CN111418608A - Ag-MoS2@TiO2Nano photocatalytic bactericidal material and preparation method thereof - Google Patents
Ag-MoS2@TiO2Nano photocatalytic bactericidal material and preparation method thereof Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 46
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 33
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 31
- 239000000463 material Substances 0.000 title claims abstract description 29
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- 238000002360 preparation method Methods 0.000 title claims description 15
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Images
Classifications
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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
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B01J35/23—
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses Ag-MoS2@TiO2The nano photocatalytic bactericidal material is prepared by applying chitosan to the reaction of nano titanium dioxide, molybdenum disulfide and silver ions to prepare Ag-MoS2@TiO2The nano material keeps good in-situ dispersion characteristics, improves the catalytic efficiency of titanium dioxide in natural light, and has excellent sterilization effect. The invention uses high-frequency high-energy ultrasonic wavesHandling opening of MoS2Lamellar layer, and MoS can be simultaneously enabled at 110-140 DEG C2Breaking, in this way breaking up the fault of the MoS2The small molecules are doped into the nano titanium dioxide crystal. The Ag-MoS prepared by the method of the invention2@TiO2The nano material has uniform size, good dispersibility, good photocatalysis effect and good sterilization effect.
Description
Technical Field
The invention relates to the technical field of photocatalytic sterilization materials, in particular to a preparation method of an Ag ion-loaded MoS2 quantum dot composite TiO2 nano photocatalytic sterilization material.
Background
The photocatalysis technology is a very effective technology for solving the environmental pollution and the energy crisis. Titanium dioxide (TiO)2) Is an important inorganic photocatalytic material, the titanium dioxide has the advantages of high photocatalysis, high stability, low toxicity and the like, and the TiO2Can perform a photocatalytic reaction under the irradiation of ultraviolet rays to decompose organic matters into carbon dioxide and water, and can be used for removing the organic matters, sterilizing, disinfecting, treating sewage and the like. At the same time, from TiO2The formed film has the characteristics of photocatalysis and super-hydrophilicity, so that the film has the functions of self-cleaning, decontamination, easy cleaning, water mist prevention and the like, and has attracted wide attention. However, since the ultraviolet energy in sunlight accounts for no more than 5%, and ordinary titanium dioxide requires relatively high-intensity ultraviolet light to exert excellent catalytic action, the catalytic rate of ordinary titanium dioxide using natural light is not high, and ideal effects of disinfection, sterilization, self-cleaning and the like cannot be achieved. Theoretically, by the reaction of TiO2The modification means such as metal/nonmetal ion doping, noble metal loading, heterojunction structure and the like can be carried out to make the titanium dioxide better utilize sunlight, improve the catalytic efficiency of the titanium dioxide under natural light, and obtain molybdenum disulfide (MoS)2) Is a graphene-like two-dimensional semiconductor nano material, the combination of molybdenum disulfide and titanium dioxide is one of the key points of research in the field, however, no heterostructure which is simple to operate, suitable for large-scale production and capable of simultaneously obtaining titanium dioxide and molybdenum dioxide and has excellent catalytic effect performance under natural light exists in the prior artA method.
Silver is an ancient germicide. Compared with the conventional disinfectant, the silver ion disinfectant has higher safety and better killing effect; compared with antibiotic disinfectants, silver has spectral disinfection and drug resistance, and has unique advantages and great potential for resisting superbacteria and the like. However, the currently commonly used silver ion-containing disinfectant has some inherent defects, for example, silver ions are easily consumed by chloride ions and the like, and are easily decomposed by visible light and are not easily absorbed by cells, which greatly limits the killing effect of silver ions; if the killing effect is achieved simply by increasing the dosage, immeasurable damage can be caused to the human body and the environment. Silver ions are used as a dissolving-out type disinfectant, and are easy to damage skin along with water flow when in use and run off to water to cause environmental pollution. The silver-containing bactericidal disinfectant with high efficiency and stability is always the focus of research.
Therefore, in order to solve the problems in the prior art, it is important to provide a technique that is simple in operation, low in consumption, high in yield, suitable for large-scale production, free from secondary pollution to the environment, and capable of preparing a nano photocatalytic sterilization material with high photoresponse efficiency and good sterilization effect.
Disclosure of Invention
The invention aims to avoid the defects in the prior art and provide the preparation method of the efficient Ag-loaded MoS2 quantum dot composite TiO2 nano photocatalytic sterilization material (the nano photocatalytic sterilization material is recorded as 'Ag-MoS') which is simple and convenient to operate, easy to realize, low in consumption, high in yield, good in repeatability, suitable for large-scale production or free of secondary pollution to the environment2@TiO2") of the same method.
The purpose of the invention is realized by the following technical scheme:
provides an Ag-MoS2@TiO2The preparation method of the nano photocatalytic sterilization material comprises the following steps:
(1) mixing nano titanium dioxide, molybdenum disulfide and chitosan according to the weight ratio of 75: 1: 2, mixing and grinding for 10-30 min to obtain mixed powder;
(2) adding N-methyl pyrrolidone into the mixed powder, stirring and mixing to obtain a mixed solution, wherein the mass ratio of the nano titanium dioxide to the N-methyl pyrrolidone is 1: 10-1: 1000, parts by weight;
(3) putting the mixed solution into an ultrasonic cleaning machine for treatment for 0.5-2 hours;
(4) heating the mixed solution after ultrasonic treatment to 110-140 ℃, and reacting for 1-2 hours;
(5) adding AgNO3 solution into the reaction solution obtained in the step (4), and stirring for 50-70 minutes at normal temperature, wherein the concentration of Ag + in the AgNO3 solution is 1000 ppm;
(6) and controlling the temperature of the mixed solution after the heat treatment to be 80-100 ℃ and evaporating to dryness until the mixed solution becomes powder.
Preferably, step (3) and step (4) are operated repeatedly.
Preferably, the power of the ultrasonic treatment is 200-300W.
Preferably, the nano titanium dioxide is titanium dioxide of a commercial P25 type, and the grain size is 20 nm; the particle size of the molybdenum disulfide is 2-10 μm.
Preferably, the mass ratio of the nano titanium dioxide to the N-methyl pyrrolidone is 1: 100.
preferably, in step (5), the stirring speed is 500 rpm.
The other purpose of the invention is realized by the following technical scheme:
Ag-MoS2@TiO2Nano photocatalytic bactericidal material, said Ag-MoS2@TiO2The nano photocatalytic sterilization material is prepared by the method.
The invention has the beneficial effects that:
the invention creatively applies the chitosan to the reaction of the nano titanium dioxide and the molybdenum disulfide, and aims to prepare the nano titanium dioxide and molybdenum disulfide heterostructure for solving the technical problem. Chitosan inhibits MoS by utilizing strong electropositivity and steric hindrance of chitosan2Agglomeration of quantum dots and greatly improved TiO2Dispersibility, so that MoS is produced2@TiO2The nano material keeps good in-situ dispersion characteristic and has extremely large specific surface area, thereby greatly improving the catalytic efficiency. MoS2The nano material is an excellent silver ion carrier. MoS2The quantum dots have extremely large specific surface area and can provide a large number of adsorption sites for silver ions; the Ag-S bond enables silver ions to be firmly adsorbed on the surface of MoS 2. Therefore, the MoS2 quantum dot composite nano TiO2 is an excellent silver ion carrier.
Meanwhile, Ag ions can be adsorbed on MoS2Formation of Ag-MoS on quantum dots2@TiO2The nano photocatalytic sterilization material and the chitosan can increase the adsorption capacity of Ag ions on the nano titanium dioxide and improve the concentration of the silver ions in unit volume, and the nano titanium dioxide can be used as a carrier of the silver ions, so that the stability and sterilization efficiency of the silver ions are enhanced; meanwhile, the addition of the silver ions also enables the nano titanium dioxide to obtain a sterilization effect under the condition of no light, and the silver ion loaded nano titanium dioxide has a more excellent sterilization effect than the silver ions and the nano titanium dioxide.
In addition, the amino groups in the chitosan can effectively capture free silver ions, prevent the loss of the silver ions, further promote the slow release effect of the silver ions and enhance the long-term antibacterial effect of the composite material. On the other hand, the rich amino and hydroxyl in the chitosan are beneficial to improving TiO2The visible light activity of the titanium dioxide composite material can inhibit the agglomeration of MoS2 quantum dots, and the non-metal element doping is formed, so that the absorption spectrum of the titanium dioxide is red-shifted to a visible light region, and the catalytic efficiency of the titanium dioxide in natural light is improved. In addition, chitosan also improves TiO2In favour of TiO2And MoS2And (4) doping and combining.
Further, due to the presence of chitosan, the MoS obtained can be obtained2@TiO2Can be directly dried to prepare powder material, the particle size of the powder material is not increased after the powder material is redispersed, and the redispersed MoS2@TiO2Directly or by adding other adjuvants. MoS prepared by the invention2@TiO2Can be stored at room temperature for more than 1 year without precipitation after redispersion.
Operationally, the present invention opens the MoS using high frequency, high energy ultrasonic treatment2Sheet layer at the same timeMoS is carried out at 110-140 DEG C2MoS fragmentation to facilitate fracture2The small molecules are doped into the nano titanium dioxide crystal. MoS prepared by the invention2@TiO2Molybdenum disulfide (MoS) in (1)2) Has unique band gap structure, strong absorption to visible light, MoS due to its strong quantum confinement effect2The quantum dots can efficiently transfer electrons to TiO2So that the MoS of the whole body2@TiO2Has excellent photocatalytic effect. Photo-generated electrons from MoS under sunlight irradiation2Up to TiO2The photocatalysis of visible light response is realized; at the same time, MoS2The load of the quantum dots is beneficial to the separation of electron holes, and the quantum yield of photocatalysis is improved. The heat treatment can allow MoS2And TiO2Complete reaction and compounding, adding silver nitrate, evaporating to dryness at low temperature to ensure that Ag ions are firmly loaded on MoS2@TiO2Form stable Ag-MoS2@TiO2A nano photocatalytic sterilizing material.
Compared with the prior art, the Ag-MoS of the invention2@TiO2The preparation method of the nano photocatalytic sterilization material is simple and convenient to operate, easy to implement, short in time consumption, low in cost, high in yield, good in repeatability and suitable for large-scale production or has no secondary pollution to the environment. Ag-MoS prepared by the preparation method2@TiO2The nano material has uniform size, good dispersibility, good photocatalysis effect and good sterilization effect.
Drawings
The invention is further illustrated by means of the attached drawings, the content of which is not in any way limitative of the invention.
FIG. 1 shows Ag-MoS obtained in example 1 of the present invention2@TiO2Transmission electron microscopy imaging of the nanomaterial.
FIG. 2 shows Ag-MoS obtained in example 1 of the present invention2@TiO2Elemental profile of the nanomaterial.
FIG. 3 shows Ag-MoS obtained in example 1 of the present invention2@TiO2Characterization of the killing effect on Escherichia coli.
Detailed Description
While the following is a preferred embodiment of the present invention, it should be noted that those skilled in the art can make various modifications and improvements without departing from the principle of the present invention, and such modifications and improvements are considered to be within the scope of the present invention. The embodiments of the present invention are not limited to the following specific examples. Changes may be made as appropriate without departing from the scope of the main right.
In the embodiment of the invention, the silver nitrate, the molybdenum disulfide and the chitosan powder are purchased from an Aladdin reagent, and the P25 type nano titanium dioxide is purchased from a winning industrial group.
Example 1
Ag-MoS of the present example2@TiO2The preparation method of the nano photocatalytic sterilization material comprises the following steps:
(1) mixing nano titanium dioxide, molybdenum disulfide and chitosan according to the weight ratio of 75: 1: 2 mixing and grinding for 20min to obtain mixed powder;
(2) adding N-methyl pyrrolidone into the mixed powder, stirring and mixing to obtain a mixed solution, wherein the mass ratio of the nano titanium dioxide to the N-methyl pyrrolidone is 1: 100, respectively;
(3) putting the mixed solution into an ultrasonic cleaning machine for 1 hour, wherein the power of ultrasonic treatment is 250W;
(4) heating the mixed solution after ultrasonic treatment to 120 ℃, and reacting for 2.5 hours;
(5) adding AgNO into the reaction liquid in the step (4)3Stirring the solution for 1 hour at normal temperature at the stirring speed of 500rpm, wherein the AgNO3Ag in solution+The concentration of (A) is 1000 ppm;
(6) the mixture after heat treatment is controlled at 100 ℃ and evaporated to dryness to become powder.
Ag-MoS prepared by the method of this example2@TiO2The results of the tests of the nano photocatalytic sterilization material are shown in figures 1-4, wherein figure 1 shows Ag-MoS2@TiO2Imaging picture of low power transmission electron microscope of nano material(TEM); FIG. 2 is Ag-MoS2@TiO2X-ray diffraction spectroscopy (XRD) of the nanomaterial; FIG. 3 shows pure nano-titanium dioxide, MoS2@TiO2And Ag-MoS2@TiO2The comparative graph of the photocatalytic degradation dye curves of the three substances.
FIG. 1 shows Ag-MoS2@TiO2The nano material has good in-situ dispersion characteristic.
In fig. 2, it can be seen that Ag, Mo, Ti and O elements are simultaneously present in the prepared nano material powder, that is, the silver ion-loaded molybdenum disulfide composite titanium dioxide nano material is successfully prepared.
FIG. 3 compares TiO2(P25)、MoS2@TiO2And Ag-MoS2@TiO2The killing effect on escherichia coli. The OPNG is used as an indicator of the cell wall damage of the escherichia coli, and the stronger the characteristic absorption peak at 420nm, the better the killing effect on the escherichia coli is shown; the Ag-MoS2@ TiO2 has the strongest bactericidal effect due to the synergistic effect of the three materials.
Example 2
The main technical solution of this embodiment is substantially the same as that of embodiment 1, and the features that are not explained in this embodiment adopt the explanations in embodiment 1, and are not described herein again. The present embodiment is different from embodiment 1 in that:
(1) grinding the nano titanium dioxide, the molybdenum disulfide and the chitosan for 30min to obtain mixed powder;
(2) the mass ratio of the nano titanium dioxide to the N-methyl pyrrolidone is 1: 1000, parts by weight;
(3) carrying out ultrasonic treatment for 0.5 hour, wherein the power of the ultrasonic treatment is 200W;
(4) heat treatment is carried out to 110 ℃, and reaction is carried out for 2 hours;
(5) adding AgNO3The solution is stirred for 50 minutes at normal temperature
(6) Evaporated to dryness at 80 ℃ to a powder.
Example 3
The main technical solution of this embodiment is substantially the same as that of embodiment 1 or embodiment 2, and the features that are not explained in this embodiment adopt the explanations in embodiment 1 or embodiment 2, which are not described herein again. The present embodiment is different from embodiment 1 in that:
(1) grinding the nano titanium dioxide, the molybdenum disulfide and the chitosan for 10min to obtain mixed powder;
(2) the mass ratio of the nano titanium dioxide to the N-methyl pyrrolidone is 1: 10;
(3) carrying out ultrasonic treatment for 2 hours, wherein the power of the ultrasonic treatment is 300W;
(4) heat treatment is carried out to 140 ℃, and reaction is carried out for 4 hours;
(5) adding AgNO3The solution was stirred at room temperature for 70 minutes
(6) Evaporated to dryness at 90 ℃ to a powder.
Example 4
The main technical solution of this embodiment is substantially the same as that of embodiment 1, and the features that are not explained in this embodiment adopt the explanations in embodiment 1, and are not described herein again. The present embodiment is different from embodiment 1 in that: repeating the steps (3) and (4) for 2 times.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and do not limit the protection scope of the claims. It will be understood by those skilled in the art that various modifications and equivalents may be made to the embodiments of the present invention without departing from the spirit and scope of the invention.
Claims (7)
1.Ag-MoS2@TiO2The preparation method of the nano photocatalytic sterilization material is characterized by comprising the following steps:
(1) mixing nano titanium dioxide, molybdenum disulfide and chitosan according to the weight ratio of 75: 1: 2, mixing and grinding for 10-30 min to obtain mixed powder;
(2) adding N-methyl pyrrolidone into the mixed powder, stirring and mixing to obtain a mixed solution, wherein the mass ratio of the nano titanium dioxide to the N-methyl pyrrolidone is 1: 10-1: 1000, parts by weight;
(3) putting the mixed solution into an ultrasonic cleaning machine for treatment for 0.5-2 hours;
(4) heating the mixed solution after ultrasonic treatment to 110-140 ℃, and reacting for 1-2 hours;
(5) adding AgNO into the reaction liquid in the step (4)3Stirring the solution for 50-70 minutes at normal temperature, wherein the AgNO is3Ag in solution+The concentration of (A) is 1000 ppm;
(6) and controlling the temperature of the mixed solution after the heat treatment to be 80-100 ℃ and evaporating to dryness until the mixed solution becomes powder.
2. Ag-MoS according to claim 12@TiO2The preparation method of the nano photocatalytic sterilization material is characterized in that the steps (3) and (4) can be repeatedly operated.
3. Ag-MoS according to claim 12@TiO2The preparation method of the nano photocatalytic sterilization material is characterized in that the power of ultrasonic treatment is 200-300W.
4. Ag-MoS according to claim 12@TiO2The preparation method of the nano photocatalytic sterilization material is characterized in that the nano titanium dioxide is commercial P25 type titanium dioxide, and the grain size is 20 nm; the particle size of the molybdenum disulfide is 2-10 μm.
5. Ag-MoS according to claim 12@TiO2The preparation method of the nano photocatalytic sterilization material is characterized in that the mass ratio of the nano titanium dioxide to the N-methyl pyrrolidone is 1: 100.
6. Ag-MoS according to claim 12@TiO2The preparation method of the nano photocatalytic sterilization material is characterized in that in the step (5), the stirring speed is 500 rpm.
7. Root Ag-MoS2@TiO2A nano photocatalytic bactericidal material comprising the Ag-MoS according to any one of claims 1 to 62@TiO2Nano photocatalytic sterilizationThe preparation method of the material.
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