CN113134370A - Ternary heterojunction photocatalytic antibacterial material and preparation method thereof - Google Patents
Ternary heterojunction photocatalytic antibacterial material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 53
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 51
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
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- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 9
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 9
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 9
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 23
- 239000007864 aqueous solution Substances 0.000 claims description 20
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- 241000191967 Staphylococcus aureus Species 0.000 description 2
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
The invention relates to a ternary heterojunction photocatalytic antibacterial material and a preparation method thereof, wherein the material is a ternary heterojunction photocatalytic antibacterial material based on black phosphorus/polymer carbon quantum dots/molybdenum disulfide, and the preparation method comprises the following steps: dissolving chitosan in deionized water, adding NaOH, performing hydrothermal reaction, and performing centrifugal separation to obtain supernatant which is a chitosan polymer carbon quantum dot solution; respectively adding sodium molybdate and thiourea into deionized water, adding polyvinylpyrrolidone, adding a chitosan polymer carbon quantum dot solution, and carrying out a hydrothermal reaction to obtain carbon quantum dot modified molybdenum disulfide; placing the black phosphorus raw material in absolute ethyl alcohol for ultrasonic dispersion to obtain black phosphorus dispersion liquid; and mixing the carbon quantum dot modified molybdenum disulfide with the black phosphorus dispersion liquid, and calcining to obtain the ternary heterojunction photocatalytic antibacterial material. The material prepared by the invention has the advantages of high utilization rate of visible light, low recombination rate of photo-generated electrons and holes, low cost and excellent photocatalytic antibacterial performance.
Description
Technical Field
The invention relates to the technical field of inorganic material synthesis, in particular to a ternary heterojunction photocatalytic antibacterial material and a preparation method thereof.
Background
The semiconductor photocatalytic material can generate photoproduction electrons and holes (h) under illumination+) In the presence of water and air, superoxide radical (. O) is generated2-) And hydroxyl radical (. OH), etc. Reactive groups h generated in this process+、·O2-And OH and the like can destroy the cell membrane of bacteria through oxidation, thereby causing leakage of the components in the bacteria body and finally inactivation, thereby achieving the aim of antibiosis. However, the traditional photocatalytic material has the defects of low utilization rate of visible light, serious recombination of photo-generated electrons and holes and poor antibacterial effect. For example, conventional TiO2And the ZnO photocatalytic antibacterial material has low utilization rate of visible light, can only utilize a small part of ultraviolet light in sunlight, and has poor antibacterial effect due to serious recombination of photo-generated electron-hole pairs. Two-dimensional materials have a unique layered structure, high carrier mobility and significant in-plane anisotropic electronic properties. Wherein the two-dimensional black phosphorus has adjustable band gap, the band gap can be adjusted from 0.3eV to 2.0eV by changing the layer number, and the two-dimensional black phosphorus can be used with common photocatalyst (such as TiO)2CdS and g-C3N4Etc.) exhibit broader and stronger light absorption capacity in the visible and near infrared regions. Molybdenum disulfide (MoS)2) It is considered to be the best alternative to noble metals because of its low cost and high activity, which is often used as a promoter. More importantly, MoS2With a two-dimensional structure like black phosphorus, the two can combine to form a large contact interface, providing an adequate channel for photo-generated charge transfer. However, due to the high photogeneration of electrons and holes by these two materialsThe recombination rate of the compound seriously influences the photo-generated electrons and holes to play an antibacterial role.
Disclosure of Invention
The invention aims to solve the technical problems and the defects and provides a ternary heterojunction photocatalytic antibacterial material and a preparation method thereof.
In order to solve the technical problems, the invention adopts the technical scheme that: a ternary heterojunction photocatalytic antibacterial material is based on black phosphorus/polymer carbon quantum dots/molybdenum disulfide.
A preparation method of a ternary heterojunction photocatalytic antibacterial material comprises the following steps:
firstly, taking a chitosan raw material, dissolving chitosan in deionized water, adding NaOH to form a chitosan aqueous solution, then adding the chitosan aqueous solution into a hydrothermal reaction kettle for hydrothermal reaction, after the reaction is finished, placing the mixture to room temperature, and performing centrifugal separation to obtain supernatant which is a chitosan polymer carbon quantum dot solution for later use;
step two, respectively adding sodium molybdate and thiourea into deionized water to form an aqueous solution, adding polyvinylpyrrolidone into the aqueous solution, then adding the chitosan polymer carbon quantum dot solution obtained in the step one, carrying out hydrothermal reaction, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation, washing the mixture with deionized water and absolute ethyl alcohol respectively, and drying the mixture to obtain carbon quantum dot modified molybdenum disulfide for later use;
taking the black phosphorus raw material, placing the black phosphorus raw material in absolute ethyl alcohol for ultrasonic dispersion, and adjusting ultrasonic power and time to obtain black phosphorus dispersion liquid with different layers and different band gaps for later use;
and step four, fully mixing the carbon quantum dot modified molybdenum disulfide obtained in the step two with the black phosphorus dispersion liquid obtained in the step three, drying under a vacuum condition, and calcining under an argon protection condition to obtain the black phosphorus/polymer carbon quantum dot/molybdenum disulfide-based ternary heterojunction photocatalytic antibacterial material.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, in the first step, every 2g of chitosan is dissolved in 20-40ml of deionized water, and 0.01-0.1g of NaOH is added for hydrothermal reaction.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, the hydrothermal reaction conditions in the first step are as follows: the reaction temperature is 150 ℃ and 250 ℃, and the reaction time is 20-30 h.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, the centrifugal separation rotating speed in the step one is 6000-10000r/min, and the centrifugal separation time is 8-12 min.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, the weight ratio of the sodium molybdate, the thiourea, the polyvinylpyrrolidone and the chitosan polymer carbon quantum dot solution in the second step is 10:7.5: 1: 10-20.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, the hydrothermal reaction conditions in the step two are as follows: the reaction temperature is 200 ℃ and 260 ℃, and the reaction time is 20-30 h.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, every 1g of black phosphorus raw material is placed in 60-100ml of absolute ethyl alcohol for ultrasonic dispersion in the third step.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, in the fourth step, every 1g of the carbon quantum dot modified molybdenum disulfide obtained in the second step is mixed with 4ml of the black phosphorus dispersion obtained in the third step.
As a further optimization of the preparation method of the ternary heterojunction photocatalytic antibacterial material, the calcination temperature in the step four is 300-400 ℃, and the calcination time is 3-7 h.
The invention has the following beneficial effects:
first, the invention utilizes black phosphorus and MoS2The two-dimensional structure is modified by the chitosan polymer carbon quantum dots, and the combination performance of the chitosan polymer carbon quantum dots and two materials and the function of transmitting photo-generated electrons and holes are utilized to further improve the photo-generated electrons in the materialsAnd the mobility of the hole, so that the recombination of the photo-generated electrons and the hole is inhibited, and the material with high visible light utilization rate, low recombination rate of the photo-generated electrons and the hole, low cost and excellent photocatalytic antibacterial performance is prepared.
The black phosphorus/polymer carbon quantum dot/molybdenum disulfide ternary heterojunction photocatalytic antibacterial material obtained according to the invention is characterized by being capable of fully utilizing sunlight, effectively killing common bacteria under the illumination condition, having wide development prospect in the aspect of antibacterial materials, being capable of modifying the surfaces of medical equipment, antibacterial ceramics and the like, and improving the antibacterial effect under the illumination.
Drawings
FIG. 1 is a block diagram of the preparation process of the photocatalytic antibacterial material according to the present invention;
fig. 2 is a graph showing the antibacterial effect of the photocatalytic antibacterial material of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
A ternary heterojunction photocatalytic antibacterial material is based on black phosphorus/polymer carbon quantum dots/molybdenum disulfide.
Example 1
A preparation method of a ternary heterojunction photocatalytic antibacterial material comprises the following steps:
firstly, taking 2g of chitosan raw material, dissolving chitosan in 30ml of deionized water, adding 0.1g of NaOH, stirring and dissolving to form a chitosan aqueous solution, then adding the chitosan aqueous solution into a 50ml hydrothermal reaction kettle for hydrothermal reaction at the reaction temperature of 180 ℃ for 24h, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation at the centrifugal separation rotating speed of 8000r/min for 10min, and obtaining supernatant which is a chitosan polymer carbon quantum dot solution for later use;
and step two, respectively adding 2g of sodium molybdate and 1.5g of thiourea into 30ml of deionized water to form an aqueous solution, adding 0.2g of polyvinylpyrrolidone into the aqueous solution, then adding 2ml of the chitosan polymer carbon quantum dot solution obtained in the step one, carrying out hydrothermal reaction at 220 ℃ for 24h, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation, respectively washing the mixture with deionized water and absolute ethyl alcohol for three times, and drying to obtain the carbon quantum dot modified molybdenum disulfide for later use.
Example 2
Taking 0.5g of block black phosphorus raw material, placing the block black phosphorus raw material in 40ml of absolute ethyl alcohol, and performing ultrasonic dispersion for 20min under the condition of 300W to obtain black phosphorus dispersion liquid for later use;
and step four, fully mixing 0.5g of carbon quantum dot modified molybdenum disulfide obtained in the step two with 2ml of black phosphorus dispersion liquid obtained in the step three, drying under a vacuum condition, and calcining under an argon protection condition at the calcining temperature of 350 ℃ for 5h to obtain the ternary heterojunction photocatalytic antibacterial material based on the black phosphorus/polymer carbon quantum dots/molybdenum disulfide.
Example 3
2g of sodium molybdate, 0.2g of polyvinylpyrrolidone and 1.5g of thiourea were added to 30mL of deionized water, and dissolved by stirring at room temperature. Transferring the obtained solution into a 50mL hydrothermal reaction kettle, keeping the temperature at 220 ℃ for 24h, placing the solution to room temperature, performing centrifugal separation, washing the solution with deionized water and ethanol for three times respectively, and drying the solution to obtain MoS2And (3) powder.
2mL of the black phosphorus dispersion obtained in example 2 and 0.5g of MoS were taken2And (3) fully mixing and grinding the powder, and calcining for 5 hours at 350 ℃ under the protection of Ar gas to obtain the black phosphorus/molybdenum disulfide binary heterojunction material.
Example 4
Respectively inoculating the bacterial colonies of staphylococcus aureus and escherichia coli into 50mL LB broth liquid culture medium, putting the culture medium into an incubator at 37 ℃ for 12h to obtain original bacterial liquid, and calibrating the concentration of the original bacterial liquid to 105CFU/mL by using sterile water.
0.2g of the samples obtained in examples 1, 2 and 3 (carbon quantum dot-modified molybdenum disulfide, black phosphorus/polymer carbon quantum dot/molybdenum disulfide-based ternary heterojunction photocatalytic antibacterial material and black phosphorus/molybdenum disulfide binary heterojunction material) were dispersed in 10ml of ldmso to prepare solutions to be tested, respectively. And (3) respectively taking 100 mu L of the 2 kinds of original bacterial solutions prepared in the previous step, adding the obtained solution into 10mL of LB culture medium, preparing 6 groups of each bacterial solution of each solution to be detected, wherein each group comprises three groups in parallel, and one group is a blank group. Respectively adding 10 μ L of solution to be tested, culturing at 240rpm and 37 deg.C under illumination, taking out one group at 0h, 2h, 4h, 6h and 8h, detecting light absorption value in ultraviolet spectrophotometer, and obtaining growth curve of Staphylococcus aureus and Escherichia coli according to the absorbance (shown in figure 2).
Example 5
A preparation method of a ternary heterojunction photocatalytic antibacterial material comprises the following steps:
firstly, taking 2g of chitosan raw material, dissolving chitosan in 20ml of deionized water, adding 0.05g of NaOH, stirring and dissolving to form a chitosan aqueous solution, then adding the chitosan aqueous solution into a 50ml hydrothermal reaction kettle for hydrothermal reaction at the reaction temperature of 150 ℃ for 30h, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation at the centrifugal separation rotating speed of 6000r/min for 12min, and obtaining supernatant which is a chitosan polymer carbon quantum dot solution for later use;
and step two, respectively adding 2g of sodium molybdate and 1.5g of thiourea into 30ml of deionized water to form an aqueous solution, adding 0.2g of polyvinylpyrrolidone into the aqueous solution, then adding 2ml of the chitosan polymer carbon quantum dot solution obtained in the step one, carrying out hydrothermal reaction at the reaction temperature of 200 ℃ for 30h, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation, respectively washing the mixture with deionized water and absolute ethyl alcohol for three times, and drying the mixture to obtain the carbon quantum dot modified molybdenum disulfide for later use.
Taking 0.5g of block black phosphorus raw material, placing the block black phosphorus raw material in 40ml of absolute ethyl alcohol, and performing ultrasonic dispersion for 20min under the condition of 300W to obtain black phosphorus dispersion liquid for later use;
and step four, fully mixing 0.5g of carbon quantum dot modified molybdenum disulfide obtained in the step two with 2ml of black phosphorus dispersion liquid obtained in the step three, drying under a vacuum condition, and calcining under an argon protection condition at the calcining temperature of 300 ℃ for 7h to obtain the ternary heterojunction photocatalytic antibacterial material based on the black phosphorus/polymer carbon quantum dots/molybdenum disulfide.
Example 6
A preparation method of a ternary heterojunction photocatalytic antibacterial material comprises the following steps:
firstly, taking 2g of chitosan raw material, dissolving chitosan in 40ml of deionized water, adding 0.08g of NaOH, stirring and dissolving to form a chitosan aqueous solution, then adding the chitosan aqueous solution into a 50ml hydrothermal reaction kettle for hydrothermal reaction at the reaction temperature of 200 ℃ for 20h, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation at the centrifugal separation rotating speed of 10000r/min for 8min, and obtaining supernatant which is a chitosan polymer carbon quantum dot solution for later use;
and step two, respectively adding 2g of sodium molybdate and 1.5g of thiourea into 30ml of deionized water to form an aqueous solution, adding 0.2g of polyvinylpyrrolidone into the aqueous solution, then adding 2ml of the chitosan polymer carbon quantum dot solution obtained in the step one, carrying out hydrothermal reaction at the reaction temperature of 260 ℃ for 20h, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation, respectively washing the mixture with deionized water and absolute ethyl alcohol for three times, and drying the mixture to obtain the carbon quantum dot modified molybdenum disulfide for later use.
Taking 0.5g of block black phosphorus raw material, placing the block black phosphorus raw material in 40ml of absolute ethyl alcohol, and performing ultrasonic dispersion for 20min under the condition of 300W to obtain black phosphorus dispersion liquid for later use;
and step four, fully mixing 0.5g of the carbon quantum dot modified molybdenum disulfide obtained in the step two with 2ml of the black phosphorus dispersion liquid obtained in the step three, drying under a vacuum condition, and calcining under an argon protection condition at the calcining temperature of 400 ℃ for 3h to obtain the ternary heterojunction photocatalytic antibacterial material based on the black phosphorus/polymer carbon quantum dot/molybdenum disulfide.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A ternary heterojunction photocatalysis antibacterial material is characterized in that: the material is a ternary heterojunction photocatalytic antibacterial material based on black phosphorus/polymer carbon quantum dots/molybdenum disulfide.
2. A preparation method of a ternary heterojunction photocatalytic antibacterial material is characterized by comprising the following steps: the method comprises the following steps:
firstly, taking a chitosan raw material, dissolving chitosan in deionized water, adding NaOH to form a chitosan aqueous solution, then adding the chitosan aqueous solution into a hydrothermal reaction kettle for hydrothermal reaction, after the reaction is finished, placing the mixture to room temperature, and performing centrifugal separation to obtain supernatant which is a chitosan polymer carbon quantum dot solution for later use;
step two, respectively adding sodium molybdate and thiourea into deionized water to form an aqueous solution, adding polyvinylpyrrolidone into the aqueous solution, then adding the chitosan polymer carbon quantum dot solution obtained in the step one, carrying out hydrothermal reaction, after the reaction is finished, placing the mixture to room temperature, carrying out centrifugal separation, washing the mixture with deionized water and absolute ethyl alcohol respectively, and drying the mixture to obtain carbon quantum dot modified molybdenum disulfide for later use;
taking the black phosphorus raw material, placing the black phosphorus raw material in absolute ethyl alcohol for ultrasonic dispersion, and adjusting ultrasonic power and time to obtain black phosphorus dispersion liquid with different layers and different band gaps for later use;
and step four, fully mixing the carbon quantum dot modified molybdenum disulfide obtained in the step two with the black phosphorus dispersion liquid obtained in the step three, drying under a vacuum condition, and calcining under an argon protection condition to obtain the black phosphorus/polymer carbon quantum dot/molybdenum disulfide-based ternary heterojunction photocatalytic antibacterial material.
3. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: in the first step, every 2g of chitosan is dissolved in 20-40ml of deionized water, and 0.01-0.1g of NaOH is added for hydrothermal reaction.
4. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: the hydrothermal reaction conditions in the first step are as follows: the reaction temperature is 150 ℃ and 250 ℃, and the reaction time is 20-30 h.
5. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: the centrifugal separation rotating speed in the first step is 6000-10000r/min, and the centrifugal separation time is 8-12 min.
6. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: and step two, the weight ratio of the sodium molybdate, the thiourea, the polyvinylpyrrolidone and the chitosan polymer carbon quantum dot solution is 10:7.5: 1: 10-20.
7. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: the hydrothermal reaction conditions in the step two are as follows: the reaction temperature is 200 ℃ and 260 ℃, and the reaction time is 20-30 h.
8. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: in the third step, every 1g of black phosphorus raw material is placed in 60-100ml of absolute ethyl alcohol for ultrasonic dispersion.
9. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: and in the fourth step, every 1g of the carbon quantum dot modified molybdenum disulfide obtained in the second step is mixed with 4ml of the black phosphorus dispersion liquid obtained in the third step.
10. The method for preparing the ternary heterojunction photocatalytic antibacterial material as claimed in claim 2, wherein the method comprises the following steps: the calcination temperature in the fourth step is 300-400 ℃, and the calcination time is 3-7 h.
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