting to obtain white flocculent g-C 3N4 sheets;
Dispersing TiO 2 in NaOH solution, adding g-C 3N4 tablets, performing ultrasonic dispersion on the mixture for 30 min, performing magnetic stirring on the mixture for 5h, and then transferring the mixture into a reaction kettle with a polytetrafluoroethylene lining for hydrothermal reaction; and then filtering and washing the reactant with deionized water to neutrality, and drying to obtain the graphite carbon nitride/titanate nanocomposite.
2. The method for preparing the graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1, wherein the method comprises the following steps: the mass ratio of urea to pale yellow powder g-C 3N4 blocks in the step 1 is 20:1.
3. The method for preparing the graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1, wherein the method comprises the following steps: the dosage ratio of TiO 2 to NaOH in the step 3 is 0.1 g:66 mL.
4. The method for preparing the graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1, wherein the method comprises the following steps: the dosage ratio of TiO 2 to g-C 3N4 tablets in the step 3 is 1:6.
5. The method for preparing the graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1, wherein the method comprises the following steps: the concentration of the NaOH solution in the step 3 is 10 mol/L.
6. The method for preparing the graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1, wherein the method comprises the following steps: the hydrothermal reaction condition in the step 3 is that the reaction is carried out at the temperature of 130 ℃ and 72 h.
7. The method for preparing the graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1, wherein the method comprises the following steps: the drying condition in the step 3 is specifically that 8h is dried at 80 ℃.
8. The method for preparing the graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1, wherein the method comprises the following steps: the mass ratio of the graphite carbon nitride to the titanate in the graphite carbon nitride/titanate nanocomposite is 6:1.
9. The graphite carbon nitride/titanate nanocomposite obtained by the method for producing a graphite carbon nitride/titanate nanocomposite adsorbent according to claim 1, characterized in that: the nano composite material is in a multi-layer sheet shape, the sheet is corroded to have holes with different sizes, and irregular spherical TNTs nano particles are wrapped around the graphite flake carbon nitride.
10. The use of a graphite carbon nitride/titanate nanocomposite prepared by the method for preparing a graphite carbon nitride/titanate nanocomposite adsorption material according to claim 1 in photocatalytic degradation of photocatalytic methylene blue.
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