CN114345393A - Preparation method of defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst - Google Patents
Preparation method of defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst Download PDFInfo
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Abstract
A preparation method of defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst belongs to the field of photocatalytic water treatment. The method comprises the following steps: preparation of TiO by sol-gel method2Nanoparticles; second, second high temperature calcination to obtain thin g-C3N4V,; three, ball milling and compounding to obtain sandwich structure TiO2‑xUltra-thin g-C3N4/TiO2‑x(ii) a Fourthly, solid phase reduction is carried out to obtain the final defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxideA Z-type heterojunction photocatalyst. According to the preparation method of the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst, oxygen vacancies are introduced to widen the light absorption range of the photocatalyst, a sandwich structure is constructed to increase the space conduction and separation of photon-generated carriers, and the Z-type heterojunction improves the capability of the photocatalyst in generating strong oxidizing species, so that the activity and stability of the photocatalyst are stimulated in many aspects, and tetracycline or other types of pollutants in water are effectively removed.
Description
Technical Field
The invention belongs to the field of photocatalytic water treatment, and particularly relates to a preparation method of a defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst, which can be used for removing tetracycline in water more efficiently.
Background
For decades, antibiotics have played an important role in the preservation of human health. Among them, tetracyclines are of great significance for their wide application. However, excessive antibiotic entering the environment can cause a series of hazards, such as breaking ecological balance, threatening the human body, seriously interfering with the ecosystem, and the like. Thus, a great deal of research has been conducted to solve this problem. Among them, visible light photocatalysis is considered as a promising method.
TiO2As a traditional photocatalyst, the photocatalyst has proved to have good engineering application value. However, it also has some considerable disadvantages, such as too wide a band gap resulting in extremely poor visible light activity. However, the proposal of oxygen vacancies breaks this impasse. The generation of oxygen vacancies can significantly change the band gap position and color of the catalyst, and significantly prolong the wavelength absorption range of the catalyst. In addition, oxygen vacancies can enhance the catalyst's ability to absorb dissolved oxygen in water, thereby increasing the yield of strongly oxidizing species. It is worth mentioning from g-C3N4Since the introduction into the field of photocatalysis, research thereon has received increasing attention. g-C3N4The narrow band gap results in a stronger visible response. However, the high recombination rate of photogenerated carriers is a constraint on g-C3N4The key factor in development. Changing its micro-topography is an effective strategy. Wherein the thinner the thickness of the two-dimensional material, the more catalytically active sites result in better photocatalytic activity. Thus, ultra-thin g-C is used3N4Solving the problem of antibiotic pollution is a good choice.
Based on the above, aiming at the current situation that the antibiotic removal effect is not ideal and the existing catalyst in the environmental photocatalysis field has insufficient efficacy, if TiO containing oxygen vacancy is used2With ultra-thin g-C3N4The combination forms a heterojunction, is used for solving the pollution problem of the tetracycline, and can obtain good effect.
Disclosure of Invention
Aiming at the defects of the existing photocatalyst, the invention provides a preparation method of a defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst in order to more effectively remove tetracycline or other pollutants in water, and the method uses TiO containing oxygen vacancies2The nanoparticles are distributed in ultrathin g-C3N4The two sides of the photocatalyst can form a sandwich-shaped three-dimensional structure, so that the transmission path of the carrier can be effectively shortened, more reaction sites are provided, the photocatalytic performance of the photocatalyst is improved, and tetracycline in water can be more effectively removed.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst comprises the following steps:
step one, preparing TiO by a sol-gel method2Nanoparticle: dispersing butyl titanate in absolute ethyl alcohol to form a solution a, mixing deionized water, absolute ethyl alcohol and nitric acid to form a solution b, stirring the solution b fully, dropwise adding the solution b into the solution a, then stirring the mixed solution strongly until gelation is achieved, drying, and calcining at high temperature to obtain TiO2A nanoparticle;
step two, preparing ultrathin g-C by secondary calcination method3N4Nanosheet: placing urea in a porcelain boat for high-temperature calcination, naturally cooling to room temperature, repeating the high-temperature calcination process again, washing the obtained light yellow powder with deionized water and ethanol for multiple times to ensure the purity of the light yellow powder, and obtaining ultrathin g-C3N4Nanosheets;
step three, preparing TiO with sandwich structure by planetary ball milling method2Ultra-thin g-C3N4/TiO2: ultra-thin g-C3N4Nanosheet and TiO2Mixing the nano particles, putting the mixture into a ball milling tank, adding absolute ethyl alcohol and deionized water, ball milling for a plurality of hours at a high rotating speed, and finally fully drying the obtained mixture to obtain the sandwich structure TiO2Ultra-thin g-C3N4/TiO2A photocatalyst;
step four, preparing the TiO rich in oxygen vacancy by a solid phase reduction method2-xUltra-thin g-C3N4/TiO2-xZ-type heterojunction photocatalyst: adding TiO into sandwich structure2Ultra-thin g-C3N4/TiO2Mixing with sodium borohydride and grinding, then placing the mixture in a tubular furnace under N2Calcining and reducing under the atmosphere, fully washing the obtained powder with deionized water to remove residual impurities, and then drying to obtain the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst.
Further, in the first step, the volume ratio of the butyl titanate to the absolute ethyl alcohol in the solution a is 1: 1 to 4.
Further, in the first step, the volume ratio of the deionized water, the nitric acid and the absolute ethyl alcohol in the solution b is 4:1: 4-4: 4:4, and the volume ratio of the solution a to the solution b is 20-30 mL: 18-24 mL, wherein the stirring temperature is 20-30 ℃, and the stirring time is 30-60 min.
Further, in the first step, the stirring time of the mixed solution is 4-6 hours, the drying temperature is 60-70 ℃, and the drying time is 6-8 hours.
Further, in the first step, the high-temperature calcination is carried out at a temperature of 500-600 ℃ for 120-180 min, and the heating rate is 2-4 ℃/min.
Further, in the second step, the high-temperature calcination is carried out at a temperature of 500-600 ℃ for 4-8 h, and the heating rate is 2-4 ℃/min.
Further, in step three, the ultrathin g-C3N4Nanosheet, TiO2The mixing ratio of the nano particles, the deionized water and the absolute ethyl alcohol is 1 g: 1-4 g: 5-10 mL: 5-10 mL.
Further, in the third step, the ball milling speed is 300-500 rpm, the time is 2-5 hours, the drying temperature is 60-70 ℃, and the time is 6-8 hours.
Further, in the fourth step, the sandwich structure TiO2Ultra-thin g-C3N4/TiO2The mass ratio of the sodium borohydride to the sodium borohydride is 1: 1-5, wherein the calcining temperature is 300-450 ℃, the calcining time is 20-80 min, the heating rate is 2-4 ℃/min, the drying temperature is 60-70 ℃, and the drying time is 6-8 h.
The defect type titanium dioxide/ultrathin carbon nitride/defect type titanium dioxide Z-shaped heterojunction photocatalyst prepared by the method is applied to the field of photocatalytic water treatment.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a preparation method of a defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst for the first time, which is used for effectively removing tetracycline or other pollutants in water. The synthesis process mainly adopts a sol-gel combined secondary calcination method and simultaneously combines the modes of planetary grinding, in-situ reduction and the like. The Z-type heterojunction, the formation of oxygen vacancy and the special three-dimensional structure act together, so that the band gap of the catalyst is reduced, the separation of electron-hole pairs is effectively promoted, and the visible light photocatalytic activity of the catalyst is improved. At the same time, for TCH removal, pH, NH3-N、SO4 2-Different influences of water quality parameters such as adding amount, initial concentration and the like and operation conditions on degradation rate, and the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst can also effectively treat tetracycline from the realityAnd (4) removing the wastewater. This approach provides an attractive preferred solution for photocatalytic degradation of antibiotics in the visible and will be of great interest in photocatalytic applications.
Drawings
FIG. 1 is a UV-visible diffuse reflectance diagram according to the present invention;
FIG. 2 is a diagram of the forbidden band width of the catalyst according to the present invention;
FIG. 3 is a graph of the catalytic degradation of the performance evaluation of the catalyst of the present invention;
FIG. 4 is a graph of the absorption wavelength of the tetracyclines of the present invention as a function of time;
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments, but not limited thereto, and modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
The invention introduces oxygen vacancy to widen the light absorption range of the catalyst, constructs a sandwich structure to increase the space conduction and separation of photon-generated carriers, and improves the capability of the photocatalyst to generate strong oxidizing species by the Z-shaped heterojunction, thereby exciting the activity and stability of the photocatalyst in many aspects and effectively removing tetracycline or other types of pollutants in water.
Example 1:
a preparation method of a defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst (S-TUCNov) specifically comprises the following steps:
(1) preparation of TiO by sol-gel method2Nanoparticle: dispersing 5mL of butyl titanate into 20mL of absolute ethyl alcohol to form a solution a, mixing 8mL of deionized water, 8mL of absolute ethyl alcohol and 2mL of nitric acid to form a solution b, stirring the solution b for 30min at 20 ℃, dropwise adding the solution b into the solution a, then stirring the mixed solution strongly for 4h to gelatinize, drying at 60 ℃ for 12h, calcining at 500 ℃ for 120min, and raising the temperature at the rate of 2 ℃/min to obtain TiO2A nanoparticle;
(2) preparation of ultrathin g-C by secondary calcination method3N4Nanosheet: generally, 15g of urea is placed in a porcelain boat, the urea is calcined for 4h at the high temperature of 550 ℃ at the heating rate of 2 ℃/min, the high-temperature calcination process is repeated after the urea is naturally cooled to the room temperature, the obtained light yellow powder is washed for multiple times by deionized water and ethanol respectively to ensure the purity of the light yellow powder, and ultrathin g-C is obtained3N4Nanosheets;
(3) method for preparing sandwich structure TiO by planet ball milling method2Ultra-thin g-C3N4/TiO2: 5g of ultrathin g-C3N4Nanosheet with 10g of TiO2Mixing the nano particles, putting into a ball milling tank, adding 5mL of absolute ethyl alcohol and 10mL of deionized water, ball milling for 3h at the rotating speed of 300rpm, and finally drying the obtained mixture for 6h at 70 ℃ to obtain the TiO with the sandwich structure2Ultra-thin g-C3N4/TiO2A photocatalyst;
(4) preparation of oxygen vacancy-rich TiO by solid-phase reduction method2-xUltra-thin g-C3N4/TiO2-xZ-type heterojunction photocatalyst: adding 5g of sandwich structure TiO2Ultra-thin g-C3N4/TiO2And 5g of sodium borohydride were mixed and ground, and the mixture was then placed in a tube furnace under N2Calcining and reducing for 80min at 350 ℃ in the atmosphere, wherein the heating rate is 5 ℃/min, fully washing the obtained powder with deionized water to remove residual impurities, and then drying to obtain the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst.
Comparative example 1:
Comparative example 2:
ultrathin g-C3N4The preparation method of the photocatalyst (UCN) comprises the following steps: preparation of ultrathin g-C by secondary calcination method3N4Nanosheet: generally, 15g of urea is placed in a porcelain boat, the urea is calcined for 4h at the high temperature of 550 ℃ at the heating rate of 2 ℃/min, the high-temperature calcination process is repeated after the urea is naturally cooled to the room temperature, the obtained light yellow powder is washed for multiple times by deionized water and ethanol respectively to ensure the purity of the light yellow powder, and ultrathin g-C is obtained3N4Nanosheets.
Comparative example 3:
TiO with sandwich structure2Ultra-thin g-C3N4/TiO2The preparation method of the heterojunction photocatalyst (S-TUCN) specifically comprises the following steps:
(1) preparation of TiO by sol-gel method2Nanoparticle: dispersing 5mL of butyl titanate into 20mL of absolute ethyl alcohol to form a solution a, mixing 8mL of deionized water, 8mL of absolute ethyl alcohol and 2mL of nitric acid to form a solution b, stirring the solution b for 30min at 20 ℃, dropwise adding the solution b into the solution a, then stirring the mixed solution strongly for 4h to gelatinize, drying at 60 ℃ for 12h, calcining at 500 ℃ for 120min, and raising the temperature at the rate of 2 ℃/min to obtain TiO2A nanoparticle;
(2) preparation of ultrathin g-C by secondary calcination method3N4Nanosheet: generally, 15g of urea is placed in a porcelain boat, the urea is calcined for 4h at the high temperature of 550 ℃ at the heating rate of 2 ℃/min, the high-temperature calcination process is repeated after the urea is naturally cooled to the room temperature, the obtained light yellow powder is washed for multiple times by deionized water and ethanol respectively to ensure the purity of the light yellow powder, and ultrathin g-C is obtained3N4Nanosheets;
(3) method for preparing sandwich structure TiO by planet ball milling method2Ultra-thin g-C3N4/TiO2: 5g of ultrathin g-C3N4Nanosheet with 10g of TiO2Mixing the nano particles, putting into a ball milling tank, adding 5mL of absolute ethyl alcohol and 10mL of deionized water, ball milling for 3h at the rotating speed of 300rpm, and finally drying the obtained mixture for 6h at 70 ℃ to obtain the TiO with the sandwich structure2UltraThin g-C3N4/TiO2A photocatalyst.
The activity investigation method for degrading tetracycline by photocatalysis provided by the invention comprises the following steps:
A300W xenon lamp provided with a 420nm cut-off filter is used as an excitation light source, and the photocatalytic degradation of the catalyst on the high-toxicity tetracycline is researched under the irradiation of visible light. Briefly, 50mg of photocatalyst was uniformly suspended in 50mL of a 10mg/L tetracycline solution at a magnetic stirring speed of 500 rpm. Before irradiation of visible light, the mixed solution was stirred in the dark for 30min to reach adsorption-desorption equilibrium. At the same time intervals, 2.0mL of the suspension was taken, and after filtration through a 0.22 μm membrane, absorbance measurement was performed at 357nm to determine the tetracycline concentration.
In order to analyze the optical properties of the photocatalyst, ultraviolet-visible diffuse reflection and band gap analysis were performed, as shown in fig. 1 and 2. With home-made TiO having only UV absorption2In contrast, UCNs have a slightly wider light absorption range from ultraviolet to visible light due to their narrower band gap. On this basis, S-TUCN produces a significant red shift by combination, enhances the absorption range of visible light, and reduces the bandgap to 2.56 eV. In addition, the introduction of oxygen vacancies further expands the absorption of visible light and shortens the band gap to 1.65 eV. S-TUCNov has the strongest visible light absorption efficiency, with its light absorption edge extending to around 750nm, respectively. This demonstrates that the formation of heterojunctions and oxygen vacancies can effectively alter the band gap position while improving catalytic performance.
As shown in FIG. 2, the degradation performance of S-TUCNov has been leading. After visible light treatment for 60min, TiO2TCH removal rates for UCN, S-TUCN and S-TUCNov were 15.5%, 74.1%, 81.7% and 87.7%, respectively. Meanwhile, the tetracycline concentration in the S-TUCNov system continuously decreases with the increase of the illumination time. Therefore, studies indicate that S-TUCNov has the most excellent photocatalytic performance. The results show that the sandwich structure TiO prepared by the invention2-xUltra-thin g-C3N4/TiO2-xThe Z-type heterojunction photocatalyst can remove tetracycline or other pollutants in water more effectively.
The invention is not the best known technology. The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A preparation method of defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst is characterized in that: the method comprises the following steps:
step one, preparing TiO by a sol-gel method2Nanoparticle: dispersing butyl titanate in absolute ethyl alcohol to form a solution a, mixing deionized water, absolute ethyl alcohol and nitric acid to form a solution b, stirring the solution b fully, dropwise adding the solution b into the solution a, then stirring the mixed solution strongly until gelation is achieved, drying, and calcining at high temperature to obtain TiO2A nanoparticle;
step two, preparing ultrathin g-C by secondary calcination method3N4Nanosheet: placing urea in a porcelain boat for high-temperature calcination, naturally cooling to room temperature, repeating the high-temperature calcination process again, and washing the obtained light yellow powder with deionized water and ethanol for multiple times to obtain ultrathin g-C3N4Nanosheets;
step three, preparing TiO with sandwich structure by planetary ball milling method2Ultra-thin g-C3N4/TiO2: ultra-thin g-C3N4Nanosheet and TiO2Mixing the nano particles, putting the mixture into a ball milling tank, adding absolute ethyl alcohol and deionized water, ball milling for a plurality of hours at a high rotating speed, and finally fully drying the obtained mixture to obtain the sandwich structure TiO2Ultra-thin g-C3N4/TiO2A photocatalyst;
step four, preparing the TiO rich in oxygen vacancy by a solid phase reduction method2-xUltra-thin g-C3N4/TiO2-xZ-type heterojunction photocatalyst: adding TiO into sandwich structure2Ultra-thin g-C3N4/TiO2Mixing with sodium borohydride and grinding, then placing the mixture in a tubular furnace under N2Calcining and reducing under the atmosphere, fully washing the obtained powder with deionized water to remove residual impurities, and then drying to obtain the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-type heterojunction photocatalyst.
2. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in the first step, the volume ratio of the butyl titanate to the absolute ethyl alcohol in the solution a is 1: 1 to 4.
3. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in the first step, the volume ratio of deionized water, nitric acid and absolute ethyl alcohol in the solution b is 4:1: 4-4: 4:4, and the volume ratio of the solution a to the solution b is 20-30 mL: 18-24 mL, wherein the stirring temperature is 20-30 ℃, and the stirring time is 30-60 min.
4. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in the first step, the stirring time of the mixed solution is 4-6 hours, the drying temperature is 60-70 ℃, and the drying time is 6-8 hours.
5. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in the first step, the high-temperature calcination is carried out at a temperature of 500-600 ℃ for 120-180 min at a temperature rise rate of 2-4 ℃/min.
6. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in the second step, the high-temperature calcination is carried out at the temperature of 500-600 ℃ for 4-8 h, and the heating rate is 2-4 ℃/min.
7. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in step three, the ultrathin g-C3N4Nanosheet, TiO2The mixing ratio of the nano particles, the deionized water and the absolute ethyl alcohol is 1 g: 1-4 g: 5-10 mL: 5-10 mL.
8. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in the third step, the ball milling speed is 300-500 rpm, the time is 2-5 h, the drying temperature is 60-70 ℃, and the time is 6-8 h.
9. The method for preparing the defective titanium dioxide/ultrathin carbon nitride/defective titanium dioxide Z-shaped heterojunction photocatalyst according to claim 1, wherein the method comprises the following steps: in the fourth step, the sandwich structure TiO2Ultra-thin g-C3N4/TiO2The mass ratio of the sodium borohydride to the sodium borohydride is 1: 1-5, wherein the calcining temperature is 300-450 ℃, the calcining time is 20-80 min, the heating rate is 2-4 ℃/min, the drying temperature is 60-70 ℃, and the drying time is 6-8 h.
10. A defect type titanium dioxide/ultrathin carbon nitride/defect type titanium dioxide Z-shaped heterojunction photocatalyst prepared according to any one of claims 1 to 9 is applied to the field of photocatalytic water treatment.
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| CN115090304A (en) * | 2022-08-10 | 2022-09-23 | 深圳市康弘智能健康科技股份有限公司 | F-TiO 2-x Preparation method of Pt nano photocatalyst film and application of Pt nano photocatalyst film in air purification |
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