CN113751027A - Ultrathin MgIn2S4Nano-sheet sterilization photocatalytic material and preparation method thereof - Google Patents
Ultrathin MgIn2S4Nano-sheet sterilization photocatalytic material and preparation method thereof Download PDFInfo
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- CN113751027A CN113751027A CN202111154419.9A CN202111154419A CN113751027A CN 113751027 A CN113751027 A CN 113751027A CN 202111154419 A CN202111154419 A CN 202111154419A CN 113751027 A CN113751027 A CN 113751027A
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- ultrathin
- mgin
- nanosheet material
- nano
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
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Abstract
The invention relates to an ultrathin MgIn2S4A nano-sheet sterilization photocatalytic material and a preparation method thereof. The ultra-thin MgIn2S4The thickness of the nano-sheet material is 4-5nm, the nano-sheet material is a double-layer nano-sheet, the transverse dimension is 0.8-1.2 mu m, and the specific surface area is 40-45m2The photocatalyst is prepared by combining a low-temperature reflux method and an ultrasonic stripping method, the light absorption range can reach 600nm, the particle size is small, the specific surface area is large, the number of active sites of reaction is large, the migration distance of a photon-generated carrier is short, the migration efficiency is high, and the photocatalyst has excellent photocatalytic sterilization performance.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to ultrathin MgIn2S4A nano-sheet sterilization photocatalytic material and a preparation method thereof.
Background
With the rapid development of economy, people pay more and more attention to the environment and self health problems, and under the demand, the development of antibacterial materials is vigorous and hot. The traditional organic antibacterial material has the defects of weak antibacterial property, poor heat resistance and stability, harmful self decomposition products and volatile matters to human bodies, inapplicability to high-temperature processing and the like, limits the application range of the traditional organic antibacterial material, and is gradually replaced by an inorganic antibacterial material. The traditional inorganic antibacterial agent mainly realizes the antibacterial effect by carrying metal ions (such as silver, copper, zinc and the like) on various carriers (such as zeolite, zirconium phosphate, fusible glass, silica gel, activated carbon and the like). In recent years, the novel photocatalytic sterilization material has good chemical stability and lasting effect, overcomes the defects of the Ag-based inorganic antibacterial agent (such as antibacterial performance reduction caused by the denaturation under the conditions of illumination, halogen contact or heating and the like), and enters the visual field of people.
Since the first report of TiO by Matsunaga et al in 19852The photocatalytic sterilization effect and the research on the photocatalytic sterilization performance based on semiconductors are concerned by broad scholars. By means of the electrons, holes and active oxygen species (. O) formed on the surface of the catalyst, which are generated during the photocatalysis2 -OH and1O2etc.) oxidation-reduction of intracellular and extracellular components of bacteria, resulting inThe bacteria are inactivated, thereby achieving the sterilization and disinfection effects. The semiconductor-based photocatalytic sterilization technology has little pollution to the environment, does not generate byproducts harmful to human bodies, and can be used for treating the degradation of organic matters in the environment, so that the semiconductor-based photocatalytic sterilization technology is possible to develop into a safe and feasible sterilization technology.
Most reports are now based on TiO2Photocatalytic sterilization study of (1), however, TiO2It belongs to wide band gap semiconductor, and can be excited only under the condition of UV light, so that its photocatalytic bactericidal activity also is implemented under the condition of UV light, but the UV light is very small in proportion in natural light, only is about 4%, and is limited by TiO, so that it is a wide band gap semiconductor2The main reason for widespread use. Therefore, the search for a photocatalyst that can effectively sterilize bacteria under visible light has become a new and innovative subject of researchers at present.
The valence band of the metal sulfide consists of the 2p orbital of S, has a narrow band gap and good visible light absorption performance, and is an excellent photocatalytic material capable of responding to visible light. For example: gao et al report that pure CdS and a compound of graphene oxide and CdS have a good killing effect on escherichia coli and staphylococcus aureus under visible light, see j.hazard.mater, 2013, page 412-. Sun et al reported Ag2S/Bi2S3The bacteriostasis rate of the compound to escherichia coli in 1 hour under sunlight can reach 100 percent, see environ. Patent document CN107282070A discloses preparation of ZnIn with three-dimensional flower sheet structure on zinc sheet substrate by one-step hydrothermal method2S4The micro-nano wire array film has great application prospect in the fields of photocatalytic sterilization, photocatalytic hydrogen production, photocatalytic degradation of organic pollutants, artificial photosynthesis, solar cells and the like. Patent document CN104525222A discloses a carbon nanotube composite ZnIn2S4The green advanced water treatment agent can remove high-concentration organic pollutants in water, is suitable for advanced treatment of various waste water, is environment-friendly and free of secondary pollution, and has the advantages of being antibacterial, deodorizing, capable of adsorbing other heavy metal ions and the like.
The synthesis method of the metal sulfide nanometer material is various, such as template technology, hydrothermal synthesis method, solvent thermal synthesis method and the like. The template technology is to synthesize a nano material by using a gap in a matrix material with nano holes as a template. But also can be divided into a hard template method, a high molecular polymer method, a micro emulsion method, a monomolecular film method and a biomolecular template method. The hydrothermal synthesis method is a method for preparing a research material by using water as a reaction medium in a high-temperature high-pressure environment of a sealed pressure vessel. The solvothermal synthesis method is a development of hydrothermal reaction, and it is different from hydrothermal reaction in that the solvent used is an organic solvent instead of water. In the solvothermal reaction, one or more precursors are dissolved in a non-aqueous solvent, and under the liquid phase or supercritical condition, reactants are dispersed in the solution and become relatively active, the reaction occurs, and the product is slowly generated. In addition, the synthesis method of the metal sulfide nano material also includes a radiation chemical synthesis method, a sol-gel method, a chemical precipitation method, electrodeposition and the like.
Patent document CN110436509A discloses a method for synthesizing copper sulfide triangular nanosheets, which comprises the following steps: step 1, preparing a polyethyleneimine water solution with the concentration of 0.045g/mL-0.050g/mL, and adding a copper chloride water solution with the concentration of 0.3mmol/mL-0.7mmol/mL while stirring to obtain a solution A; step 2, after the solution A is stirred for 1 to 5 minutes, adding a pH regulator with the pH value of 8 to 10 under stirring to obtain a solution B; step 3, after the solution B is stirred for 1min to 5min, adding a reducing agent under stirring to obtain a solution C; and 4, heating the solution C to 55-65 ℃, adding a sodium sulfide aqueous solution with the concentration of 0.3-0.7 mmol/mL, reacting for 4-8 h, centrifuging, and taking the solid for resuspension to obtain the copper sulfide triangular nanosheet, wherein the volume ratio of the polyethyleneimine aqueous solution to the copper chloride aqueous solution in the step 1 is (200-): 250): 1. Patent document CN108821348B discloses a preparation method of cobalt sulfide nanosheet material, which comprises the following steps: 1) adding cobalt acetate tetrahydrate into a mixed solution of ethylene glycol and isopropanol, and uniformly stirring to obtain a solution A; 2) dropwise adding an ammonia water solution with the concentration of 0.6-0.8mol/L into the aqueous solution of the sodium sulfide until the pH value is 11.2-11.8 to obtain a solution B; 3) adding the solution B into the solution AUniformly dispersing by using ultrasonic waves, then placing the mixture into a homogeneous reactor, reacting at 185-200 ℃ under the condition of uniform-speed rotation, washing after the reaction is finished, and freeze-drying to obtain the cobalt sulfide nanosheet material. Patent document CN110817961A discloses a preparation method of a molybdenum disulfide nanosheet material, which comprises the following steps: (1) uniformly mixing molybdenum disulfide powder with a proper amount of hydrophilic surfactant, and then adding a proper amount of electrolyte solution with the concentration not lower than 0.01mol/L to prepare electrochemical reaction base material slurry; (2) placing the electrochemical reaction mother material slurry in an electrochemical reaction device for electrochemical intercalation reaction; (3) mixing the material in the cathode chamber subjected to electrochemical intercalation reaction with a hydrophilic surfactant, ultrasonically dispersing in deionized water again, and centrifuging to obtain a concentrated solution; (4) and fully drying the concentrated solution to obtain the molybdenum disulfide nanosheet material. Patent document CN113087020A discloses a preparation method of ternary metal sulfide nanosheets, which specifically comprises the following steps: step S1, preparing a manganese salt solution, a cadmium salt solution and a sodium diethyldithiocarbamate solution; step S2 of preparing Mn (DDTC) using a manganese salt solution, a cadmium salt solution, and a sodium diethyldithiocarbamate solution2Precursor and Cd (DDTC)2A precursor; step S3, mixing Mn (DDTC)2Precursor and Cd (DDTC)2Dispersing the precursor in a solvent to obtain a dispersion liquid; step S4, coating the dispersion on a substrate, and heating in inert gas to obtain ternary metal sulfide MnxCd1-xAnd (3) S nanosheet.
And as the photocatalytic material, if the reaction active sites are sufficient and the migration distance of photo-generated electrons and holes is short, the photocatalytic efficiency can be effectively improved and better sterilization performance can be obtained. At present, no ultra-thin MgIn with excellent bactericidal performance is found as in the application2S4Nanoplatelet materials and reports of their preparation and use.
Disclosure of Invention
The invention aims to provide an ultrathin nanosheet material, aiming at the defects in the prior art.
Still another object of the present invention is to provide a method for preparing the ultrathin nanosheet material.
Another object of the present invention is to provide a use of the ultrathin nanosheet material.
In order to achieve the first object, the invention adopts the technical scheme that:
an ultrathin nanosheet material, the ultrathin nanosheet material being ultrathin MgIn2S4The nano sheet has a thickness of 4-5nm and is double-layer MgIn2S4The nano-sheet has a transverse dimension of 0.8-1.2 μm and a specific surface area of 40-45m2/g。
As a preferred embodiment of the present invention, the ultra-thin MgIn2S4The nano sheet is prepared by combining a low-temperature reflux method and ultrasonic stripping, and the preparation method comprises the following steps: dissolving an indium source, a magnesium source and a sulfur source in deionized water, heating and stirring, then carrying out ultrasonic stripping, and centrifuging to obtain a supernatant as a final product.
As a preferable example thereof, the indium source used is indium nitrate or indium acetate, the magnesium source used is magnesium acetate or magnesium nitrate, and the sulfur source used is thioacetamide or cysteine.
As another preferred example, the sulfur source is in excess of at least 1/3 during the preparation process.
As another preferable example thereof, MgIn obtained after the heating reaction2S4Cleaning with deionized water or ethanol for 2-5 times, and ultrasonic stripping.
More preferably, the power of ultrasonic stripping is 200-300W, and the time of ultrasonic stripping is 0.5-5 h.
As another preferable example thereof, the reaction temperature is 80-120 ℃ and the reaction time is 3-8 h.
As another preferred example, the rotating speed of the centrifuge is 3000-.
In order to achieve the second object, the invention adopts the technical scheme that:
the preparation method of the ultrathin nanosheet material comprises the following steps: dissolving an indium source, a magnesium source and a sulfur source in deionized water, heating and stirring, then carrying out ultrasonic stripping, and centrifuging to obtain a supernatant as a final product.
In order to achieve the third object, the invention adopts the technical scheme that:
the ultrathin nanosheet material can be used for photocatalytic sterilization, photocatalytic hydrogen production, photocatalytic degradation of organic pollutants or preparation of solar cells.
The invention has the advantages that:
1. the invention provides an ultrathin MgIn2S4The nano-sheet has larger specific surface area and more active sites, and the shape of the ultrathin nano-sheet is favorable for shortening the migration distance of a photon-generated carrier, promoting the separation of the photon-generated carrier and improving the efficiency of photocatalytic sterilization.
2. The invention provides an ultrathin MgIn2S4The preparation method of the nanosheet does not need special equipment and harsh conditions, has simple process and strong controllability, is easy to realize large-scale production and has practicability.
3. The invention investigates MgIn prepared under different conditions2S4The product performance is found that the method can prepare ultrathin MgIn2S4The nanosheet is thinner, and has more excellent photocatalytic sterilization performance.
Drawings
FIG. 1: XRD patterns of example 1 and comparative examples 1 and 2.
FIG. 2: atomic force microscope photograph of example 1.
FIG. 3: scanning electron microscopy images of example 1.
FIG. 4: scanning electron microscope picture of comparative example 1.
FIG. 5: scanning electron microscope picture of comparative example 2.
FIG. 6: o of example 1 and comparative examples 1 and 22 -Free radical EPR profile.
FIG. 7: the OH radical EPR spectra of example 1 and comparative examples 1 and 2.
FIG. 8: example 1 and comparative examples 1 and 21O2Free radical EPR spectrum of (a).
FIG. 9: the photocatalytic sterilization effect graphs of example 1 and comparative examples 1 and 2.
Detailed Description
The following detailed description of the present invention will be made with reference to the accompanying drawings.
Example 1 ultra-thin MgIn of the invention2S4Preparation of nanosheet (I)
Dissolving 1.5mmol of magnesium acetate and 3mmol of anhydrous indium chloride in 250mL of deionized water, stirring at room temperature for 30min, adding 8mmol of thioacetamide, then placing in an oil bath kettle, heating to 95 ℃, and stirring vigorously for 5 h. Centrifuging the obtained suspension, collecting precipitate, washing with deionized water twice, dispersing again in 200mL deionized water, performing ultrasonic treatment at 40KHz and 250W for 30min, centrifuging at 6000r.p.m. speed for 5min, and collecting supernatant as final product.
Example 2 ultra-thin MgIn of the invention2S4Preparation of nanosheet (II)
Dissolving 1.5mmol of magnesium acetate and 3mmol of anhydrous indium chloride in 250mL of deionized water, stirring at room temperature for 30min, adding 10mmol of thioacetamide, then placing in an oil bath kettle, heating to 95 ℃, and stirring vigorously for 5 h. Centrifuging the obtained suspension, collecting precipitate, washing with deionized water twice, dispersing again in 200mL deionized water, performing ultrasonic treatment at 40KHz and 250W for 30min, centrifuging at 6000r.p.m. speed for 5min, and collecting supernatant as final product.
Example 3 ultra-thin MgIn of the invention2S4Preparation of nanosheet (III)
Dissolving 1.5mmol of magnesium acetate and 3mmol of anhydrous indium chloride in 250mL of deionized water, stirring at room temperature for 30min, adding 8mmol of thioacetamide, then placing in an oil bath kettle, heating to 95 ℃, and stirring vigorously for 5 h. Centrifuging the obtained suspension, collecting precipitate, washing with deionized water twice, dispersing again in 200mL deionized water, performing ultrasonic treatment at 40KHz and 300W for 30min, centrifuging at 6000r.p.m. speed for 5min, and collecting supernatant as final product.
Example 4 ultra-thin MgIn of the invention2S4Preparation of nanosheet (IV)
Dissolving 1.5mmol of magnesium acetate and 3mmol of anhydrous indium chloride in 250mL of deionized water, stirring at room temperature for 30min, adding 8mmol of thioacetamide, then placing in an oil bath kettle, heating to 80 ℃, and stirring vigorously for 8 h. Centrifuging the obtained suspension, collecting precipitate, washing with deionized water five times, dispersing into 200mL deionized water again, performing ultrasonic treatment at 40KHz and 250W for 5h, centrifuging at 8000r.p.m. speed for 10min, and collecting supernatant as final product.
Example 5 ultra-thin MgIn of the invention2S4Preparation of nanosheet (V)
Dissolving 1.5mmol of magnesium acetate and 3mmol of anhydrous indium chloride in 250mL of deionized water, stirring at room temperature for 30min, adding 8mmol of thioacetamide, then placing in an oil bath kettle, heating to 120 ℃, and stirring vigorously for 3 h. Centrifuging the obtained suspension, collecting precipitate, washing with deionized water for three times, dispersing into 200mL deionized water again, performing ultrasonic treatment at 40KHz and 250W for 2h, centrifuging at 3000r.p.m. speed for 30min, and collecting supernatant as final product.
Comparative example 1
In order to highlight the excellent performance of the ultrathin nanosheet sterilizing photocatalyst material provided by the invention, a granular MgIn is synthesized2S4For comparison.
Ultrasonically dissolving 1.5mmol of magnesium acetate, 3mmol of anhydrous indium chloride and 8mmol of thioacetamide in 250mL of deionized water, placing the deionized water in an oven, heating the deionized water at 80 ℃ for 2h, centrifuging, collecting precipitate, and drying the precipitate for later use.
Comparative example 2
The reaction steps are the same as those in the embodiment 1, and the raw material proportion in the reaction process is regulated to be that the molar ratio of the magnesium source to the indium source to the sulfur source is 1: 2: 4, i.e. 1.5mmol of magnesium acetate, 3mmol of anhydrous indium chloride and 6mmol of thioacetamide, to prepare the product MgIn2S4And (3) nano materials.
Comparative example 3
The reaction steps are the same as those in the example 1, the ultrasonic power is controlled to be 150W in the reaction process, and the product MgIn is prepared2S4And (3) nano materials.
Comparative example 4
The reaction procedure was the same as in example 1, and the ultrasonic work in the reaction process was controlledThe rate is 350W, and the product MgIn is prepared2S4And (3) nano materials.
Example 6 topography Observation
The morphology of the product was observed using a Hitachi S4800 scanning electron microscope. The SEM of example 1 is shown in FIG. 3, and the SEM of the products of examples 2-5 is similar to that of example 1, indicating that MgIn is prepared2S4Nanosheets, evaluated, MgIn of example 12S4The thickness of the nano-sheet is 4-5nm, and the nano-sheet is double-layer MgIn2S4Nanosheets having a transverse dimension of 1 μm and a specific surface area of 42.1m2Mg of MgIn of examples 2-52S4The thickness of the nano-sheet is 4-5nm, and the nano-sheet is double-layer MgIn2S4The nano sheet has transverse size of 0.8-1.2 μm and specific surface area of 40-45m2The range of/g.
FIG. 4 is a scanning electron microscope picture of comparative example 1, showing that bulk MgIn is obtained by the preparation2S4A material.
FIG. 5 is a scanning microscope photograph of the product prepared in comparative example 2, and it can be seen that the sample is difficult to peel off and ultra-thin MgIn cannot be obtained when the amount of the sulfur source added is small2S4Nanosheets.
The product of comparative example 3 was also similar to comparative example 2, and the samples were found to be difficult to peel.
The scanning observation of the product of comparative example 4 by an electron microscope shows that MgIn is obtained2S4Nanosheets, but with greater thickness, more like granules.
Example 7 characterization of free radical production
The free radicals generated by the samples were characterized using a Bruker ESR5000 electron paramagnetic resonance spectrometer. Referring to fig. 6, 7, and 8, the ultra-thin nano-sized flaky MgIn prepared when an excessive sulfur source is added2S4The generated signals of the superoxide radical, hydroxyl radical and singlet oxygen are obviously stronger than those of the granular MgIn2S4And samples with less sulfur source added.
Example 8 photocatalytic bactericidal Property test
For the MgIn obtained above2S4Subjecting the nanosheet to lightAnd (3) testing catalytic sterilization performance: mixing and stirring 23.3mL of sample with the concentration of 1mg/mL and 1.7mL of suspension bacteria liquid with the concentration of 0.5 McLeeb unit of escherichia coli uniformly, stirring for 30min under a dark condition, then turning on a 300W xenon lamp with a 400nm filter for illumination, extracting 0min and 30min under the dark condition and 100 mu L of solution for diluting 1000 times after turning on the lamp for 5min, 10min, 20min, 30min, 60min, 90min and 120min, then uniformly mixing 100 mu L of diluted mixed solution and 300 mu L of physiological saline, and then coating the mixed solution on a sheep blood agar plate. After being cultured in an incubator overnight, the culture medium is taken out and observed for counting.
For the MgIn obtained above2S4And (3) carrying out a performance test of killing staphylococcus aureus by photocatalysis on the nanosheets, wherein the steps are the same as the steps for testing escherichia coli except that the escherichia coli in the bacterial liquid is replaced by the staphylococcus aureus.
For the MgIn obtained above2S4And (3) carrying out a performance test of killing the drug-resistant staphylococcus aureus by the nanosheets through photocatalysis, wherein the steps are the same as the steps for testing escherichia coli except that escherichia coli in the bacterial liquid is replaced by the drug-resistant staphylococcus aureus.
As can be seen from FIG. 9, the ultra-thin MgIn prepared in example 12S4The killing effect of the nanosheet on three bacteria is remarkably stronger than that of the granular MgIn of comparative example 12S4And the sample of comparative example 2. The results of the photocatalytic sterilization performance test of the other examples and comparative examples are shown in table 1. The result of the photocatalytic sterilization performance test shows that the ultrathin MgIn prepared by the method of the invention2S4The nano-sheet has excellent bactericidal performance and is obviously stronger than products prepared under other conditions.
TABLE 1 percentage of viable bacteria (%) -at 30min time point for the products of examples 2-5 and comparative examples 3-4
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and additions can be made without departing from the method of the present invention, and these modifications and additions should also be regarded as the protection scope of the present invention.
Claims (10)
1. The ultrathin nanosheet material is characterized in that the ultrathin nanosheet material is ultrathin MgIn2S4The nano sheet has a thickness of 4-5nm and is double-layer MgIn2S4The nano-sheet has a transverse dimension of 0.8-1.2 μm and a specific surface area of 40-45m2/g。
2. The ultrathin nanosheet material of claim 1, wherein the ultrathin MgIn is2S4The nano sheet is prepared by combining a low-temperature reflux method and ultrasonic stripping, and the preparation method comprises the following steps: dissolving an indium source, a magnesium source and a sulfur source in deionized water, heating and stirring, then carrying out ultrasonic stripping, and centrifuging to obtain a supernatant as a final product.
3. An ultrathin nanosheet material as recited in claim 2, wherein the indium source used is indium nitrate or indium acetate, the magnesium source used is magnesium acetate or magnesium nitrate, and the sulfur source used is thioacetamide or cysteine.
4. The ultrathin nanosheet material of claim 2, wherein the sulfur source is present in an excess of at least 1/3 during the preparation.
5. The ultrathin nanosheet material of claim 2, wherein the MgIn obtained after the heating reaction2S4Cleaning with deionized water or ethanol for 2-5 times, and ultrasonic stripping.
6. The ultrathin nanosheet material of claim 5, wherein the power of ultrasonic stripping is 200-300W and the time of ultrasonic stripping is 0.5-5 h.
7. The ultrathin nanosheet material of claim 2, wherein the reaction temperature is from 80 to 120 ℃ and the reaction time is from 3 to 8 hours.
8. The ultrathin nanosheet material as recited in claim 2, wherein the centrifuge rotation speed is 3000-8000r.p.m. and the centrifugation time is 5-30 min.
9. The method of preparing an ultrathin nanosheet material of any one of claims 1 to 8, wherein the method of preparing comprises: dissolving an indium source, a magnesium source and a sulfur source in deionized water, heating and stirring, then carrying out ultrasonic stripping, and centrifuging to obtain a supernatant as a final product.
10. Use of an ultra thin nanoplatelet according to any of claims 1-8 for photocatalytic sterilization, photocatalytic hydrogen production, photocatalytic degradation of organic contaminants or for the preparation of solar cells.
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Application publication date: 20211207 |