CN114210318A - Novel BiSnSbO6-ZnO photocatalytic composite material and preparation method and application thereof - Google Patents
Novel BiSnSbO6-ZnO photocatalytic composite material and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
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- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
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- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
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Abstract
The invention discloses a novel BiSnSbO6a-ZnO photocatalytic composite material, a preparation method and application thereof, relating to the technical field of environmental protection. The invention adopts a solid-phase sintering method to carry out the preparation of ZnO negative ions with smaller particle sizeBiSnSbO carried on large-particle-size material6In the above, the prepared novel BiSnSbO6The ZnO photocatalytic composite material can absorb ultraviolet light and visible light, has good antibacterial performance on pathogenic microorganisms, greatly improves the luminous energy utilization efficiency of the composite photocatalytic material and the antibacterial efficiency on the pathogenic microorganisms, and is suitable for popularization and application in the market.
Description
Technical Field
The invention relates to the technical field of environmental protection, relates to preparation and application of a photocatalytic composite material, and particularly discloses a novel BiSnSbO6A preparation method of the-ZnO photocatalytic composite material and application thereof in the aspect of antibiosis.
Background
With the rapid development of economic level, people's requirements for green and healthy life are higher and higher, and environmental problems become one of the important problems concerned by people. And the problems of microbial pollution, formaldehyde pollution and the like directly affect the living environment and pose serious threats to the human health. Although people can utilize the benefits of microorganisms to brew, generate electricity by bacteria and the like, the harmfulness of the microorganisms threatens the health of people at all times. Although the traditional antibacterial methods such as high-temperature sterilization, ultraviolet radiation and antibiotic sterilization have good effects, the traditional antibacterial methods have the limitations of being easy to cause cancers, not environment-friendly and the like. Therefore, the development of the antibacterial material with low cost and safety is of great significance.
However, as a new antibacterial technology, compared with the existing widely used antibacterial technology of chemical antibacterial agents, the photocatalytic antibacterial material can avoid or reduce the formation of potential toxic antibacterial byproducts as much as possible, and in the antibacterial process, sunlight, fluorescent lamps, ultraviolet lamps, LED lamps and the like can be used as excitation light sources to hydrolyze water into hydrogen and oxygen to generate active oxygen groups with strong oxidizability, such as hydroxyl radicals and the like, wherein the active oxygen groups can destroy the cell structure of bacteria, degrade toxic products released by the bacteria, inactivate viruses, remove various organic pollutants, cannot cause pollution and secondary pollution to soil and water quality, is an efficient and broad-spectrum antibacterial technology, has a good antibacterial effect, and is not easy to generate drug resistance. Therefore, the method has wide application prospect in the direction of environmental management caused by pathogenic microorganisms.
Among numerous photocatalytic semiconductor materials, ZnO is widely used in research on photocatalytic degradation of organic pollutants, killing of pathogenic microorganisms, and the like due to its characteristics of low cost, high photosensitivity, and the like. However, ZnO has a wide forbidden band width (Eg ═ 3.3eV), and can only be excited by ultraviolet light which accounts for a relatively small amount of sunlight, that is, most of sunlight cannot be utilized, which greatly limits practical applications of ZnO. In addition, the rapid recombination of the photogenerated carriers is not beneficial to the improvement of the photocatalytic performance of ZnO. Therefore, for the ZnO-based photocatalyst, the increase of the absorption range of the ZnO-based photocatalyst to light and the promotion of the separation of photogenerated electrons and holes are beneficial to the improvement of the photocatalytic performance of the ZnO-based photocatalyst.
Therefore, the problem to be solved by the technical personnel in the field is how to develop a novel photocatalytic antibacterial composite material to improve the utilization efficiency of light energy and the bacteriostatic efficiency of the material to pathogenic microorganisms.
Disclosure of Invention
In view of the above, the present invention provides a novel BiSnSbO to solve the problems in the prior art6-ZnO photocatalytic composite material and preparation method and application thereof.
The photocatalytic composite material prepared by the method has good antibacterial efficiency on pathogenic microorganisms under the illumination condition, and shows wide application prospect.
In order to achieve the purpose, the technical scheme of the invention is as follows:
BiSnSbO6The preparation method of the photocatalytic material specifically comprises the following steps:
weighing powdery raw material Bi according to molar ratio2O3、SnO2And Sb2O5Uniformly mixing, grinding, drying, roasting, cooling and uniformly grinding to obtain the BiSnSbO6A photocatalytic material.
Preferably, said Bi2O3、SnO2And Sb2O5The molar ratio of (1: 2: 1), the drying temperature is 200 ℃, and the time is 4 hours.
And the roasting operation is as follows:
a. raising the temperature in the high-temperature sintering furnace from 20 ℃ to 350 ℃ for 80 min;
b. keeping the temperature at 350 ℃ for 240 min;
c. raising the temperature of the furnace from 350 ℃ to 720 ℃ for 80 min;
d. keeping the temperature at 720 ℃ for 240 min;
e. heating the furnace from 720 ℃ to 900 ℃ for 60 min;
f. preserving heat at 900 ℃ for 1500min, cooling along with the furnace, taking out the powder, and grinding the powder uniformly to obtain pure BiSnSbO6A photocatalytic material.
In addition, the invention also requests to protect a novel BiSnSbO6The preparation method of the-ZnO photocatalytic composite material specifically comprises the following steps:
ZnO and BiSnSbO prepared by the method are respectively weighed according to molar ratio6Uniformly mixing, grinding and roasting to obtain the BiSnSbO6-ZnO photocatalytic composite material.
Wherein the ZnO and the BiSnSbO6The molar ratio of (1) to (2) to (1) to (3) to (4) to (1); and the specific operation of roasting is as follows:
a. raising the temperature in the high-temperature sintering furnace from 20 ℃ to 900 ℃ for 200 min;
b. preserving heat at 900 ℃ for 1500min, cooling along with the furnace, taking out the powder, grinding uniformly to finally obtain pure BiSnSbO6-ZnO photocatalytic composite material.
In addition, the invention also requests to protect the novel BiSnSbO prepared by the method6-ZnO photocatalytic composite material, said BiSnSbO6the-ZnO photocatalytic composite material has antibacterial performance, and ZnO with small particle size is loaded on BiSnSbO with large particle size6The above.
And, it is yet another object of the present invention to provide a novel BiSnSbO6-application of ZnO photocatalytic composite material in living environment.
Further, the application further comprises: the novel BiSnSbO6The ZnO photocatalytic composite material has antibacterial application to pathogenic microorganism bacteria and fungi.
According to the technical scheme, compared with the prior art, the novel BiSnSbO is provided6the-ZnO photocatalytic composite material and the preparation method and the application thereof have the following excellent effects:
firstly, the powdered BiSnSbO successfully prepared by the last method6The ZnO photocatalytic composite material increases the contact area of the active site and pathogenic microorganisms due to the increase of the specific surface area of the material, so that the ZnO photocatalytic composite material has good photocatalytic antibacterial performance when treating the pathogenic microorganisms;
secondly, BiSnSbO6And ZnO are used for constructing the II-type heterojunction composite photocatalytic material, so that the specific surface area of the composite photocatalytic material is further increased, the absorption effect of ZnO on ultraviolet light and BiSnSbO are fully exerted6The absorption effect on visible light is realized, and the photocatalytic performance of the composite photocatalytic material is further improved.
In conclusion, the catalytic material prepared by the method disclosed by the invention has excellent photocatalytic activity and good antibacterial performance on pathogenic microorganisms, so that the luminous energy utilization efficiency of the composite photocatalytic material and the antibacterial efficiency on the pathogenic microorganisms are greatly improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 shows BiSnSbO prepared in example 4 of the present invention6-XRD pattern of ZnO photocatalytic composite material.
FIG. 2 shows BiSnSbO prepared in example 4 of the present invention6SEM spectra of ZnO photocatalytic composite material.
FIG. 3 shows BiSnSbO prepared in example 4 of the present invention6-the diffuse reflectance spectrum of ultraviolet and visible of the ZnO photocatalytic composite.
FIG. 4 shows BiSnSbO prepared in example 4 of the present invention6The sterilization capability of the ZnO photocatalytic composite material to sewage.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a novel BiSnSbO6A preparation method of-ZnO photocatalytic composite material.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
The technical solution of the present invention will be further described with reference to the following specific examples.
Example 1:
the powdery catalytic material is BiSnSbO6Photocatalytic material, and said BiSnSbO6The preparation method of the photocatalytic material is a solid-phase sintering method, and comprises the following steps:
1) push buttonMolar ratio of Bi2O3：SnO2：Sb2O5Weighing powdery raw materials according to the proportion of 1:2:1, uniformly mixing and grinding;
2) keeping the temperature in a drying oven at 200 ℃ for 4 h;
3) drying, and placing into corundum crucibles, wherein the powder height in each corundum crucible is about 0.1-0.2 cm;
4) putting the corundum crucible into a high-temperature muffle furnace for sintering;
5) finally, pure single-phase BiSnSbO is obtained6A powdered catalytic material.
Wherein, the sintering process is as follows:
a. raising the temperature in the high-temperature sintering furnace from 20 ℃ to 350 ℃ for 80 min;
b. keeping the temperature at 350 ℃ for 240 min;
c. raising the temperature of the furnace from 350 ℃ to 720 ℃ for 80 min;
d. keeping the temperature at 720 ℃ for 240 min;
e. heating the furnace from 720 ℃ to 900 ℃ for 60 min;
f. preserving heat at 900 ℃ for 1500min, cooling along with the furnace, taking out the powder, and grinding the powder uniformly to obtain pure BiSnSbO6A photocatalytic material.
Example 2 to example 4: preparation of different raw material proportions
The powdery composite photocatalytic material is BiSnSbO6-ZnO composite photocatalytic material, and BiSnSbO6The preparation method of the-ZnO composite photocatalytic material is a solid-phase sintering method, and comprises the following steps:
1) BiSnSbO according to molar ratio6Weighing powder materials according to the proportion of 1:2, 1:3 and 1:4, and then uniformly mixing and grinding the powder materials;
2) placing into corundum crucibles, wherein the height of the powder in each corundum crucible is about 0.1-0.2 cm;
3) putting the corundum crucible into a high-temperature muffle furnace for sintering;
4) finally, pure BiSnSbO is obtained6-ZnO photocatalytic composite material.
Wherein, the sintering process is as follows:
a. raising the temperature in the high-temperature sintering furnace from 20 ℃ to 900 ℃ for 200 min;
b. preserving heat at 900 ℃ for 1500min, cooling along with the furnace, taking out the powder, grinding uniformly to finally obtain pure BiSnSbO6-ZnO photocatalytic composite material.
In addition, to further verify and demonstrate the excellent effects of the technical scheme of the invention compared with the prior art, the BiSnSbO prepared in the example 4 is subjected to series of characterization and performance tests on the photocatalytic composite material prepared in the invention6-ZnO photocatalytic composite material (BiSnSbO)6The mol ratio of ZnO to ZnO is 1:4) is applied to the antibacterial field, and the specific content is as follows:
wherein ZnO and BiSnSbO are used as the main components6The materials with the molar ratio of 2:1 and 3:1 are found to have aggregation phenomenon through SEM, so that ZnO and BiSnSbO are adopted in subsequent antibacterial experiments6Of a 4:1 molar ratio of the component (a) may cause agglomeration due to BiSnSbO6Aggregation may occur during high-temperature sintering for a long time. One, BiSnSbO6Characterization of the Properties of the-ZnO photocatalytic composite Material
BiSnSbO prepared as in example 46And (4) detecting the ZnO photocatalytic composite material.
The original material for the test is high in purity, and can be observed through X-ray diffraction spectrum, scanning electron microscope and transmission electron microscope, namely BiSnSbO6And ZnO are compounded together, and BiSnSbO6The shape of the-ZnO photocatalytic composite material is irregular, and ZnO with smaller grain diameter is loaded on BiSnSbO with larger grain diameter6Above (see FIG. 2), BiSnSbO6The average particle size of the-ZnO photocatalytic composite material is about 2-4 microns.
And BiSnSbO is subjected to double-wavelength ultraviolet visible diffuse reflection spectrometer6The characteristic absorption edge of the ZnO photocatalytic composite material generated under the condition of light irradiation is measured (shown in figure 3), BiSnSbO6The forbidden band width of the ZnO photocatalytic composite material is 2.81 eV; and after the forbidden bandwidth is known, BiSnSbO can be obtained by calculation with a formula6VB and CB of (a) are 3.29eV and 0.51eV, respectively, and VB and CB of ZnO are 2.83eV and-0.31 eV, respectively. VB and CB average ratio of ZnOBiSnSbO6Is more negative than the VB and CB energy bands, so that a type II heterojunction structure can be formed, so that-Can be transferred from ZnO to BiSnSbO6And h is+Can be obtained from BiSnSbO6Migrate to ZnO, promote the effective separation of electron-hole pairs and enhance the photocatalytic activity.
Second, antibacterial property against Escherichia coli
1. By using BiSnSbO6-ZnO photocatalytic composite material for inhibiting escherichia coli
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. The cultured cell suspension was transferred to a beaker containing a sample, and the bacteria were allowed to contact the sample sufficiently (sample concentrations: 125mg/L, 250mg/L, 500mg/L, and 1g/L, respectively). Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an LB liquid culture medium, shaking up, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator, and carrying out inverted culture under the culture conditions that: the temperature is 37 ℃ and the time is 18 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel. And finally, according to the change of the number of the bacterial colonies at different time points of illumination, a time-antibacterial efficiency curve chart is made.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
The experimental result shows that BiSnSbO is used as the material6Under the irradiation of light of the ZnO photocatalytic composite material, along with the prolonging of irradiation time, the antibacterial efficiency of the composite material with different concentrations is gradually enhanced, wherein the antibacterial effect of the composite material with the concentration of 500mg/L on escherichia coli is the best, and 99.63% is achieved within 6 h. The detailed data are shown in Table 1.
TABLE 1 BiSnSbO6Data related to antibacterial efficiency of-ZnO photocatalytic composite material on escherichia coli
2. By using BiSnSbO6Photocatalytic material for inhibiting escherichia coli
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. And (3) transferring the bacterial liquid from the cultured bacterial liquid, adding the bacterial liquid into a beaker containing a sample to ensure that the bacteria are fully contacted with the sample, and selecting the concentration of the sample to be 500mg/L according to the antibacterial efficiency of the composite material with different concentrations. Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an LB liquid culture medium, shaking up, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator, and carrying out inverted culture under the culture conditions that: the temperature is 37 ℃ and the time is 18 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
The experimental result shows that BiSnSbO is used as the material6Under the irradiation of the photocatalysis material light, the antibacterial efficiency of the composite material with different concentrations is gradually enhanced along with the extension of the irradiation time, wherein the concentration of 500mg/L BiSnSbO6The antibacterial effect of the photocatalytic material on escherichia coli reaches 64.17% after 6 hours of illumination. The data are summarized in Table 2.
TABLE 2 BiSnSbO6Data related to antibacterial efficiency of photocatalytic material on escherichia coli
| Illumination time (h) | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 500mg/L | 0.00％ | 0.00％ | 16.86％ | 17.08％ | 51.19％ | 0.00％ | 64.17％ |
3. Inhibiting escherichia coli by adopting ZnO photocatalytic material
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. And (3) transferring the bacterial liquid from the cultured bacterial liquid, adding the bacterial liquid into a beaker containing a sample to ensure that the bacteria are fully contacted with the sample, and selecting the concentration of the sample to be 500mg/L according to the antibacterial efficiency of the composite material with different concentrations. Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an LB liquid culture medium, shaking up, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator, and carrying out inverted culture under the culture conditions that: the temperature is 37 ℃ and the time is 18 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
Experimental results show that under the irradiation of the ZnO photocatalytic material, along with the prolonging of the irradiation time, the antibacterial efficiency of the composite material with different concentrations is gradually enhanced, wherein the antibacterial effect of the ZnO photocatalytic material with the concentration of 500mg/L on escherichia coli reaches 28.57% when the ZnO photocatalytic material is irradiated for 2 hours. The data are summarized in Table 3.
TABLE 3 data relating to the antibacterial efficiency of ZnO photocatalytic material to Escherichia coli
| Illumination time (h) | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 500mg/L | 0.00％ | 0.00％ | 28.57％ | 18.03％ | 0.00％ | 16.67％ | 11.74％ |
The three different photocatalytic materials are adopted to carry out an antibacterial experiment on escherichia coli, and the specific comparative analysis is as follows: respectively using BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6And the anti-colibacillus performance of the two single photocatalytic materials ZnO are compared, and BiSnSbO is utilized on the premise of consistent initial conditions6The photocatalytic material inhibits escherichia coli under the LED illumination condition, and the optimal antibacterial efficiency of the photocatalytic material on the escherichia coli reaches 64.17% after 6 hours. The ZnO photocatalytic material is used for inhibiting escherichia coli under the LED illumination condition, and the optimal antibacterial efficiency on the escherichia coli reaches 28.57% within 2 hours. Under the same initial conditions, BiSnSbO is utilized6The best antibacterial efficiency of the-ZnO photocatalytic composite material to escherichia coli is 100% under the LED illumination condition for 6 hours. In the comparison of BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6And the antibacterial efficiency of the ZnO single photocatalytic material to escherichia coli can be obviously shown, namely BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6The antibacterial efficiency of two single photocatalytic materials of ZnO is much higher, so that BiSnSbO can be seen6the-ZnO photocatalytic composite material has better photocatalytic antibacterial activity.
In conclusion, BiSnSbO, which destroys the intact morphology of cells during the photocatalytic antibacterial process under the same initial conditions6-ZnO photocatalytic composite material ratio BiSnSbO6And the ZnO single photocatalytic material has good performance and high efficiency.
Second, antibacterial property against staphylococcus aureus
1. By using BiSnSbO6-ZnO photocatalytic composite material for inhibiting staphylococcus aureus
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. The cultured cell suspension was transferred to a beaker containing a sample, and the bacteria were allowed to contact the sample sufficiently (sample concentrations: 125mg/L, 250mg/L, 500mg/L, and 1g/L, respectively). Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an LB liquid culture medium, shaking up, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator, and carrying out inverted culture under the culture conditions that: the temperature is 37 ℃ and the time is 18 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel. And finally, according to the change of the number of the bacterial colonies at different time points of illumination, a time-antibacterial efficiency curve chart is made.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
The experimental result shows that BiSnSbO is used as the material6Under the irradiation of light of the ZnO photocatalytic composite material, the antibacterial efficiency of the composite material with different concentrations is gradually enhanced along with the extension of the irradiation time, wherein the antibacterial effect of the composite material with the concentration of 500mg/L on staphylococcus aureus is the best, and the antibacterial effect reaches 100% after the composite material is irradiated for 4 hours. The data are summarized in Table 4.
TABLE 4 BiSnSbO6Data related to antibacterial efficiency of ZnO photocatalytic composite material on staphylococcus aureus
2. By using BiSnSbO6Photocatalytic material for inhibiting staphylococcus aureus
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. And (3) transferring the bacterial liquid from the cultured bacterial liquid, adding the bacterial liquid into a beaker containing a sample to ensure that the bacteria are fully contacted with the sample, and selecting the concentration of the sample to be 500mg/L according to the antibacterial efficiency of the composite material with different concentrations. Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an LB liquid culture medium, shaking up, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator, and carrying out inverted culture under the culture conditions that: the temperature is 37 ℃ and the time is 18 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
The experimental result shows that BiSnSbO is used as the material6Under the irradiation of the photocatalysis material light, the antibacterial efficiency of the composite material with different concentrations is gradually enhanced along with the extension of the irradiation time, wherein the concentration of 500mg/L BiSnSbO6The antibacterial effect of the photocatalytic material on staphylococcus aureus reaches 19.2% after 1 hour of illumination. The data are summarized in Table 5.
TABLE 5 BiSnSbO6Data related to antibacterial efficiency of photocatalytic material on staphylococcus aureus
| Illumination time (h) | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 500mg/L | 0.00％ | 19.20％ | 11.60％ | 0.00％ | 3.80％ | 21.60％ | 18.60％ |
3. Inhibiting staphylococcus aureus by ZnO photocatalysis material
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. And (3) transferring the bacterial liquid from the cultured bacterial liquid, adding the bacterial liquid into a beaker containing a sample to ensure that the bacteria are fully contacted with the sample, and selecting the concentration of the sample to be 500mg/L according to the antibacterial efficiency of the composite material with different concentrations. Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an LB liquid culture medium, shaking up, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator, and carrying out inverted culture under the culture conditions that: the temperature is 37 ℃ and the time is 18 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
Experimental results show that under the irradiation of the ZnO photocatalytic material, the antibacterial efficiency of the composite material with different concentrations is gradually enhanced along with the extension of the irradiation time, wherein the antibacterial effect of the ZnO photocatalytic material with the concentration of 500mg/L on staphylococcus aureus reaches 84.79% when the ZnO photocatalytic material is irradiated for 6 hours. The data are summarized in Table 3.
TABLE 6 data relating to the antibacterial efficiency of ZnO photocatalytic material against Staphylococcus aureus
The three different photocatalytic materials are adopted to carry out an antibacterial experiment on staphylococcus aureus, and the specific comparative analysis is as follows: respectively using BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6And the performances of the two single photocatalytic materials of ZnO against staphylococcus aureus are compared, and BiSnSbO is utilized on the premise of consistent initial conditions6The photocatalytic material inhibits staphylococcus aureus under the condition of LED illumination, and the optimal antibacterial efficiency of the photocatalytic material to staphylococcus aureus reaches 19.2% within 1 hour. The ZnO photocatalytic material is used for inhibiting staphylococcus aureus under the LED illumination condition, and the optimal antibacterial efficiency of the ZnO photocatalytic material on the staphylococcus aureus reaches 84.79% in 6 hours. Under the same initial conditions, BiSnSbO is utilized6The best antibacterial efficiency of the-ZnO photocatalytic composite material to staphylococcus aureus is 100% under the LED illumination condition for 4 hours. In the comparison of BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6And the antibacterial efficiency of the ZnO single photocatalytic material to staphylococcus aureus can be obviously shown, and BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6The antibacterial efficiency of two single photocatalytic materials of ZnO is much higher, so that BiSnSbO can be seen6the-ZnO photocatalytic composite material has better photocatalytic antibacterial activity.
Third, the antibacterial property to candida albicans
1. By using BiSnSbO6-ZnO photocatalytic composite material for inhibiting candida albicans
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. The cultured cell suspension was transferred to a beaker containing a sample, and the bacteria were allowed to contact the sample sufficiently (sample concentrations: 125mg/L, 250mg/L, and 500mg/L, respectively). Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an improved Martinus liquid culture medium, shaking uniformly, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator for inverted culture, wherein the culture conditions are as follows: the temperature is 28 ℃ and the time is 48 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel. And finally, according to the change of the number of the bacterial colonies at different time points of illumination, a time-antibacterial efficiency curve chart is made.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
The experimental result shows that BiSnSbO is used as the material6Under the irradiation of light of the ZnO photocatalytic composite material, the antibacterial efficiency of the composite material with different concentrations is gradually enhanced along with the prolonging of the irradiation time, wherein the antibacterial effect of the composite material with the concentration of 250mg/L on Candida albicans is the best, and the highest antibacterial effect reaches 62.5 percent when the composite material is irradiated for 4 hours. The data are summarized in Table 7.
TABLE 7 BiSnSbO6Data relating to the antibacterial efficiency of ZnO photocatalytic composite material to Candida albicans
2. By using BiSnSbO6Photocatalytic material for inhibiting candida albicans
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. And (3) transferring the bacterial liquid from the cultured bacterial liquid, adding the bacterial liquid into a beaker containing a sample to ensure that the bacteria are fully contacted with the sample, and selecting the concentration of the sample to be 250mg/L according to the antibacterial efficiency of the composite material with different concentrations. Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an improved Martinus liquid culture medium, shaking uniformly, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator for inverted culture, wherein the culture conditions are as follows: the temperature is 28 ℃ and the time is 48 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
The experimental result shows that BiSnSbO is used as the material6BiSnSbO with the concentration of 250mg/L under the irradiation of light of a photocatalytic material6The antibacterial effect of the photocatalytic material on the candida albicans reaches 46.90% after 1 hour of illumination. The data are summarized in Table 8.
TABLE 8 BiSnSbO6Data related to antibacterial efficiency of photocatalytic material on candida albicans
| Illumination time (h) | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 500mg/L | 0.00％ | 46.90％ | 32.80％ | 4.90％ | 0.00％ | 0.00％ | 28.60％ |
3. Method for inhibiting candida albicans by using ZnO photocatalytic material
The antibacterial performance of the material is measured by adopting a gradient dilution method and a flat plate bacterial colony counting method. The photocatalytic antibacterial experiment process comprises the following steps: weighing a sample, adding the sample into a beaker, adding 0.9% NaCl solution, and performing ultrasonic treatment to uniformly disperse and dissolve the sample. And (3) transferring the bacterial liquid from the cultured bacterial liquid, adding the bacterial liquid into a beaker containing a sample to ensure that the bacteria are fully contacted with the sample, and selecting the concentration of the sample to be 500mg/L according to the antibacterial efficiency of the composite material with different concentrations. Starting illumination and timing, respectively taking samples illuminating different time points under a 35W LED lamp, respectively sampling 1mL of mixed solution at each time point, diluting the mixed solution to a proper concentration by using an improved Martinus liquid culture medium, shaking uniformly, uniformly coating 100 mu L of the mixed solution on a culture dish, putting the mixed solution in a constant-temperature incubator for inverted culture, wherein the culture conditions are as follows: the temperature is 28 ℃ and the time is 48 h. The experiment was set up as a control group. All experimental results are the average of the number of colonies grown after three experiments in parallel.
The antibacterial efficiency is (number of colonies illuminated by light without adding the sample-number of colonies illuminated by the added sample)/number of colonies illuminated by light without adding the sample x 100%
Experimental results show that the antibacterial effect of the ZnO photocatalytic material with the concentration of 250mg/L on Candida albicans reaches 11.76% when the ZnO photocatalytic material is irradiated for 3 hours. The data are summarized in Table 9.
TABLE 9 data relating to the antibacterial efficiency of ZnO photocatalytic material against Candida albicans
| Illumination time (h) | 0 | 1 | 2 | 3 | 4 | 5 | 6 |
| 500mg/L | 0.00％ | 0.00％ | 0.00％ | 11.76％ | 0.00％ | 0.00％ | 0.00％ |
The three different photocatalytic materials are adopted to carry out antibacterial experiments on the Candida albicans, and specific comparative analysis is carried out, such asThe following: respectively using BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6And the performance of the ZnO single photocatalytic material against Candida albicans is compared, and BiSnSbO is utilized on the premise of consistent initial conditions6The photocatalytic material inhibits candida albicans under the LED illumination condition, and the optimal antibacterial efficiency on the candida albicans reaches 46.9% within 1 hour. The ZnO photocatalytic material is used for inhibiting candida albicans under the LED illumination condition, and the optimal antibacterial efficiency on the candida albicans reaches 11.76% when the time is 3 hours. Under the same initial conditions, BiSnSbO is utilized6The best antibacterial efficiency of the-ZnO photocatalytic composite material to the golden candida albicans is 62.5% under the LED illumination condition for 4 hours. In the comparison of BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6And the antibacterial efficiency of the ZnO single photocatalytic material to staphylococcus aureus can be obviously shown, and BiSnSbO6-ZnO photocatalytic composite material and BiSnSbO6The antibacterial efficiency of two single photocatalytic materials of ZnO is much higher, so that BiSnSbO can be seen6the-ZnO photocatalytic composite material has better photocatalytic antibacterial activity.
In conclusion, BiSnSbO is generated in the photocatalysis antibacterial process under the same initial conditions6-ZnO photocatalytic composite material ratio BiSnSbO6And the ZnO single photocatalytic material has good performance and high efficiency. And synthesized BiSnSbO6The ZnO photocatalytic composite material also has an antibacterial effect on fungi with more complex forms.
Furthermore, the prepared material is used for the antibacterial research of the domestic wastewater by combining the earlier theoretical data on the antibacterial aspect, and the prepared material can effectively inhibit or kill pathogenic microorganisms in the wastewater. BiSnSbO as shown in FIG. 36After the sewage diluted by a certain multiple is treated by the ZnO photocatalytic composite material, the treated water (100 microliters) is smeared on a solid flat plate. The antibacterial effect was evaluated by colony counting. Bacterial colonies in the wastewater were significantly reduced and disappeared. The results show that BiSnSbO6the-ZnO photocatalytic composite material has good antibacterial effect on pathogenic microorganisms.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. BiSnSbO6The preparation method of the photocatalytic material is characterized by comprising the following steps:
weighing powdery raw material Bi according to molar ratio2O3、SnO2And Sb2O5Uniformly mixing, grinding, drying, roasting, cooling and uniformly grinding to obtain the BiSnSbO6A photocatalytic material.
2. The BiSnSbO of claim 16The preparation method of the photocatalytic material is characterized in that the Bi2O3、SnO2And Sb2O5The molar ratio of (1: 2: 1), the drying temperature is 200 ℃, and the time is 4 hours.
3. The BiSnSbO of claim 16The preparation method of the photocatalytic material is characterized in that the roasting specifically comprises the following steps:
a. raising the temperature in the high-temperature sintering furnace from 20 ℃ to 350 ℃ for 80 min;
b. keeping the temperature at 350 ℃ for 240 min;
c. raising the temperature of the furnace from 350 ℃ to 720 ℃ for 80 min;
d. keeping the temperature at 720 ℃ for 240 min;
e. heating the furnace from 720 ℃ to 900 ℃ for 60 min;
f. preserving heat at 900 ℃ for 1500min, cooling along with the furnace, taking out the powder, and grinding the powder uniformly to obtain pure BiSnSbO6A photocatalytic material.
4. Novel BiSnSbO6The preparation method of the ZnO photocatalytic composite material is characterized by comprising the following steps:
separately weighing ZnO and BiSnSbO prepared by the method of claim 1 according to molar ratio6Uniformly mixing, grinding and roasting to obtain the BiSnSbO6-ZnO photocatalytic composite material.
5. The novel BiSnSbO of claim 46The preparation method of the-ZnO photocatalytic composite material is characterized in that ZnO and BiSnSbO are used6The molar ratio of (A) to (B) is 2:1, 3:1 and 4: 1.
6. The novel BiSnSbO of claim 46The preparation method of the ZnO photocatalytic composite material is characterized in that the roasting specifically comprises the following steps:
a. raising the temperature in the high-temperature sintering furnace from 20 ℃ to 900 ℃ for 200 min;
b. preserving heat at 900 ℃ for 1500min, cooling along with the furnace, taking out the powder, grinding uniformly to finally obtain pure BiSnSbO6-ZnO photocatalytic composite material.
7. A novel BiSnSbO prepared by the process of claim 46-ZnO photocatalytic composite material, characterized in that said BiSnSbO6the-ZnO photocatalytic composite material has antibacterial performance, and ZnO with small particle size is loaded on BiSnSbO with large particle size6The above.
8. A novel BiSnSbO prepared by the process of claim 46-ZnO photocatalytic composite material or novel BiSnSbO according to claim 76-application of ZnO photocatalytic composite material in living environment.
9. The use of claim 8, further comprising: the novel BiSnSbO6The ZnO photocatalytic composite material has antibacterial application to pathogenic microorganism bacteria and fungi.
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