CN116282159A - Mesoporous Nb with large aperture 2 O 5 Photocatalytic material, preparation method and application thereof - Google Patents

Mesoporous Nb with large aperture 2 O 5 Photocatalytic material, preparation method and application thereof Download PDF

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CN116282159A
CN116282159A CN202310206640.7A CN202310206640A CN116282159A CN 116282159 A CN116282159 A CN 116282159A CN 202310206640 A CN202310206640 A CN 202310206640A CN 116282159 A CN116282159 A CN 116282159A
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photocatalytic material
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郭盛祺
靳凤先
沈伯雄
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Hebei University of Technology
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Abstract

The invention relates to the technical field of photocatalytic materials, in particular to a large-aperture mesoporous Nb 2 O 5 The invention uses Cetyl Trimethyl Ammonium Bromide (CTAB) as a surfactant, and adopts a hydrothermal method to prepare mesoporous Nb with large aperture 2 O 5 The photocatalytic material greatly improves the adsorption performance of the photocatalytic material and exposes more photocatalytic reaction active sites; the preparation method is simple and feasible, the production cost is low, and the obtained photocatalytic material has excellent photocatalytic performance. The photocatalyst provided by the invention can degrade organic dye in water, has a good degradation effect and has good practicability.

Description

Mesoporous Nb with large aperture 2 O 5 Photocatalytic material, preparation method and application thereof
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to a large-aperture mesoporous Nb 2 O 5 Photocatalytic material, preparation method and application thereof.
Background
With the development of society, the use of a large amount of fossil fuel causes a series of problems such as energy shortage, environmental pollution and the like, which seriously jeopardize the life of people. At present, the photocatalysis technology is widely applied to the fields of environmental management, energy conversion and the like as a green pollution-free environment-friendly technology so as to ensure clean and renewable energy supply and reduce harmful environmental impact related to fossil fuel consumption.
As a central link of the photocatalytic technology, a number of materials useful in the field of photocatalysis have been reported in recent years, wherein Nb 2 O 5 Photocatalytic materials are widely focused by people due to their remarkable properties of good thermodynamic stability, non-toxicity, good acid corrosion resistance (except sulfuric acid and hydrofluoric acid), and the like.
Although Nb 2 O 5 There are unique advantages as photocatalytic materials, but there are a number of drawbacks that affect their photocatalytic performance. Wherein, the adsorption capacity of the photocatalyst to the reaction substance also affects the photocatalytic effect. Therefore, how to provide a simple means to improve the structure of the photocatalyst so as to expose more photocatalytic reaction active sites to enhance the adsorption of pollutants by the catalytic material has important scientific and practical significance for improving the photocatalytic performance of the photocatalytic material.
In view of the above drawbacks, the present inventors have finally achieved the present invention through long-time studies and practices.
Disclosure of Invention
The invention aims to solve the problem of how to provide a simple means, improve the structure of a photocatalyst to expose more photocatalytic reaction active sites to enhance the adsorption of pollutants by a catalytic material, and provides a mesoporous Nb with large aperture 2 O 5 Photocatalytic material, preparation method and application thereof.
In order to achieve the above object, the present invention discloses a large apertureMesoporous Nb of (2) 2 O 5 The preparation method of the photocatalytic material comprises the following steps:
s1, dissolving hexadecyl trimethyl ammonium bromide in ethanol, and stirring to form a uniform solution;
s2, nbCl 5 Adding the mixture into the solution obtained in the step S1, and stirring until the mixture is completely dissolved;
s3, slowly dripping ammonia water solution into the mixed solution obtained in the step S2 to form suspension, and stirring for 1-3 h at room temperature;
s4, centrifuging the suspension obtained in the step S3, discarding supernatant, uniformly dispersing the precipitate in deionized water, and performing hydrothermal reaction;
and S5, centrifuging the product obtained in the step S4, washing with deionized water and absolute ethyl alcohol in sequence, and drying.
The addition amount of the hexadecyl trimethyl ammonium bromide in the step S1 is 0.005 g-0.03 g.
The volume fraction of the ammonia water solution in the step S3 is 2-8wt%.
The hydrothermal reaction temperature in the step S4 is 120-200 ℃.
And the hydrothermal reaction time in the step S4 is 12-36 h.
In the step S5, the reaction product is washed for 2-4 times by using deionized water, and then is washed for 2-4 times by using absolute ethyl alcohol.
The drying temperature in the step S5 is 60-80 ℃.
And in the step S5, the drying time is 6-12 hours.
The invention also discloses a large-aperture mesoporous Nb prepared by the preparation method 2 O 5 Photocatalytic material and mesoporous Nb with large aperture 2 O 5 The application of the photocatalytic material in photocatalytic degradation of rhodamine B solution.
Compared with the prior art, the invention has the beneficial effects that: the invention uses Cetyl Trimethyl Ammonium Bromide (CTAB) as a surfactant, and adopts a hydrothermal method to prepare mesoporous Nb with large aperture 2 O 5 Photocatalytic material, greatly improving the adsorptivity of the photocatalytic materialCan expose more photocatalytic reaction active sites; the preparation method is simple and feasible, the production cost is low, and the obtained photocatalytic material has excellent photocatalytic performance.
Drawings
FIG. 1 is an XRD pattern of the photocatalytic material in examples 1 to 3 and comparative examples 1 to 7, in which FIG. 1 is C5-Nb prepared in example 1 2 O 5 Photocatalytic material, 2 is C10-Nb prepared in example 2 2 O 5 Photocatalytic material, 3 is C20-Nb prepared in example 3 2 O 5 Photocatalytic material, 4 is S5-Nb prepared in comparative example 1 2 O 5 Photocatalytic material 5 is S10-Nb prepared in comparative example 2 2 O 5 Photocatalytic material 6 is S20-Nb prepared in comparative example 3 2 O 5 Photocatalytic material 7 is P5-Nb prepared in comparative example 4 2 O 5 Photocatalytic material 8 is P10-Nb prepared in comparative example 5 2 O 5 Photocatalytic material 9 is P20-Nb prepared in comparative example 6 2 O 5 Photocatalytic material, 10 is Nb prepared in comparative example 7 2 O 5 A photocatalytic material;
FIG. 2 is N 2 Adsorption-desorption isotherms, in which 1 is the photocatalytic material prepared in example 2 and 2 is the photocatalytic material prepared in comparative example 7;
FIG. 3 is a graph showing pore size distribution, wherein 1 is the photocatalytic material prepared in example 2, and 2 is the photocatalytic material prepared in comparative example 7;
FIG. 4 is a graph showing degradation of rhodamine B by different photocatalytic materials prepared according to the change of the irradiation time, wherein 1 is C5-Nb prepared in example 1 2 O 5 Photocatalytic material, 2 is C10-Nb prepared in example 2 2 O 5 Photocatalytic material, 3 is C20-Nb prepared in example 3 2 O 5 Photocatalytic material, 4 is S5-Nb prepared in comparative example 1 2 O 5 Photocatalytic material 5 is S10-Nb prepared in comparative example 2 2 O 5 Photocatalytic material 6 is S20-Nb prepared in comparative example 3 2 O 5 Photocatalytic material 7 is P5-Nb prepared in comparative example 4 2 O 5 Photocatalytic material 8 is comparative example 5P10-Nb prepared in (3) 2 O 5 Photocatalytic material 9 is P20-Nb prepared in comparative example 6 2 O 5 Photocatalytic material, 10 is Nb prepared in comparative example 7 2 O 5 Photocatalytic material.
FIG. 5 is a graph showing the degradation of rhodamine B by photocatalytic materials prepared at different hydrothermal reaction temperatures with time of illumination, wherein FIG. 1 is a graph showing the degradation of 120-C10-Nb prepared in example 4 2 O 5 Photocatalytic material, 2 is 140-C10-Nb prepared in example 5 2 O 5 Photocatalytic material, 3 is 160-C10-Nb prepared in example 6 2 O 5 Photocatalytic material, 4 is C5-Nb prepared in example 2 2 O 5 Photocatalytic material 5 is 200-C10-Nb prepared in example 7 2 O 5 Photocatalytic material.
FIG. 6 is a graph showing the degradation of rhodamine B by photocatalytic materials prepared at different hydrothermal reaction times, with time of illumination, wherein FIG. 1 is C10-Nb prepared in example 8 2 O 5 -12 photocatalytic material, 2 is C10-Nb prepared in example 9 2 O 5 -18 photocatalytic material, 3 is C10-Nb prepared in example 2 2 O 5 Photocatalytic material, 4 is C5-Nb prepared in example 10 2 O 5 -30 photocatalytic material, 5 is C10-Nb prepared in example 11 2 O 5 -36 photocatalytic material.
Detailed Description
The above and further technical features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
Example 1
Mesoporous Nb with large aperture 2 O 5 A method of preparing a photocatalytic material comprising the steps of:
step 1: 0.005g cetyltrimethylammonium bromide (CTAB) was dissolved in 5mL ethanol and stirred to form a homogeneous solution;
step 2: 0.5g NbCl 5 Adding the mixture into the solution obtained in the step 1, and stirring until the mixture is completely dissolved;
step 3: slowly dripping 25mL of ammonia water solution with the volume fraction of 4wt% into the mixed solution obtained in the step 2 to form a suspension, and stirring for 2h at room temperature;
step 4: centrifuging the suspension obtained in the step 3, discarding the supernatant, taking the precipitate, uniformly dispersing in 25mL of deionized water, placing in a 50mL reaction kettle, and heating for 24 hours at 180 ℃ in a blast drying oven;
step 5: and (3) centrifuging the product obtained in the step (4), washing with deionized water and absolute ethyl alcohol for 3 times in sequence, and drying for 6 hours in a vacuum environment at 60 ℃.
Cx-Nb for the prepared sample 2 O 5 And represents the content of the added surfactant. In this example, x is 5mg, i.e., the product obtained in this example is expressed as C5-Nb 2 O 5 。
Example 2
The difference between this embodiment and embodiment 1 is that: in step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) was added to 5mL of ethanol and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this example is expressed as C10-Nb 2 O 5 。
Example 3
The difference between this embodiment and embodiment 1 is that: in step 1, 0.02g of cetyltrimethylammonium bromide (CTAB) was added and dissolved in 5mL of ethanol and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this example is expressed as C20-Nb 2 O 5 。
Example 4
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 120 ℃ for 24 hours. The remaining steps and parameters were the same as in example 1. The product obtained in this example is denoted 120-C10-Nb2O5.
Example 5
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 140 ℃ for 24 hours. The remaining steps and parameters were the same as in example 1. The product obtained in this example is designated 140-C10-Nb2O5.
Example 6
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 160 ℃ for 24 hours. The remaining steps and parameters were the same as in example 1. The product obtained in this example is denoted 160-C10-Nb2O5.
Example 7
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 200 ℃ for 24 hours. The remaining steps and parameters were the same as in example 1. The product obtained in this example is denoted 200-C10-Nb2O5.
Example 8
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 180 ℃ for 12 hours. The remaining steps and parameters were the same as in example 1. The product obtained in this example is designated C10-Nb2O5-12.
Example 9
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 180 ℃ for 18h. The remaining steps and parameters were the same as in example 1. The product obtained in this example is designated C10-Nb2O5-18.
Example 10
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 180 ℃ for 30 hours. The remaining steps and parameters were the same as in example 1. The product obtained in this example is designated C10-Nb2O5-30.
Example 11
The difference between this embodiment and embodiment 1 is that: in the step 1, 0.01g of cetyltrimethylammonium bromide (CTAB) is added into 5mL of ethanol and stirred to form a uniform solution; in step 4, heating is carried out in a forced air drying oven at 180 ℃ for 36h. The remaining steps and parameters were the same as in example 1. The product obtained in this example is designated C10-Nb2O5-36.
Comparative example 1
The difference between this comparative example and example 1 is that: in step 1, sodium Dodecyl Sulfate (SDS) was dissolved in 5mL of ethanol without adding cetyltrimethylammonium bromide (CTAB) as a surfactant, and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this comparative example is expressed as S5-Nb 2 O 5 。
Comparative example 2
The difference between this comparative example and example 1 is that: in step 1, not 0.005g of cetyltrimethylammonium bromide (CTAB) was added as a surfactant, but 0.01g of Sodium Dodecyl Sulfate (SDS) was dissolved in 5mL of ethanol, and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this comparative example is expressed as S10-Nb 2 O 5 。
Comparative example 3
The difference between this comparative example and example 1 is that: in step 1, not 0.005g of cetyltrimethylammonium bromide (CTAB) was added as a surfactant, but 0.02g of Sodium Dodecyl Sulfate (SDS) was dissolved in 5mL of ethanol, and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this comparative example is expressed as S20-Nb 2 O 5 。
Comparative example 4
The difference between this comparative example and example 1 is that: in step 1, instead of cetyl trimethylammonium bromide (CTAB) as a surfactant, an equal amount of polyvinylpyrrolidone (PVP) was dissolved in 5mL of ethanol and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this comparative example is expressed as P5-Nb 2 O 5 。
Comparative example 5
The difference between this comparative example and example 1 is that: in step 1, 0.0 is not added05g cetyl trimethylammonium bromide (CTAB) as surfactant, instead 0.01g polyvinylpyrrolidone (PVP) was dissolved in 5mL ethanol and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this comparative example is expressed as P10-Nb 2 O 5 。
Comparative example 6
The difference between this comparative example and example 1 is that: in step 1, instead of cetyl trimethylammonium bromide (CTAB) as a surfactant, 0.02g of polyvinylpyrrolidone (PVP) was dissolved in 5mL of ethanol and stirred to form a homogeneous solution. The remaining steps and parameters were the same as in example 1. The product obtained in this comparative example is expressed as P20-Nb 2 O 5 。
Comparative example 7
The difference between this comparative example and example 1 is that: no cetyltrimethylammonium bromide (CTAB) was added in step 1. The remaining steps and parameters were the same as in example 1. Since the comparative example contains no surfactant during the preparation, nb is used 2 O 5 And (3) representing.
FIG. 1 is an XRD pattern, in which FIG. 1 is C5-Nb prepared in example 1 2 O 5 Photocatalytic material, 2 is C10-Nb prepared in example 2 2 O 5 Photocatalytic material, 3 is C20-Nb prepared in example 3 2 O 5 Photocatalytic material, 4 is S5-Nb prepared in comparative example 1 2 O 5 Photocatalytic material 5 is S10-Nb prepared in comparative example 2 2 O 5 Photocatalytic material 6 is S20-Nb prepared in comparative example 3 2 O 5 Photocatalytic material 7 is P5-Nb prepared in comparative example 4 2 O 5 Photocatalytic material 8 is P10-Nb prepared in comparative example 5 2 O 5 Photocatalytic material 9 is P20-Nb prepared in comparative example 6 2 O 5 Photocatalytic material, 10 is Nb prepared in comparative example 7 2 O 5 Photocatalytic material.
As can be seen from fig. 1, it was found that the catalysts obtained in examples 1 to 3 and comparative examples 1 to 7 showed no other impurity peaks in the XRD pattern, compared with the samples without the surfactant, after the surfactant was added, indicating that the obtained photocatalytic material maintained a uniform crystal structure, no other crystal phases were generated or other impurities were introduced.
FIG. 2 is sample N 2 Adsorption-desorption isotherms, in which 1 is the photocatalytic material prepared in example 2 and 2 is the photocatalytic material prepared in comparative example 7.
FIG. 3 is a graph showing pore size distribution of a sample, in which 1 is the photocatalytic material prepared in example 2 and 2 is the photocatalytic material prepared in comparative example 7.
As can be seen from fig. 2 and 3, at N 2 The samples prepared in example 2 and comparative example 7 both showed type IV isotherms in the adsorption-desorption isotherms, indicating that the samples obtained in example 2 and comparative example 7 both had mesoporous structures. In addition, from the pore size distribution, the sample obtained by adding cetyltrimethylammonium bromide (CTAB) in example 2 showed a significant increase in pore content between 5nm and 30nm compared to the sample in comparative example 7, indicating that the addition of cetyltrimethylammonium bromide (CTAB) contributes to the change in pore structure of the sample and thus to the generation of more active sites.
Photocatalytic degradation rhodamine B experiment:
performing a photocatalytic degradation rhodamine B experiment in a photocatalytic reaction device; the catalyst and rhodamine B solution are uniformly mixed in a reactor and react for 30min under the dark condition, after the photocatalytic material reaches adsorption-desorption equilibrium, the rhodamine B is irradiated, and no additional sacrificial agent or noble metal cocatalyst is added in the reaction process. The reaction device comprises a 300W xenon lamp light source, a magnetic stirrer, a photocatalytic quartz reactor and an ultraviolet-visible spectrophotometer.
FIG. 4 is a graph showing degradation of rhodamine B by different photocatalytic materials prepared in examples 1 to 3 and comparative examples 1 to 7 with time to light, in which FIG. 1 is C5-Nb prepared in example 1 2 O 5 Photocatalytic material, 2 is C10-Nb prepared in example 2 2 O 5 Photocatalytic material, 3 is C20-Nb prepared in example 3 2 O 5 Photocatalytic material, 4 is S5-Nb prepared in comparative example 1 2 O 5 Photocatalytic material 5 is S10-Nb prepared in comparative example 2 2 O 5 Photo-catalysisChemical materials, 6 is S20-Nb prepared in comparative example 3 2 O 5 Photocatalytic material 7 is P5-Nb prepared in comparative example 4 2 O 5 Photocatalytic material 8 is P10-Nb prepared in comparative example 5 2 O 5 Photocatalytic material 9 is P20-Nb prepared in comparative example 6 2 O 5 Photocatalytic material, 10 is Nb prepared in comparative example 7 2 O 5 Photocatalytic material. The experimental conditions are as follows: concentration of photocatalytic material: 0.2g/L; rhodamine B concentration: 10mg/L; mixing the photocatalytic material and rhodamine B, reacting for 30min under dark condition, enabling the adsorption of the photocatalytic material to the rhodamine B to reach saturation, and then reacting under illumination condition.
Photocatalytic activities of the photocatalytic materials prepared in examples 1 to 3 and comparative examples 1 to 7 were evaluated by degrading rhodamine B at an initial concentration of 10 mg/L. As can be seen from FIG. 4, after 30min of adsorption-desorption equilibrium, nb without adding the surfactant in comparative example 7 2 O 5 The adsorption efficiency of the photocatalytic material to rhodamine B is about 5%, while in other embodiments, nb is added with a surfactant 2 O 5 The adsorption efficiency of the photocatalytic material to rhodamine B is between 15 and 30 percent. After 30min of light irradiation, nb without adding surfactant 2 O 5 The degradation rate of the photocatalytic material to rhodamine can only reach 20%, and the degradation efficiency of other photocatalytic materials added with Cetyl Trimethyl Ammonium Bromide (CTAB), sodium Dodecyl Sulfate (SDS) and polyvinylpyrrolidone (PVP) to rhodamine is better than that of Nb without adding a surfactant 2 O 5 The method comprises the steps of carrying out a first treatment on the surface of the Wherein Nb with cetyltrimethylammonium bromide (CTAB) is added 2 O 5 The photocatalytic material has the best degradation performance on rhodamine B, can degrade more than 95 percent of rhodamine only for 20 minutes, and is far superior to Nb added with Sodium Dodecyl Sulfate (SDS) and polyvinylpyrrolidone (PVP) 2 O 5 Photocatalytic material.
FIG. 5 is a graph showing the degradation of rhodamine B by photocatalytic materials prepared at different hydrothermal reaction temperatures with time of illumination, wherein FIG. 1 is a graph showing the degradation of 120-C10-Nb prepared in example 4 2 O 5 Photocatalytic material, 2 is prepared in example 5140-C10-Nb of (2) 2 O 5 Photocatalytic material, 3 is 160-C10-Nb prepared in example 6 2 O 5 Photocatalytic material, 4 is C10-Nb prepared in example 2 2 O 5 Photocatalytic material 5 is 200-C10-Nb prepared in example 7 2 O 5 Photocatalytic material. The experimental conditions are as follows: concentration of photocatalytic material: 0.2g/L; rhodamine B concentration: 10mg/L; mixing the photocatalytic material and rhodamine B, reacting for 30min under dark condition, enabling the adsorption of the photocatalytic material to the rhodamine B to reach saturation, and then reacting under illumination condition.
The photocatalytic activity of the photocatalytic materials prepared in example 2 and examples 4 to 7 was evaluated by degrading rhodamine B at an initial concentration of 10 mg/L. As can be seen from FIG. 5, as the hydrothermal temperature increases, nb is produced 2 O 5 The activity of the photocatalytic material is gradually improved, the degradation efficiency of rhodamine B is gradually improved, and Nb with the best photocatalytic activity is obtained at the hydrothermal temperature of 180 DEG C 2 O 5 Photocatalytic material. At the same time, as the temperature continues to increase to 200 ℃, nb 2 O 5 The photocatalytic activity of the photocatalytic material is not greatly changed from that of the photocatalytic material obtained at 180 ℃.
FIG. 6 is a graph showing the degradation of rhodamine B by photocatalytic materials prepared at different hydrothermal reaction times, with time of illumination, wherein FIG. 1 is C10-Nb prepared in example 8 2 O 5 -12 photocatalytic material, 2 is C10-Nb prepared in example 9 2 O 5 -18 photocatalytic material, 3 is C10-Nb prepared in example 2 2 O 5 Photocatalytic material, 4 is C10-Nb prepared in example 10 2 O 5 -30 photocatalytic material, 5 is C10-Nb prepared in example 11 2 O 5 -36 photocatalytic material. The experimental conditions are as follows: concentration of photocatalytic material: 0.2g/L; rhodamine B concentration: 10mg/L; mixing the photocatalytic material and rhodamine B, reacting for 30min under dark condition, enabling the adsorption of the photocatalytic material to the rhodamine B to reach saturation, and then reacting under illumination condition.
The degradation of rhodamine B at an initial concentration of 10mg/L was evaluatedPhotocatalytic activity of the photocatalytic materials prepared in example 2 and examples 8 to 11. As can be seen from FIG. 6, as the hydrothermal time increases, nb is produced 2 O 5 The activity of the photocatalytic material is gradually improved, and Nb with the best photocatalytic activity is obtained when the hydrothermal reaction time is 24 hours 2 O 5 The degradation rate of the photocatalytic material to rhodamine B reaches 100 percent after 20 minutes. When the hydrothermal time is continuously increased to 30 hours, the degradation rate of rhodamine B is reduced to 90% within 20 minutes, and the photocatalytic efficiency of the sample obtained by the hydrothermal reaction for 36 hours is relatively similar.
From the above experimental results, compared with the surfactants such as Sodium Dodecyl Sulfate (SDS) and polyvinylpyrrolidone (PVP), the introduction of cetyltrimethylammonium bromide (CTAB) in the preparation process can effectively promote Nb 2 O 5 The generation of large-aperture mesopores in the photocatalytic material enhances the adsorption capacity of the photocatalytic material and exposes more photocatalytic reaction active sites, thereby enhancing the photocatalytic performance. Meanwhile, nb prepared by the method 2 O 5 The optimal hydrothermal reaction temperature of the photocatalytic material is 180 ℃, and the optimal hydrothermal reaction time is 24 hours.
The foregoing description of the preferred embodiment of the invention is merely illustrative of the invention and is not intended to be limiting. It will be appreciated by persons skilled in the art that many variations, modifications, and even equivalents may be made thereto without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. Mesoporous Nb with large aperture 2 O 5 The preparation method of the photocatalytic material is characterized by comprising the following steps:
s1, dissolving hexadecyl trimethyl ammonium bromide in ethanol, and stirring to form a uniform solution;
s2, nbCl 5 Adding the mixture into the solution obtained in the step S1, and stirring until the mixture is completely dissolved;
s3, slowly dripping ammonia water solution into the mixed solution obtained in the step S2 to form suspension, and stirring for 1-3 h at room temperature;
s4, centrifuging the suspension obtained in the step S3, discarding supernatant, uniformly dispersing the precipitate in deionized water, and performing hydrothermal reaction;
and S5, centrifuging the product obtained in the step S4, washing with deionized water and absolute ethyl alcohol in sequence, and drying.
2. A large pore size mesoporous Nb as in claim 1 2 O 5 The preparation method of the photocatalytic material is characterized in that the addition amount of the hexadecyl trimethyl ammonium bromide in the step S1 is 0.005 g-0.03 g.
3. A large pore size mesoporous Nb as in claim 1 2 O 5 The preparation method of the photocatalytic material is characterized in that the mass fraction of the ammonia water solution in the step S3 is 2-8wt%.
4. A large pore size mesoporous Nb as in claim 1 2 O 5 The preparation method of the photocatalytic material is characterized in that the hydrothermal reaction temperature in the step S4 is 120-200 ℃.
5. A large pore size mesoporous Nb as in claim 1 2 O 5 The preparation method of the photocatalytic material is characterized in that the hydrothermal reaction time in the step S4 is 12-36 h.
6. A large pore size mesoporous Nb as in claim 1 2 O 5 The preparation method of the photocatalytic material is characterized in that in the step S5, deionized water is firstly used for washing the reaction product for 2-4 times, and then absolute ethyl alcohol is used for washing the reaction product for 2-4 times.
7. A large pore size mesoporous Nb as in claim 1 2 O 5 The preparation method of the photocatalytic material is characterized in that the drying temperature in the step S5 is 60-80 ℃.
8. As claimed inA large pore size mesoporous Nb as recited in claim 1 2 O 5 The preparation method of the photocatalytic material is characterized in that the drying time in the step S5 is 6-12 h.
9. A large-pore-diameter mesoporous Nb produced by the production method according to any one of claims 1 to 8 2 O 5 Photocatalytic material.
10. A large pore size mesoporous Nb as in claim 9 2 O 5 The application of the photocatalytic material in photocatalytic degradation of rhodamine B solution.
CN202310206640.7A 2023-03-06 2023-03-06 Mesoporous Nb with large aperture 2 O 5 Photocatalytic material, preparation method and application thereof Pending CN116282159A (en)

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CN107903144A (en) * 2017-11-17 2018-04-13 北京林业大学 One kind uses metal load type Nb2O5Method of the catalyst to lignin-base phenolic compound hydrogenation deoxidation
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