CN115090303A - Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst and preparation method and application thereof - Google Patents
Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst, preparation method and application thereof, and Bi 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst consists of Bi 2 S 3 And Bi 5 O 7 I composition, wherein, Bi 2 S 3 And Bi 5 O 7 The molar ratio of I is 0.1-9: 1. Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalysisThe preparation is obtained by two steps, firstly, the nano-banded Bi is prepared by a hydrothermal synthesis method 5 O 7 I, adding thioacetamide for erosion, and finally obtaining Bi through ion exchange reaction under hydrothermal condition 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst. The invention constructs Bi with visible light response 2 S 3 /Bi 5 O 7 The I Z type heterojunction accelerates the separation of photon-generated carriers, has high-efficiency photocatalytic activity and stability under visible light, has high-efficiency killing and degrading effects on harmful microorganisms and dye pollutants in water, and has good practical value and potential application prospect in the fields of water purification, marine antifouling and the like.
Description
Technical Field
The invention relates to a composite photocatalyst, a preparation method and application thereof, and specifically relates to a Bi 2 S 3 /Bi 5 O 7 An I Z type heterojunction composite photocatalyst, a preparation method and an application thereof, which belong to the technical field of photocatalysis.
Background
With the development of industrialization, global water pollution becomes more and more serious, and in order to meet the major challenge, a large number of students begin to explore an environment-friendly and green environmental pollution treatment method, especially TiO is discovered in 1972 2 After being able to decompose water using visible light to generate hydrogen, more and more scientists have begun to research photocatalytic technology to address environmental pollution. TiO 2 2 ZnO, etc. are currently the most commonly used photocatalytic materials, but their applications are limited due to their low quantum efficiency, narrow response range to visible light, and high recombination rate of photogenerated carriers. In order to improve the visible light catalytic activity, researchers have developed some novel photocatalysts, such as Bi-based semiconductor materials, MoS 2 Ag-based materials, metal organic framework Materials (MOFs), and the like.
In recent years, bismuth-based semiconductorsBulk materials have attracted attention due to the unique layered structure. The Bi-based material is composed of two layers of [ Bi ] 2 O 2 ] 2+ The layered structure assembled by arrangement provides more space for the transfer of photogenerated carriers. Due to the orbital hybridization of Bi 6s and O2 p, the symmetry of the material is reduced, a dipole is generated, and the response range to visible light is expanded. Among bismuth-based semiconductor materials, Bi 5 O 7 I as a structural derivative of the BiOI has excellent photocatalytic activity due to the wide band gap and the presence of an I5 p hybrid orbital. In particular, Bi 5 O 7 The wide band gap of I (2.84-2.94eV) is much larger than that of BiOI, and can effectively inhibit the recombination of photogenerated carriers. However, Bi monomer 5 O 7 The response range of the photocatalyst I to visible light is narrow, and the photocatalytic activity of the photocatalyst is reduced. Therefore, it is urgent to further modify and study the heterojunction, and the heterojunction can widen the response range to visible light and enhance Bi by semiconductor composite construction 5 O 7 Photocatalytic activity of I.
Due to bismuth sulfide (Bi) 2 S 3 ) Due to the unique layered structure and the narrow band gap width (1.3-1.7eV), the visible light response range is good, and the visible light response range is widely applied to photocatalytic degradation of organic pollutants, reduction of heavy metal ions, water decomposition and the like. In addition, Bi 2 S 3 The solubility product is small, a heterojunction can be obtained by compounding the semiconductor material with other bismuth-based semiconductor materials through an in-situ ion exchange method, and the photocatalytic activity of the semiconductor material can be effectively improved. Thus, Bi is added 2 S 3 And Bi 5 O 7 The heterojunction formed by compounding I can effectively promote the separation efficiency of photon-generated carriers, enhance the utilization rate of visible light, efficiently and quickly degrade organic pollutants and kill bacteria, and has wide application prospect in the aspects of solving water pollution and marine antifouling.
Disclosure of Invention
The invention aims to solve the technical problem of providing Bi aiming at the defects in the prior art 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst, preparation method and application thereof, and Bi of the invention 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst has high-efficiency photocatalytic activity and stability under visible light, and has high-efficiency killing and degradation effects on harmful microorganisms and dye pollutants in water.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention firstly provides Bi 2 S 3 /Bi 5 O 7 I Z type composite photocatalyst consisting of Bi sulfide 2 S 3 And bismuth-rich bismuth oxyiodide Bi 5 O 7 I composition, wherein, Bi 2 S 3 And Bi 5 O 7 The molar ratio of I is 0.1-9: 1.
The invention firstly provides Bi 2 S 3 /Bi 5 O 7 The preparation method of the I Z type heterojunction composite photocatalyst comprises the following steps:
(1)Bi 5 O 7 preparation of I:
adding bismuth nitrate Bi (NO) into ultrapure water 3 ) 3 ·5H 2 O, adding NaOH solution after ultrasonic dispersion, and stirring and dissolving to obtain suspension A1; adding potassium iodide KI into ultrapure water, and stirring until the potassium iodide KI is completely dissolved to obtain a dispersion liquid B1; dropwise adding the dispersion liquid B1 into the suspension liquid A1, continuously stirring to obtain a mixed liquid 1 after dropwise adding is finished, carrying out high-temperature reaction on the mixed liquid 1, cooling to room temperature after reaction, and carrying out suction filtration, washing and drying to obtain Bi with a nano-belt-shaped structure 5 O 7 I；
(2)Bi 2 S 3 /Bi 5 O 7 Preparation of I Z type heterojunction composite photocatalyst:
bi obtained in the step (1) 5 O 7 I, adding the mixture into ultrapure water, and performing ultrasonic dispersion to obtain a dispersion liquid A2; then adding thioacetamide C 2 H 5 Adding NS into ultrapure water to be completely dissolved to obtain dispersion liquid B2; then dropwise adding the dispersion liquid B2 into the suspension liquid A2, continuously stirring to obtain a mixed liquid 2 after dropwise adding is finished, carrying out high-temperature reaction on the mixed liquid 2, cooling to room temperature after reaction, and carrying out suction filtration, washing and drying to obtain Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
In the above technical scheme, in the step (1), the ultrasonic dispersion has a frequency of 100W-300W and a time of 0.5 h-4 h.
In the technical scheme, in the step (1), the concentration of the NaOH solution is 1.0-3.0 mol/L; and adjusting the pH value of the system to 9-14 after adding the NaOH solution.
In the above technical solution, in the step (1), the Bi (NO) is 3 ) 3 ·5H 2 The molar ratio of O to KI is 1: 1-5.
In the technical scheme, in the step (1), the dispersion liquid B1 is dropwise added into the suspension liquid A1, and after the dropwise addition is completed, the mixture is continuously stirred for 0.5 to 4 hours to obtain a mixed liquid 1, wherein the stirring speed is 200 to 2000 r/min.
In the technical scheme, in the step (1), the mixed solution 1 is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the reaction kettle is placed into an electric heating constant-temperature blast drying oven and is subjected to heat treatment at 120-200 ℃ for 8-32 hours to perform high-temperature reaction; after the reaction is finished, cooling the reaction kettle to room temperature, and performing suction filtration, washing and drying to obtain Bi with a nano belt-shaped structure 5 O 7 I。
In the above technical scheme, in the step (2), the ultrasonic dispersion has a frequency of 100W-300W and a time of 0.5 h-4 h.
In the above technical solution, in the step (2), the step C 2 H 5 NS and Bi 5 O 7 0.1 to 10% of I: 1.
in the technical scheme, in the step (2), the dispersion liquid B2 is dropwise added into the suspension liquid A2, and after the dropwise addition is finished, the stirring is continued for 0.5-4 hours to obtain a mixed liquid 2, wherein the stirring speed is 200-2000 r/min.
In the technical scheme, in the step (2), the mixed solution 2 is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, the reaction kettle is placed in an electric heating constant-temperature blast drying box, and heat treatment is carried out at 120-200 ℃ for 8-32 hours to carry out high-temperature reaction; after the reaction is finished, cooling the reaction kettle to room temperature, and performing suction filtration,Washed and dried to obtain Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
The invention also provides Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst is prepared by the preparation method and is prepared from bismuth sulfide Bi 2 S 3 And bismuth-rich bismuth oxyiodide Bi 5 O 7 I composition, wherein, Bi 2 S 3 And Bi 5 O 7 The molar ratio of I is 0.1-9: 1.
The invention also provides Bi 2 S 3 /Bi 5 O 7 The application of the I Z type heterojunction composite photocatalyst in the aspect of dye degradation.
The invention also provides Bi 2 S 3 /Bi 5 O 7 The application of the I Z type heterojunction composite photocatalyst in the sterilization aspect.
Compared with the prior art, the method has the following characteristics:
(1) the invention adopts a simple hydrothermal synthesis method and Bi prepared by an in-situ ion exchange method 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst has good visible light absorption performance and photocatalysis performance, can efficiently degrade dyes and kill bacteria, and has better photocatalysis activity than Bi 2 S 3 And Bi 5 O 7 I, monomer material;
(2) bi prepared by the invention 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst has good stability and reusability;
(3) bi prepared by the invention 2 S 3 /Bi 5 O 7 The I heterojunction composite photocatalyst has a Z-shaped heterostructure, accelerates the separation of photo-generated carriers, improves the visible light catalytic activity, and has good practical value and potential application prospect in the fields of water purification, marine antifouling and the like.
Drawings
FIG. 1: XRD patterns of the samples prepared in inventive example 1 and comparative example 1, wherein the abscissa is 2 θ (angle) and the unit is degree (degree); intensity on the ordinate, in a.u. (absolute units);
FIG. 2-a: bi prepared in inventive example 1 5 O 7 I Field Emission Scanning Electron Microscope (FESEM) photograph;
FIG. 2-b: bi prepared in comparative example 1 of the invention 2 S 3 A Field Emission Scanning Electron Microscope (FESEM) photograph of (a);
FIG. 2-c: a Field Emission Scanning Electron Microscope (FESEM) photograph (1 μm) of the sample prepared in example 1 of the present invention;
FIG. 2-d: a Field Emission Scanning Electron Microscope (FESEM) photograph (500nm) of the sample prepared in example 1 of the present invention;
FIG. 3: ultraviolet-visible diffuse reflectance spectra (UV-DRS) of samples prepared in inventive example 1 and comparative example 1, wherein the abscissa is Wavelength (Wavelength) in nm (nanometers) and the ordinate is Absorbance in a.u (absolute units);
FIG. 4: the RhB concentration of the sample prepared in the embodiment 1 of the invention changes with Time in the photocatalytic degradation reaction, wherein the abscissa is Time, the unit is min, and the ordinate is C t /C 0 ，C 0 Initial concentration of RhB before reaction initiation, C t The rhB concentration at reaction time t (■ represents Bi) 5 O 7 I. ● represents Bi 2 S 3 And a represents Bi 2 S 3 /Bi 5 O 7 I. T represents Blank);
FIG. 5: the Time-dependent change curve of the Survival condition of the bacteria in the photocatalytic sterilization reaction of the pseudomonas aeruginosa by the sample prepared in the embodiment 1 of the invention is shown in the abscissa of Time in min and in the ordinate of survivability in (wherein ■ represents Blank and ● represents Bi) 5 O 7 I. A represents Bi 2 S 3 And xxx represents Bi 2 S 3 /Bi 5 O 7 I)。
Detailed Description
The following detailed description of the embodiments of the present invention is provided, but the present invention is not limited to the following descriptions:
the invention is prepared by mixing Bi 2 S 3 And Bi 5 O 7 I compounding, namely constructing a composite material with a Z-shaped heterostructure, accelerating the separation of a photon-generated carrier on the surface of the composite material, further improving the photocatalytic performance, and carrying out the photocatalytic treatment on Bi 2 S 3 And Bi 5 O 7 The practical application of the two materials I in the field of photocatalysis is of great significance.
The technical scheme of the invention is illustrated by combining the following specific embodiments:
comparative example 1:
monomer Bi 2 S 3 The preparation method comprises the following steps:
0.1mmol of Bi 5 O 7 I is added to 30mL of ultrapure water and, after 0.5h of ultrasonic dispersion at a frequency of 240W, an excess (30mL of 30mM strength) of C is added with continuous stirring 2 H 5 The NS solution is continuously stirred for 1h at the speed of 800r/min, transferred into a 100mL polytetrafluoroethylene reaction kettle, reacted for 12h at the temperature of 180 ℃, cooled to room temperature, filtered, collected and precipitated, washed by deionized water and ethanol, and dried at the temperature of 60 ℃ and normal pressure to obtain Bi 2 S 3 Monomer material, noted Bi 2 S 3 。
Example 1:
bi 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst is prepared by the following preparation method:
(1)Bi 5 O 7 preparation of I: adding 2mmol of Bi (NO) into 40mL of ultrapure water 3 ) 3 ·5H 2 O, performing ultrasonic dispersion for 0.5h at the frequency of 240W, and then adding 20mL of 1.5mol/L NaOH solution to obtain a dispersion A1; simultaneously adding 6mmol KI into 20mL of ultrapure water, and stirring until the KI is completely dissolved to obtain a suspension B1; then dropwise adding the dispersion liquid B1 into the suspension liquid A1, continuously stirring for 1h at 1000r/min, transferring the mixed liquid 1 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting the reaction kettle into an electric heating constant-temperature air-blowing drying oven for heat treatment for 24h at 180 ℃; then cooling the reaction kettle to room temperature, and obtaining the rod through suction filtration, washing and dryingBi of a layered structure 5 O 7 I；
(2)Bi 2 S 3 /Bi 5 O 7 Preparation of I Z type heterojunction composite photocatalyst: 0.1mmol of Bi obtained above 5 O 7 Adding the I into 30mL of ultrapure water, and dispersing by ultrasonic treatment for 0.5h at the frequency of 240W to obtain a dispersion liquid A2; simultaneously adding 0.2mmol of C 2 H 5 Adding NS into 30mL of ultrapure water, and completely dissolving to obtain a dispersion liquid B2; then dropwise adding the dispersion liquid B2 into the suspension liquid A2, continuously stirring for 1h at 1000r/min, transferring the mixed liquid 2 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting the high-pressure reaction kettle into an electric heating constant-temperature air-blowing drying oven for heat treatment for 12h at 180 ℃; after the reaction is finished, cooling the reaction kettle to room temperature, and obtaining Bi through suction filtration, washing and drying 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
The XRD patterns of the samples obtained in inventive example 1 and comparative example 1 are shown in FIG. 1, and it can be seen from FIG. 1 that pure Bi is obtained 2 S 3 All diffraction peaks of (2) can be related to Bi 2 S 3 Matching (JCPDS card number 84-0279) indicates high purity and good crystallization. For pure Bi 5 O 7 I, these diffraction peaks can be associated with Bi-rich form 5 O 7 I (JCPDS card number 40-0548). Bi 2 S 3 /Bi 5 O 7 The spectrum of the I composite material contains Bi 2 S 3 And bismuth-rich type Bi 5 O 7 All characteristic peaks of I. Furthermore, with pure Bi 5 O 7 I phase to Bi 2 S 3 /Bi 5 O 7 The peak position of the I composite material is hardly shifted, indicating that Bi 2 S 3 Supported pair of Bi 5 O 7 The lattice structure of I has little effect.
Scanning electron micrographs of samples obtained in inventive example 1 and comparative example 1 are shown in FIG. 2, and from FIG. 2, Bi 5 O 7 I is a nanoribbon structure exhibiting a width of about 1 μm. Bi 2 S 3 Then is by C 2 H 5 Complete corrosion of Bi by NS 5 O 7 I, forming a nano rod-shaped structure with the width of about 1 μm and the thickness of about 300 nm. Bi 2 S 3 /Bi 5 O 7 The I composite material shows a band-like structure with a width of about 1 μm, and the surface is covered with a network structure formed by interweaving nanorods. These nanorods are Bi obtained by ion exchange reaction 2 S 3 In Bi 5 O 7 Surface in-situ growth of I nanoribbon, resulting in Bi 5 O 7 I surface coating Bi 2 S 3 And (4) covering the nanorods.
The ultraviolet-visible diffuse reflectance spectra of the samples obtained in inventive example 1 and comparative example 1 are shown in FIG. 3, and it can be seen from FIG. 3 that pure Bi is present 2 S 3 Exhibits strong light absorption from ultraviolet to visible region, and Bi 5 O 7 I shows good light absorption in the visible region around 400 nm. On the other hand, with pure Bi 5 O 7 I phase to I phase of Bi 2 S 3 /Bi 5 O 7 The I composite material has wider light absorption range and stronger visible light responsiveness, which can be attributed to Bi 2 S 3 /Bi 5 O 7 I forms a Z-type heterostructure. The results show that Bi 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite material shows good light absorption performance to visible light, so that the material has possible application in photocatalysis.
Example 2:
bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst, which is different from example 1 in that Bi (NO) is controlled 3 ) 3 ·5H 2 The molar ratio of O to KI is 1:2, and Bi (NO) is controlled 3 ) 3 ·5H 2 O、Bi 5 O 7 The ultrasonic time is 1h, the stirring time is controlled to be 1.5h, the stirring speed is controlled to be 800r/min, the hydrothermal reaction temperature is controlled to be 160 ℃, and the ultrasonic-hydrothermal-hydrolysis-resistant material is prepared by the following preparation method:
(1) adding 2mmol of Bi (NO) into 40mL of ultrapure water 3 ) 3 ·5H 2 O, ultrasonically dispersing for 1h at the frequency of 210W, and then adding 20mL of 1.5mol/L NaOH solution to obtain a suspension A1; meanwhile, 4mmol of KI is added into 20mL of ultrapure water, and the KI is stirred until the KI is completely dissolved, so that a dispersion liquid B1 is obtained; then theDropwise adding the dispersion liquid B1 into the suspension liquid A1, continuously stirring for 1.5h at 800r/min, transferring the mixed liquid 1 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and placing the reaction kettle into an electric heating constant-temperature air-blast drying oven for heat treatment at 160 ℃ for 24 h; then cooling the reaction kettle to room temperature, and obtaining Bi with a nano-belt structure through suction filtration, washing and drying 5 O 7 I；
(2) 0.05mmol of Bi obtained in (1) 5 O 7 Adding the I into 30mL of ultrapure water, and dispersing by ultrasonic treatment for 1h at the frequency of 210W to obtain a dispersion liquid A2; simultaneously adding 0.2mmol of C 2 H 5 NS is added into 30mL of ultrapure water to be completely dissolved, and dispersion liquid B2 is obtained; then dropwise adding the dispersion liquid B2 into the suspension liquid 2A, continuously stirring for 1.5h at 800r/min, transferring the mixed liquid 2 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting the high-pressure reaction kettle into an electric heating constant-temperature air-blowing drying oven for heat treatment for 12h at 160 ℃; after the reaction is finished, cooling the reaction kettle to room temperature, and obtaining Bi through suction filtration, washing and drying 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
Example 3:
bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst, which is different from example 1 in that Bi (NO) is controlled 3 ) 3 ·5H 2 O、Bi 5 O 7 I, ultrasonic time is 1.5h, stirring time is controlled to be 2h, stirring speed is controlled to be 1200r/min, hydrothermal reaction time is controlled to be 10h, and the ultrasonic-hydrothermal reaction kettle is prepared by the following preparation method:
(1) adding 2mmol of Bi (NO) into 40mL of ultrapure water 3 ) 3 ·5H 2 O, performing ultrasonic dispersion for 1.5h at the frequency of 180W, and then adding 20mL of 1.5mol/L NaOH solution to obtain a suspension A1; simultaneously adding 6mmol KI into 20mL of ultrapure water, and stirring until the KI is completely dissolved to obtain a suspension B1; then dropwise adding the dispersion liquid B1 into the suspension liquid A1, continuously stirring for 2 hours at 1200r/min, transferring the mixed liquid 1 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting the reaction kettle into an electric heating constant-temperature air-blowing drying oven for heat treatment for 10 hours at 180 ℃; then cooling the reaction kettle to room temperature, and coolingFiltering, washing and drying to obtain Bi with a nano-belt structure 5 O 7 I。
(2) Then 0.15mmol of Bi obtained in (1) 5 O 7 Adding the I into 30mL of ultrapure water, and dispersing by ultrasonic treatment for 1.5h at the frequency of 180W to obtain a dispersion liquid A2; simultaneously adding 0.2mmol of C 2 H 5 Adding NS into 30mL of ultrapure water, and completely dissolving to obtain a dispersion liquid B2; then dropwise adding the dispersion liquid B2 into the suspension liquid A2, continuously stirring for 2 hours at 1200r/min, transferring the mixed liquid 2 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting the high-pressure reaction kettle into an electric heating constant-temperature air-blowing drying box for heat treatment for 10 hours at 180 ℃; after the reaction is finished, cooling the reaction kettle to room temperature, and obtaining Bi through suction filtration, washing and drying 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
Application example 1: bi prepared in example 1 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst applied to visible light photocatalytic degradation of dye pollutant rhodamine B
50mL of 10 -5 M in rhodamine B (RhB) solution into a 50mL reactor, 50mg of Bi prepared in example 1 was added 2 S 3 /Bi 5 O 7 And I, a 500W xenon lamp is used as a light source to simulate sunlight, and a 420nm filter is used for filtering ultraviolet light to ensure that light received by the reaction is visible light. Stirring for 30min in a dark state to enable the catalyst and the RhB to reach an adsorption/desorption equilibrium state, then turning on a light source, respectively sampling at certain time intervals in the reaction process under dark state and illumination conditions, centrifuging, taking supernatant, measuring the absorbance of the RhB solution at 552nm wavelength on an ultraviolet visible spectrophotometer, obtaining the residual concentration of the RhB, calculating the degradation rate, and taking a blank experiment and a dark state experiment as control experiments (see figure 4).
As can be seen from FIG. 4, RhB was hardly degraded in the blank and dark experiments, and the effect on the experiments was negligible. Under visible light irradiation, Bi 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst shows good photocatalytic activity, and the photocatalytic performance is obviously superior to that of monomer Bi 2 S 3 And Bi 5 O 7 I, the degradation rate of RhB in 90min of photocatalytic reaction time can reach 100%. Therefore, Bi having good visible light absorption properties and photocatalytic activity 2 S 3 And Bi 5 O 7 The Z-type heterostructure formed by the I recombination can effectively separate the photoproduction electron-hole on the surface of the composite material, improve the visible light absorption performance and the specific surface area of the composite material and enhance the visible light catalytic performance of the composite material. Bi prepared in example 2 and example 3 2 S 3 /Bi 5 O 7 Similar results as described above can also be achieved with I.
Application example 2: bi in example 1 2 S 3 /Bi 5 O 7 Visible light killing of I Z type heterojunction composite photocatalyst on pseudomonas aeruginosa
A500W xenon lamp is used as a light source, and an optical filter is used for filtering ultraviolet light, so that the wavelength range of the ultraviolet light is 420-760 nm. Pseudomonas aeruginosa (P. aeruginosa, 2.0X 10) 8 cfu/mL) evaluation of Bi 2 S 3 /Bi 5 O 7 The visible light catalytic sterilization performance of the I Z type heterojunction composite photocatalyst.
Bacterial suspensions were prepared first, and p.aeruginosa stock solutions were inoculated into sterilized LB liquid medium, which was then placed in an air constant temperature shaker at 37 ℃ and 150rpm for overnight culture. The bacterial suspension obtained by the culture was centrifuged and suspended in 0.01mol/L PBS (pH 7.4) buffer to give a concentration of 2.0X 10 8 Aeruginosa bacterial suspension at cfu/mL. In the photocatalytic experiment, 49.5mL of sterilized 0.01mol/L PBS (pH 7.4) buffer was added to a 50mL reactor, and 500. mu.L of the bacterial suspension was added to give a bacterial concentration of 2.0X 10 6 cfu/mL, 50mg of Bi prepared in example 1 was added 2 S 3 /Bi 5 O 7 I, a catalyst. Carrying out photocatalytic reaction after the dark state adsorption reaches balance, sampling at certain time intervals in the reaction process, and determining the survival rate and the sterilization rate of bacteria by a flat plate counting method. The method comprises the following specific steps: 1.0mL of the reaction mixture was serially diluted with 0.01mol/L PBS (pH 7.4) buffer to obtain several gradients, and 100. mu.L of the diluted solution was added to the prepared LB solidAnd (3) uniformly smearing the bacterial liquid on an LB culture medium on a body culture medium. And (3) inverting the LB culture medium, putting the culture medium into an electric heating constant-temperature incubator to culture for 24 hours at 37 ℃, and obtaining the concentration of the bacteria by counting the number of colonies growing on the culture medium and corresponding dilution times so as to determine the survival rate and the sterilization rate of the bacteria. Each set of experiments was performed 3 times in parallel, and the average was taken as the final result, and the blank experiment and the dark state experiment were used as control experiments (see fig. 5).
As can be seen from fig. 5, there was almost no change in the number of p.aeruginosa in the blank experiment, indicating that the effect of visible light was negligible; in the dark condition, the number of bacteria has no obvious change, which shows that the material used in the experiment has no biological toxicity. And Bi under visible light 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst shows good photocatalytic activity, and the photocatalytic sterilization performance is obviously superior to that of monomer Bi 2 S 3 And Bi 5 O 7 And I, the sterilization rate can reach 99.99 percent after 60min of illumination. Thus, Bi 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst has excellent photocatalytic sterilization antifouling performance which can be attributed to Bi 2 S 3 And Bi 5 O 7 The composition of the I forms a Z-shaped heterostructure, accelerates the separation of photoproduction electrons and holes, and improves the photocatalytic activity of the composite material.
The experimental results show that Bi prepared in example 2 and example 3 2 S 3 /Bi 5 O 7 I can also reach Bi prepared in example 1 2 S 3 /Bi 5 O 7 And I, sterilizing effect.
The above examples are only for illustrating the technical concept and features of the present invention, and are not intended to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (10)
1. Bi 2 S 3 /Bi 5 O 7 The preparation method of the IZ type heterojunction composite photocatalyst is characterized by comprising the following steps：
(1)Bi 5 O 7 Preparation of I:
adding bismuth nitrate Bi (NO) into ultrapure water 3 ) 3 ·5H 2 O, adding NaOH solution after ultrasonic dispersion, and stirring and dissolving to obtain suspension A1; adding potassium iodide KI into ultrapure water, and stirring until the potassium iodide KI is completely dissolved to obtain a dispersion liquid B1; dropwise adding the dispersion liquid B1 into the suspension liquid A1, continuously stirring to obtain a mixed liquid 1 after dropwise adding is finished, carrying out high-temperature reaction on the mixed liquid 1, cooling to room temperature after reaction, and carrying out suction filtration, washing and drying to obtain Bi with a nano-belt-shaped structure 5 O 7 I；
(2)Bi 2 S 3 /Bi 5 O 7 Preparing an IZ type heterojunction composite photocatalyst:
bi obtained in the step (1) 5 O 7 Adding the I into ultrapure water, and performing ultrasonic dispersion to obtain a dispersion liquid A2; then adding thioacetamide C 2 H 5 NS is added into ultrapure water to be completely dissolved to obtain dispersion B2; then dropwise adding the dispersion liquid B2 into the suspension liquid A2, continuously stirring to obtain a mixed liquid 2 after dropwise adding is finished, carrying out high-temperature reaction on the mixed liquid 2, cooling to room temperature after reaction, and carrying out suction filtration, washing and drying to obtain Bi 2 S 3 /Bi 5 O 7 An IZ type heterojunction composite photocatalyst.
2. The method of claim 1, wherein: in the step (1), the ultrasonic dispersion is carried out, the ultrasonic frequency is 100W-300W, and the ultrasonic dispersion time is 0.5 h-4 h; dropwise adding the dispersion liquid B1 into the suspension liquid A1, and continuously stirring for 0.5-4 h after the dropwise adding is finished to obtain a mixed liquid 1, wherein the stirring speed is 200-2000 r/min.
3. The method of claim 1, wherein: in the step (1), the concentration of the NaOH solution is 1.0-3.0 mol/L, and the pH value of the system is adjusted to 9-14 after the NaOH solution is added.
4. The method of claim 1, wherein the method comprisesIs characterized in that: in the step (1), the Bi (NO) is 3 ) 3 ·5H 2 The molar ratio of O to KI is 1: 1-5.
5. The method of claim 1, wherein: in the step (1), transferring the mixed solution 1 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, putting the reaction kettle into an electric heating constant-temperature blast drying oven, and carrying out heat treatment at 120-200 ℃ for 8-32 h to carry out high-temperature reaction; after the reaction is finished, cooling the reaction kettle to room temperature, and performing suction filtration, washing and drying to obtain Bi with a nano belt-shaped structure 5 O 7 I。
6. The method of claim 1, wherein: in the step (2), the ultrasonic dispersion is carried out, wherein the ultrasonic frequency is 100W-300W, and the ultrasonic dispersion time is 0.5-4 h; dropwise adding the dispersion liquid B2 into the suspension liquid A2, and continuously stirring for 0.5-4 hours after the dropwise adding is finished to obtain a mixed liquid 2, wherein the stirring speed is 200-2000 r/min.
7. The method of claim 1, wherein: in the step (2), the C 2 H 5 NS and Bi 5 O 7 0.1 to 10% of I: 1.
8. the method of claim 1, wherein: in the step (2), the mixed solution 2 is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and the reaction kettle is placed into an electric heating constant-temperature blast drying oven and is subjected to heat treatment at 120-200 ℃ for 8-32 hours to perform high-temperature reaction; after the reaction is finished, cooling the reaction kettle to room temperature, and obtaining Bi through suction filtration, washing and drying 2 S 3 /Bi 5 O 7 An IZ type heterojunction composite photocatalyst.
9. Bi obtained after being prepared by the preparation method of any one of claims 1 to 8 2 S 3 /Bi 5 O 7 The IZ type heterojunction composite photocatalyst is characterized in that: the above-mentionedFrom bismuth sulfide Bi 2 S 3 And bismuth-rich bismuth oxyiodide Bi 5 O 7 I composition, wherein, Bi 2 S 3 And Bi 5 O 7 The molar ratio of I is 0.1-9: 1.
10. The Bi of claim 9 2 S 3 /Bi 5 O 7 The IZ type heterojunction composite photocatalyst is applied to dye degradation or sterilization.
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