CN115090303B - Bi (Bi) 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst and preparation method and application thereof - Google Patents
Bi (Bi) 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst and preparation method and application thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
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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, bi 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst is prepared from Bi 2 S 3 And Bi (Bi) 5 O 7 I composition, wherein Bi 2 S 3 With Bi 5 O 7 The molar ratio of the I is 0.1-9:1. Bi (Bi) 2 S 3 /Bi 5 O 7 I Z the heterojunction composite photocatalyst is obtained by two steps of operations, and is prepared by a hydrothermal synthesis method 5 O 7 I, adding thioacetamide to erode, 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 I Z type heterojunction accelerates the separation of photo-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, in particular to Bi 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst, and a preparation method and application thereof belong to the technical field of photocatalysis.
Background
With the development of industrialization, global water pollution becomes more serious, and in order to cope with the significant challenge, a large number of students begin to explore environmental protection and green environmental pollution treatment methods, and particularly in 1972, tiO is found 2 After hydrogen can be decomposed by using visible light, more and more scientists begin to study photocatalytic technology to solve environmental pollution. TiO (titanium dioxide) 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 photo-generated carrier recombination rate. In order to improve the visible light catalytic activity, researchers have developed new 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 semiconductor materials have attracted attention due to their unique layered structure. The Bi-based material is formed by double layers [ Bi ] 2 O 2 ] 2+ The layered structure of the alignment assembly 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, dipoles are generated, and the response range to visible light is expanded. Among the numerous bismuth-based semiconductor materials, bi 5 O 7 I is a structural derivative of bisi, and has excellent photocatalytic activity due to a wide band gap and the presence of an I5 p hybrid orbital. In particular, bi 5 O 7 The wide band gap (2.84-2.94 eV) of I is much larger than that of BiOI, and can effectively inhibit the recombination of photogenerated carriers. However, monomeric Bi 5 O 7 I has a narrow response range to visible light, and reduces the photocatalytic activity. Therefore, further modification research is urgent, and constructing heterojunction through semiconductor recombination can widen the response range to visible light and enhance Bi 5 O 7 Photocatalytic activity of I.
Due to bismuth sulfide (Bi) 2 S 3 ) The organic light-emitting diode has a good visible light response range due to a unique layered structure and a narrower band gap width (1.3-1.7 eV), and 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 smaller, the heterojunction can be obtained by compounding the bismuth-based 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. Therefore, bi is as follows 2 S 3 With Bi 5 O 7 The heterojunction formed by the combination of the first and the second can effectively promote the separation efficiency of photo-generated carriers, enhance the utilization rate of visible light, efficiently and quickly degrade organic pollutants and kill bacteria, and has wide application prospects in the aspects of solving water pollution and marine antifouling.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art and provides a Bi 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst, preparation method and application thereof, and Bi of the invention 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst has high-efficiency photocatalytic activity and stability under visible light, and has high-efficiency killing and degrading effects on harmful microorganisms and dye pollutants in water.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention firstly provides a Bi 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst 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 With Bi 5 O 7 The molar ratio of the I is 0.1-9:1.
The invention firstly provides a 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:
bismuth nitrate Bi (NO) was added to ultrapure water 3 ) 3 ·5H 2 O, adding NaOH solution after ultrasonic dispersion, 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; then dropwise adding the dispersion liquid B1 into the suspension liquid A1, continuously stirring after the dropwise adding is finished to obtain a mixed liquid 1, carrying out high-temperature reaction on the mixed liquid 1, cooling to room temperature after the reaction, and carrying out suction filtration, washing and drying to obtain the Bi with the nano-ribbon structure 5 O 7 I；
(2)Bi 2 S 3 /Bi 5 O 7 I Z preparation of heterojunction composite photocatalyst:
the Bi obtained in the step (1) is reacted with 5 O 7 Adding I into ultrapure water, and performing ultrasonic dispersion to obtain a dispersion liquid A2; then the thioacetamide C 2 H 5 NS is added into ultrapure water to be completely dissolved, and dispersion B2 is obtained; then adding the dispersion liquid B2 into the suspension liquid A2 dropwise, continuously stirring after the dripping is finished to obtain a mixed liquid 2, carrying out high-temperature reaction on the mixed liquid 2, cooling to room temperature after the 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 is performed at a frequency of 100-300W for 0.5-4 h.
In the technical scheme, in the step (1), the concentration of the NaOH solution is 1.0-3.0 mol/L; after NaOH solution is added, the pH of the system is adjusted to 9-14.
In the above technical solution, in step (1), the Bi (NO 3 ) 3 ·5H 2 The mol 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 stirring is continued for 0.5-4 hours after the completion of the dropwise addition to obtain the mixed liquid 1, wherein the stirring speed is 200-2000 r/min.
In the above technical scheme, in the step (1), the mixed solution 1 is transferred to a solution containing polytetrafluoroethylenePlacing the reaction kettle in an electrothermal constant-temperature blast drying box, and performing heat treatment at 120-200 ℃ for 8-32 h to perform high-temperature reaction; cooling the reaction kettle to room temperature after the reaction is finished, and obtaining the Bi with the nano-ribbon structure through suction filtration, washing and drying 5 O 7 I。
In the above technical scheme, in the step (2), the ultrasonic dispersion is performed at a frequency of 100-300W for 0.5-4 h.
In the above technical solution, in 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 the mixture liquid 2 is obtained after continuous stirring for 0.5 to 4 hours after the completion of the dropwise addition, wherein the stirring speed is 200 to 2000r/min.
In the technical scheme, in the step (2), the mixed solution 2 is transferred into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and then the reaction kettle is put into an electrothermal constant-temperature blast drying box to be subjected to heat treatment at 120-200 ℃ for 8-32 h for high-temperature reaction; after the reaction is finished, cooling the reaction kettle to room temperature, and carrying out suction filtration, washing and drying to obtain Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
The invention also provides a Bi 2 S 3 /Bi 5 O 7 I Z the 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 With Bi 5 O 7 The molar ratio of the I is 0.1-9:1.
The invention also provides a Bi 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst is applied to the aspect of degrading dyes.
The invention also provides a Bi 2 S 3 /Bi 5 O 7 The I Z type heterojunction composite photocatalyst is applied to sterilization.
Compared with the prior art, the method has the following characteristics:
(1) Bi prepared by adopting a simple hydrothermal synthesis method and utilizing an in-situ ion exchange method is adopted in the invention 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst has good visible light absorption performance and photocatalysis performance, can efficiently degrade dye and kill bacteria, and has photocatalytic activity superior to Bi 2 S 3 And Bi (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 heterojunction composite photocatalyst has a Z-type 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 samples prepared in inventive example 1 and comparative example 1, wherein the abscissa is 2θ (angle) in degrees; the ordinate is density (Intensity) in a.u. (absolute units);
fig. 2-a: bi prepared in example 1 of the present invention 5 O 7 I Field Emission Scanning Electron Microscope (FESEM) photograph;
fig. 2-b: bi prepared in comparative example 1 of the present 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 (500 nm) of the sample prepared in example 1 of the present invention;
fig. 3: the ultraviolet visible diffuse reflectance spectra (UV-DRS) of the samples prepared in inventive example 1 and comparative example 1, where the abscissa is Wavelength (Wavelength), nm (nanometers), and the ordinate is Absorbance (Absorbance), a.u. (absolute units);
fig. 4: the sample prepared in example 1 of the present invention shows a Time-dependent curve of RhB concentration in the photocatalytic degradation reaction, wherein the abscissa is Time, the unit is min, and the ordinate is C t /C 0 ，C 0 To initial concentration of RhB before reaction initiation, C t RhB concentration at reaction time t (■ represents Bi) 5 O 7 I. ζ represents Bi 2 S 3 Let @ stand for Bi 2 S 3 /Bi 5 O 7 I. And represents Blank);
fig. 5: the samples prepared in example 1 of the present invention show a Time-dependent change in bacterial Survival in the photocatalytic sterilization of Pseudomonas aeruginosa, wherein the abscissa represents Time in min and the ordinate represents survivin in% (wherein ■ represents Blank and the ordinate represents Bi) 5 O 7 I. Represents Bi 2 S 3 T represents Bi 2 S 3 /Bi 5 O 7 I)。
Detailed Description
The following detailed description of the technical scheme of the present invention is provided, but the present invention is not limited to the following descriptions:
the invention is realized by mixing Bi with 2 S 3 With Bi 5 O 7 I compounding, constructing a composite material with a Z-type heterostructure, accelerating the separation of photo-generated carriers on the surface of the composite material, further improving the photocatalytic performance and aiming at Bi 2 S 3 With Bi 5 O 7 The two materials I have great significance in the practical application in the field of photocatalysis.
The technical scheme of the invention is described below with reference to specific examples:
comparative example 1:
monomer Bi 2 S 3 Comprises the following steps:
0.1mmol of Bi 5 O 7 I was added to 30mL of ultrapure water, and after ultrasonic dispersion at a frequency of 240W for 0.5 hours, an excess (30 mL: 30 mM) of C was added with continuous stirring 2 H 5 Stirring the NS solution at 800r/min for 1h, transferringIn a polytetrafluoroethylene reaction kettle with 100mL, reacting for 12h at 180 ℃, cooling to room temperature, filtering, collecting precipitate, washing with deionized water and ethanol, and drying at 60 ℃ and normal pressure to obtain Bi 2 S 3 Monomer material, designated Bi 2 S 3 。
Example 1:
bi (Bi) 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst is prepared by the following preparation method:
(1)Bi 5 O 7 preparation of I: to 40mL of ultrapure water was added 2mmol of Bi (NO) 3 ) 3 ·5H 2 O, carrying out ultrasonic dispersion for 0.5h at the frequency of 240W, and then adding 20mL of 1.5mol/L NaOH solution to obtain a dispersion liquid A1; simultaneously adding 6mmol KI into 20mL of ultrapure water, and stirring until the KI is completely dissolved to obtain a suspension B1; then adding the dispersion liquid B1 into the suspension liquid A1 dropwise, continuously stirring for 1h at 1000r/min, transferring the mixed liquid 1 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting into an electrothermal constant-temperature blast drying oven for heat treatment at 180 ℃ for 24h; then cooling the reaction kettle to room temperature, and obtaining Bi with a rod-shaped structure through suction filtration, washing and drying 5 O 7 I；
(2)Bi 2 S 3 /Bi 5 O 7 I Z preparation of heterojunction composite photocatalyst: 0.1mmol Bi obtained above was reacted with 5 O 7 Adding I into 30mL of ultrapure water, and dispersing for 0.5h under ultrasonic treatment at the frequency of 240W to obtain a dispersion liquid A2; at the same time 0.2mmol C 2 H 5 NS was added to 30mL of ultrapure water to be completely dissolved, to obtain a dispersion B2; then adding the dispersion liquid B2 into the suspension liquid A2 dropwise, continuously stirring for 1h at 1000r/min, transferring the mixed liquid 2 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting into an electrothermal constant-temperature blast drying oven for heat treatment at 180 ℃ for 12h; after the reaction is finished, cooling the reaction kettle to room temperature, and carrying out suction filtration, washing and drying to obtain Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
Samples obtained in inventive example 1 and comparative example 1The XRD pattern of the product is shown in figure 1, and as can be seen from figure 1, pure Bi 2 S 3 All diffraction peaks of (2) can be combined with Bi 2 S 3 Matching (JCPDS card number 84-0279) shows that the purity is high and the crystallization is good. For pure Bi 5 O 7 I, these diffraction peaks can be associated with bismuth-rich Bi 5 O 7 I (JCPDS card number 40-0548). Bi (Bi) 2 S 3 /Bi 5 O 7 The spectrum of the I composite material comprises Bi 2 S 3 And bismuth-rich Bi 5 O 7 All characteristic peaks of I. In addition, with pure Bi 5 O 7 Bi compared with I 2 S 3 /Bi 5 O 7 The peak position of the I composite material hardly moves, which shows that Bi 2 S 3 Load vs Bi of (2) 5 O 7 The lattice structure of I has little effect.
The scanning electron micrographs of the samples obtained in example 1 of the present invention and comparative example 1 are shown in detail in FIG. 2, and as can be seen from FIG. 2, bi 5 O 7 I is a nanoribbon structure exhibiting a width of about 1 μm. Bi (Bi) 2 S 3 Then is C 2 H 5 NS complete attack of Bi 5 O 7 I forms a nanorod-like structure having a width of about 1 μm and a thickness of about 300nm. Bi (Bi) 2 S 3 /Bi 5 O 7 The I composite shows a ribbon structure of about 1 μm in width, the surface being covered with a network of interwoven nanorods. These nanorods are Bi obtained by ion exchange reaction 2 S 3 In Bi 5 O 7 I nanoribbon surface in situ growth leading to Bi 5 O 7 I surface is coated with Bi 2 S 3 The nanorods are covered.
The UV-visible diffuse reflectance spectra of the samples obtained in example 1 of the present invention and comparative example 1 are shown in FIG. 3, and as can be seen from FIG. 3, pure Bi 2 S 3 Exhibits strong light absorption from ultraviolet to visible region, while 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 Bi compared with I 2 S 3 /Bi 5 O 7 The I composite material has wider light absorption range and stronger visible light responsivenessThis 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 I Z type heterojunction composite materials exhibit good light absorption properties for visible light, making them possible applications in photocatalysis.
Example 2:
bi (Bi) 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst is different from example 1 in that Bi (NO 3 ) 3 ·5H 2 The molar ratio of O to KI is 1:2, bi (NO 3 ) 3 ·5H 2 O、Bi 5 O 7 The ultrasonic time is 1h, the stirring time is 1.5h, the stirring speed is 800r/min, the hydrothermal reaction temperature is 160 ℃, and the ultrasonic preparation method is characterized in that the ultrasonic preparation method comprises the following steps:
(1) To 40mL of ultrapure water was added 2mmol of Bi (NO) 3 ) 3 ·5H 2 O, performing ultrasonic dispersion for 1h at the frequency of 210W, and then adding 20mL of 1.5mol/L NaOH solution to obtain a suspension A1; simultaneously adding 4mmol KI into 20mL of ultrapure water, and stirring until the KI is completely dissolved to obtain a dispersion liquid B1; then adding the dispersion liquid B1 into the suspension liquid A1 dropwise, continuously stirring for 1.5 hours at 800r/min, transferring the mixed liquid 1 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting into an electrothermal constant-temperature blast drying box for heat treatment at 160 ℃ for 24 hours; then cooling the reaction kettle to room temperature, and obtaining the Bi with the nano-ribbon structure through suction filtration, washing and drying 5 O 7 I；
(2) 0.05mmol Bi obtained in (1) 5 O 7 Adding I into 30mL of ultrapure water, and performing ultrasonic dispersion for 1h at 210W frequency to obtain a dispersion liquid A2; at the same time 0.2mmol of C 2 H 5 NS was added to 30mL of ultrapure water to be completely dissolved, to obtain a dispersion B2; then adding the dispersion liquid B2 into the suspension liquid 2A dropwise, continuously stirring for 1.5 hours at 800r/min, transferring the mixed liquid 2 into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and putting into an electrothermal constant-temperature blast drying oven for heat treatment at 160 ℃ for 12 hours; after the reaction is finished, the reaction kettle is cooled to room temperature and is subjected to suction filtrationWashing and drying to obtain Bi 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst.
Example 3:
bi (Bi) 2 S 3 /Bi 5 O 7 I Z type heterojunction composite photocatalyst is different from example 1 in that Bi (NO 3 ) 3 ·5H 2 O、Bi 5 O 7 The ultrasonic time is 1.5h, the stirring time is 2h, the stirring speed is 1200r/min, and the hydrothermal reaction time is 10h, and the ultrasonic stirring device is prepared by the following preparation method:
(1) To 40mL of ultrapure water was added 2mmol of Bi (NO) 3 ) 3 ·5H 2 O, dispersing for 1.5h under 180W frequency, then adding 20mL of 1.5mol/L NaOH solution to obtain 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 adding the dispersion liquid B1 into the suspension liquid A1 dropwise, 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 into an electrothermal constant-temperature blast drying box for heat treatment at 180 ℃ for 10 hours; then cooling the reaction kettle to room temperature, and obtaining the Bi with the nano-ribbon structure through suction filtration, washing and drying 5 O 7 I。
(2) Then 0.15mmol Bi obtained in (1) was reacted 5 O 7 Adding I into 30mL of ultrapure water, and dispersing for 1.5 hours under ultrasonic treatment at the frequency of 180W to obtain a dispersion liquid A2; at the same time 0.2mmol of C 2 H 5 NS was added to 30mL of ultrapure water to be completely dissolved, to obtain a dispersion B2; then adding the dispersion liquid B2 into the suspension liquid A2 dropwise, 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 into an electrothermal constant-temperature blast drying oven for heat treatment at 180 ℃ for 10 hours; after the reaction is finished, cooling the reaction kettle to room temperature, and carrying out suction filtration, washing and drying to obtain Bi 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 special shapeApplication of mass-junction composite photocatalyst in visible light catalytic degradation of dye pollutant rhodamine B
As can be seen from fig. 4, rhB was hardly degraded in the blank experiment and the dark experiment, and the effect on the experiment was negligible. Bi under visible light 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst shows good photocatalytic activity, and the photocatalytic performance is obviously superior to that of monomer Bi 2 S 3 And Bi (Bi) 5 O 7 I, the degradation rate of RhB can reach 100% in 90min photocatalysis reaction time. Therefore, bi having good visible light absorption property and photocatalytic activity will be 2 S 3 And Bi (Bi) 5 O 7 The Z-shaped heterostructure formed by the combination of the I can effectively separate photo-generated electrons and holes on the surface of the composite material, improves the visible light absorption performance and the specific surface area of the composite material, and enhances the visible light catalytic performance of the composite material. Bi prepared in example 2 and example 3 2 S 3 /Bi 5 O 7 I can achieve similar results as described above.
Application example 2: bi in example 1 2 S 3 /Bi 5 O 7 I Z visible light killing of Pseudomonas aeruginosa by heterojunction composite photocatalyst
The 500W xenon lamp is used as a light source, and an optical filter is used for filtering ultraviolet light, so that the wavelength range is 420-760 nm. Pseudomonas aeruginosa (P) was used.aeruginosa，2.0×10 8 cfu/mL) evaluation of Bi 2 S 3 /Bi 5 O 7 I Z visible light catalytic sterilization performance of the heterojunction composite photocatalyst.
First, a bacterial suspension was prepared, and P.aeromonas stock was inoculated into sterilized LB liquid medium, which was then placed in an air-thermostated shaker at 37℃and 150rpm, and cultured overnight. The bacterial suspension obtained by cultivation was centrifuged and suspended in 0.01mol/L PBS (pH=7.4) buffer to give a concentration of 2.0X10 8 cfu/mL of P.aerocosa bacterial suspension. In the photocatalysis experiment, 49.5mL of sterilized 0.01mol/L PBS (pH=7.4) buffer solution is added into a 50mL reactor, and then 500 mu L of bacterial suspension is added to ensure that the bacterial concentration in the reaction solution is 2.0x10 6 cfu/mL, 50mg of Bi prepared in example 1 was added 2 S 3 /Bi 5 O 7 I catalyst. And (3) carrying out photocatalysis reaction after the dark state adsorption reaches equilibrium, sampling for a certain time in the reaction process, and determining the survival rate and the sterilization rate of bacteria by a plate counting method. The method comprises the following specific steps: 1.0mL of the reaction solution was diluted in sequence with 0.01mol/L PBS (pH=7.4) buffer according to a serial dilution method, and 100. Mu.L of the solution with different dilution factors was taken out to the prepared LB solid medium, and the bacterial liquid was uniformly smeared on the LB medium. Inverting LB culture medium, placing in an electrothermal constant temperature incubator for culturing for 24 hours at 37 ℃, and obtaining bacterial concentration by counting the number of bacterial colonies growing on the culture medium and corresponding dilution factors so as to determine the survival rate and the sterilization rate of bacteria. Each group of experiments was run in parallel 3 times, with the average value taken as the final result and the blank and dark experiments as the control experiments (see fig. 5).
As can be seen from fig. 5, there was little change in the number of p.aerobosa in the blank experiment, indicating that the effect of visible light was negligible; in the dark condition, the number of bacteria is not changed obviously, which indicates that the material used in the experiment has no biological toxicity. And Bi under visible light 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst shows good photocatalytic activity, and photocatalytic sterilization performance is obviously superior to that of monomer Bi 2 S 3 And Bi (Bi) 5 O 7 I, the illumination sterilization rate after 60min can reach 99.99 percent. Therefore, bi 2 S 3 /Bi 5 O 7 I Z heterojunction composite photocatalyst has excellent photocatalytic sterilization and antifouling properties, which can be attributed to Bi 2 S 3 And Bi (Bi) 5 O 7 The composite of I forms a Z-shaped heterostructure, accelerates the separation of photo-generated electrons and holes, and improves the photocatalytic activity of the composite material.
Experimental results show that Bi prepared in example 2 and example 3 2 S 3 /Bi 5 O 7 I can also achieve Bi prepared in example 1 2 S 3 /Bi 5 O 7 I sterilization effect.
The foregoing examples are merely illustrative of the technical concept and technical features of the present invention, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made according to the essence of the present invention should be included in the scope of the present invention.
Claims (10)
1.Bi (Bi) 2 S 3 /Bi 5 O 7 The preparation method of the IZ heterojunction composite photocatalyst is characterized by comprising the following steps of:
(1)Bi 5 O 7 preparation of I:
bismuth nitrate Bi (NO) was added to ultrapure water 3 ) 3 ·5H 2 O, adding NaOH solution after ultrasonic dispersion, 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; then dropwise adding the dispersion liquid B1 into the suspension liquid A1, continuously stirring after the dropwise adding is finished to obtain a mixed liquid 1, carrying out high-temperature reaction on the mixed liquid 1, cooling to room temperature after the reaction, and carrying out suction filtration, washing and drying to obtain the Bi with the nano-ribbon structure 5 O 7 I；
(2)Bi 2 S 3 /Bi 5 O 7 Preparation of IZ type heterojunction composite photocatalyst:
the Bi obtained in the step (1) is reacted with 5 O 7 Adding I into ultrapure water, and performing ultrasonic dispersion to obtain a dispersion liquid A2; then the thioacetamide C 2 H 5 NS is added into ultrapure water to be completely dissolved, and dispersion B2 is obtained; then adding the dispersion liquid B2 into the suspension liquid A2 dropwise, continuously stirring after the dripping is finished to obtain a mixed liquid 2, carrying out high-temperature reaction on the mixed liquid 2, cooling to room temperature after the reaction, and carrying out suction filtration, washing and drying to obtain Bi 2 S 3 /Bi 5 O 7 IZ type heterojunction composite photocatalyst.
2. The method of manufacturing according to claim 1, characterized in that: 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; and (3) dropwise adding the dispersion liquid B1 into the suspension liquid A1, and continuously stirring for 0.5-4 hours 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 manufacturing according to claim 1, characterized in that: 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 manufacturing according to claim 1, characterized in that: in step (1), the Bi (NO) 3 ) 3 ·5H 2 The mol ratio of O to KI is 1:1-5.
5. The method of manufacturing according to claim 1, characterized in that: in the step (1), the mixed solution 1 is transferred into a high-pressure reaction kettle with a polytetrafluoroethylene lining, and then the reaction kettle is put into an electrothermal constant-temperature blast drying box to be subjected to heat treatment for 8-32 h at 120-200 ℃ for high-temperature reaction; cooling the reaction kettle to room temperature after the reaction is finished, and obtaining the Bi with the nano-ribbon structure through suction filtration, washing and drying 5 O 7 I。
6. The method of manufacturing according to claim 1, characterized in that: in the step (2), the ultrasonic dispersion is carried out, the ultrasonic frequency is 100W-300W, and the ultrasonic dispersion time is 0.5-4 h; and (3) dropwise adding the dispersion liquid B2 into the suspension liquid A2, and continuously stirring for 0.5-4 h 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 manufacturing according to claim 1, characterized in that: 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 manufacturing according to claim 1, characterized in that: in the step (2), the mixed solution 2 is transferred to a high-pressure reaction kettle with a polytetrafluoroethylene lining, and then the reaction kettle is put into an electrothermal constant-temperature blast drying box to be subjected to heat treatment at 120-200 ℃ for 8-32 h for high-temperature reaction; after the reaction is finished, cooling the reaction kettle to room temperature, and carrying out suction filtration, washing and drying to obtain Bi 2 S 3 /Bi 5 O 7 IZ type heterojunction composite photocatalyst.
9. Bi obtained after the preparation by the preparation method according to any one of claims 1 to 8 2 S 3 /Bi 5 O 7 The IZ heterojunction composite photocatalyst is characterized in that: the catalyst 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 With Bi 5 O 7 The molar ratio of the I is 0.1-9:1.
10. A Bi according to claim 9 2 S 3 /Bi 5 O 7 Application of IZ type heterojunction composite photocatalyst in degrading dye or sterilizing.
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