CN114105200B - Preparation method and application of environment-friendly molybdenum disulfide/ferric oxide nanocomposite - Google Patents
Preparation method and application of environment-friendly molybdenum disulfide/ferric oxide nanocomposite Download PDFInfo
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- 239000002114 nanocomposite Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 19
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 13
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 64
- 239000000243 solution Substances 0.000 claims description 28
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- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 238000005859 coupling reaction Methods 0.000 claims description 6
- 229910052961 molybdenite Inorganic materials 0.000 claims description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 6
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- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
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- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Catalysts (AREA)
- Compounds Of Iron (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a preparation method and application of an environment-friendly molybdenum disulfide/ferric oxide nanocomposite, comprising the following steps: (1) Constructing a precursor solution containing Mo 4+ and S 2‑ into MoS 2 nanometer flower-shaped particles by a hydrothermal method; (2) And constructing Fe 2O3 on the MoS 2 by a water bath method to obtain the MoS 2/Fe2O3 nano composite structure. The method combining the hydrothermal method and the water bath method has the advantages of uniform reaction, good control of the ideal ratio and the structural morphology of the product, and the like. The larger specific surface area of the sample of the present invention results in more active sites. The carrier separation efficiency of the sample is higher based on the special energy band structures of MoS 2 and Fe 2O3, and the sample has higher SERS activity and photocatalytic activity.
Description
Technical Field
The invention belongs to the field of environment-friendly material preparation, and particularly relates to a preparation method and application of a renewable flower-shaped molybdenum disulfide/ferric oxide (MoS 2/Fe2O3) nanocomposite capable of detecting and degrading endocrine disruptors.
Background
The growing population and rapid economic development have led to rapid consumption of fossil fuels, severe environmental pollution and global warming. Therefore, the development of new environmental remediation materials that are renewable is more important than ever before. Bisphenol a (BPA) is a toxic endocrine disrupting chemical. Meanwhile, the compound is also an industrial compound widely used, is mainly used for producing plastic products such as food packages, milk bottles and the like, and is a substance which is visible everywhere in life of people. Studies have shown that even trace amounts of BPA entering the human body are associated with diseases such as heart disease, diabetes, bronchitis, significant protein denaturation of the liver and kidneys, and the like. Therefore, there is an urgent need to explore a simple, inexpensive, rapid, ultrasensitive method for detecting BPA.
Various analysis methods for detecting trace BPA are greatly developed at present, including high performance liquid chromatography, gas chromatography-mass spectrometry, enzyme-linked immunosorbent assay, molecular imprinting technology, electrochemical sensors and the like. These techniques make micro and trace analysis of BPA more rapid and sensitive. In addition, functional sensors have attracted increasing attention from researchers due to their reduced sample preparation time, simplified testing procedures.
Surface Enhanced Raman Scattering (SERS) is a highly sensitive and non-destructive analytical technique that can detect and identify compounds with single molecule sensitivity. The method has wide application prospect in the fields of medical diagnosis, biological imaging, chemical analysis, environmental monitoring and the like. The existence of trace BPA is always a problem of common concern of people, and SERS has the advantages of high detection precision, small environmental pollution, high detection speed and the like, so that the SERS is quite promising in the aspect of detecting trace BPA. However, the substrate material is essential in SERS measurement because it can achieve a large enhancement effect by both widely accepted mechanisms of electromagnetic enhancement and chemical enhancement. Ren et al prepared a SERS substrate consisting of silver core and molecularly imprinted polymer shell (Ag@MIP) that could sensitively detect BPA at concentrations as low as 1.0X10 -9 mol/L. Xue et al provides an effective method for specific detection of BPA molecules in practical application by adopting a SERS combined surface imprinting gold nanoparticle method. Although noble metals can lead to ultra-high raman intensities as SERS substrate materials, they are expensive, have poor stability and poor biocompatibility, and greatly limit their practical development. Therefore, the search for new semiconductor materials capable of compensating for the defects of noble metals is becoming a research hotspot of SERS substrates.
In addition to trace detection of BPA, one thing we have to consider is the problem of BPA removal. Because BPA is widely used in the production of polycarbonate plastics and epoxy resins, it is inevitably released from many plastic packages (such as baby bottles and plastic beverage bottles), ultimately resulting in food and environmental pollution and harm to human health. Therefore, in practical applications, it is not sufficient that the material has only excellent detection ability, and more importantly, can remove harmful substances such as BPA. In addition, new materials developed in view of cost effectiveness should also possess recyclable properties.
The flower-shaped MoS 2/Fe2O3 heterostructure is formed by combining MoS 2 nano flowers with Fe 2O3 nano particles. The minimum detection limit of the structure as a SERS substrate for detecting BPA can reach 10 -9 M. In addition, the structure also has rapid and efficient photocatalytic activity, and the degradation rate of BPA reaches 91% within 50min under ultraviolet irradiation. Based on the magnetic properties of Fe 2O3, the uniformly dispersed MoS 2/Fe2O3 can be rapidly separated from the solution by an external magnet, and an aggregate can be formed within 22 s. Proved by verification, the recovered MoS 2/Fe2O3 still has higher activity and can be recycled for at least 5 times. In a word, the invention has the advantages of high sensitivity, high degradation efficiency, reusability, low cost, environmental friendliness and the like, and the environment-friendly material which has the advantages of detection and degradation and can be recycled is expected to be widely applied to the fields of environmental detection, food safety and the like.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provide a preparation method of an environment-friendly MoS 2/Fe2O3 nanocomposite, which has the advantages of detecting and degrading BPA and being capable of being recycled. The invention has the main advantages of high detection sensitivity, high degradation efficiency, repeated utilization, low cost, environmental friendliness and the like, can skillfully avoid the problem of single use of the traditional SERS substrate, hardly generates any harm to the environment, and has important research value and good application prospect in the field of preparing environment-friendly materials.
In order to solve the technical problems, the invention is realized in such a way that the environment-friendly MoS 2/Fe2O3 nano composite material is prepared from the following raw materials in parts by weight:
the preparation method comprises the following specific steps:
①、MoS2 Preparation of nanoflower: firstly, mixing 0.5g H 4MoNa2O6 and 0.7g CH 4N2 S in 70mL of ultrapure water, magnetically stirring for 20min to obtain a uniform solution, then adding 0.5g C 6H8O7·H2 O into the solution, stirring to be completely dissolved, transferring the obtained mixed solution into an 80mL Teflon-lined autoclave, placing the autoclave into a drying box, preserving the autoclave at 220-240 ℃ for 22-24h, repeatedly centrifuging and cleaning a reaction product by using deionized water and ethanol after the reaction is cooled to room temperature, and finally drying at 70 ℃ for 6h to obtain MoS 2 powder;
②、MoS2/Fe2O3 Preparation of nanocomposite: firstly, weighing 0.2g of MoS 2 powder prepared in the step ①, 0.5g H 18FeN3O18 and 0.7g H 2NCONH2, mixing and dissolving in 70mL of ultrapure water, dispersing 0.02g C 18H29NaO3 S in the mixed solution, stirring for 30min in a water bath kettle with the temperature of 60 ℃, transferring the stirred mixed solution into an autoclave with a Teflon lining with the temperature of 80mL, storing in a drying oven with the temperature of 90 ℃ for 12h, and finally repeatedly centrifuging and cleaning a reaction product with ultrapure water and ethanol, and drying at the temperature of 70 ℃ for 6h to obtain the target product MoS 2/Fe2O3.
SERS experiments of BPA:
In the experiment, coupling reaction of phenolic estrogens and Baoli reagent is adopted to enhance the adhesive force between MoS 2/Fe2O3 substrate and BPA; three reagents were first prepared, reagent a:4.5g of p-aminobenzenesulfonic acid is dissolved in 500mL of ultrapure water, and then 5mL of 12M hydrochloric acid is added and stirred uniformly; reagent B:0.5g sodium nitrite was dissolved in 9.5mL ultrapure water; reagent C:1g of anhydrous sodium carbonate was dissolved in 9mL of ultrapure water; then preparing a BPA solution: 0.0228g of BPA powder was weighed and dissolved in 100mL of alcohol to give 10 -4 M of PBA solution (other concentrations were obtained by dilution); preparing a reagent A, a reagent B, a reagent C and a BPA solution into a coupling reagent according to a volume ratio of 1:1:1:2; finally 25. Mu.L of coupling agent and an equal amount of MoS 2/Fe2O3 ethanol solution (10 -4 M) were added dropwise to the aluminium pan for subsequent testing.
Photocatalytic experiments of BPA:
0.05g MoS 2/Fe2O3 catalyst was dispersed in 100ml aqueous solution made up of 0.001g BPA; the test solution always maintains the magnetic stirring process in the catalytic test process; firstly, adsorbing the sample in a darkroom for 10min, and then irradiating the sample under an ultraviolet lamp, wherein the sample is collected every 10 min; after each harvest, the catalyst was separated from the BPA solution by centrifugation for uv testing.
The invention has the advantages and positive effects that:
1. The preparation method of the invention (shown in figure 1) is simple, low in cost and environment-friendly, and synthesizes the composite material of Fe 2O3 nanometer particles attached to MoS 2 nanometer flowers, namely MoS 2/Fe2O3 (shown in figure 2). The target product MoS 2/Fe2O3 nano composite material provided by the invention has the advantages of high efficiency, ultrasensitivity, good stability, reusability and the like when being used as an SERS substrate, has ultrahigh sensitivity in the aspect of trace detection of BPA, and has the detection limit as low as 1X 10 -9 M (shown in figure 3).
2. The MoS 2/Fe2O3 nano composite material of the target product has degradability to BPA, and 0.05g of MoS 2/Fe2O3 catalyst is dispersed in 100ml of aqueous solution prepared from 0.001g of BPA, and is irradiated by ultraviolet light. The test solution maintains a magnetic stirring process throughout the catalytic test. Sample collection was performed every 10 min. After each harvest, the catalyst was separated from the BPA solution by centrifugation for uv testing. The degradation rate of BPA is up to 91% in 50min (shown in figure 4).
3. The MoS 2/Fe2O3 nano composite material of the target product can also realize recycling. Based on the magnetic properties of Fe 2O3, uniformly dispersed MoS 2/Fe2O3 can be rapidly separated from the solution by means of an external magnet, forming aggregates within 22 s. And any harm of the sample remaining in the environment is avoided. Proved by verification, the recovered MoS 2/Fe2O3 still has higher activity and can be recycled at least 5 times (as shown in figure 5). The recycling can save a great deal of time and cost in practical application, and has important research value and good application prospect in the field of preparing environment-friendly materials.
4. The MoS 2/Fe2O3 nanocomposite of the target product can realize trace detection of BPA and degrade the BPA under ultraviolet light, and has the advantage of recycling. The environment-friendly material is simple in preparation process and low in cost, is beneficial to large-scale production, lays a solid foundation for practical application in the future, and has wide application prospects in the fields of food safety, material science, environment monitoring and the like. At present, no relevant literature report of the multifunctional environment-friendly material exists.
Drawings
FIG. 1 is a flow chart of the preparation of the target product MoS 2/Fe2O3 of the present invention.
Fig. 2 (a) and (b) are scanning electron microscope and transmission electron microscope views of the target product MoS 2/Fe2O3 of the present invention.
FIG. 3 is a SERS spectrum of the target product MoS 2/Fe2O3 of the present invention for detecting BPA of different concentrations.
FIG. 4 is a UV spectrum of the target product MoS 2/Fe2O3 of the present invention degrading BPA in different UV irradiation times.
FIG. 5 is a SERS spectrum of the target product MoS 2/Fe2O3 of the present invention after 5 recoveries.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and specific examples.
The preparation method of the MoS 2/Fe2O3 nanocomposite in the embodiment comprises the following steps:
①、MoS2 Preparation of nanoflower: first, 0.5g H 4MoNa2O6 and 0.7g of CH 4N2 S were mixed in 70mL of ultrapure water, and magnetically stirred for 20 minutes to obtain a uniform solution. Then, 0.5g C 6H8O7·H2 O was added to the above solution and stirred until completely dissolved. The resulting mixed solution was then transferred to an 80mL teflon lined autoclave. Placing in a drying oven, and preserving at 220-240 deg.C for 22-24 hr. And after the reaction is finished and cooled to room temperature, repeatedly centrifuging and cleaning the reaction product by using deionized water and ethanol, and finally drying at 70 ℃ for 6 hours to obtain MoS 2 powder.
②、MoS2/Fe2O3 Preparation of nanocomposite: first, 0.2g of the prepared MoS 2 powder, 0.5. 0.5g H 18FeN3O18 and 0.7. 0.7g H 2NCONH2 were weighed out and mixed and dissolved in 70mL of ultra pure water. Then 0.02g C 18H29NaO3 S was dispersed in the mixed solution and placed in a water bath at 60℃for stirring for 30min. The above solution was transferred to an 80mL teflon lined autoclave and stored in a 90 ℃ dry box for 12 hours. Finally, the reaction product is repeatedly centrifugally washed by ultrapure water and ethanol, and is dried for 6 hours at 70 ℃ to obtain the target product MoS 2/Fe2O3 (shown in figure 2).
The preparation flow chart of the MoS 2/Fe2O3 nanocomposite obtained in this example is shown in fig. 1, and SEM and TEM images are shown in fig. 2.
Application example 1
In this example, the concentration of BPA to be detected was 10 -4-10-9 M, and the process was as follows:
And taking alcohol solutions with different BPA concentrations as treatment objects to carry out SERS detection. Before the experiment was carried out, we designed a coupling reaction of phenolic estrogens with a Baoli reagent in order to enhance the adhesion between MoS 2/Fe2O3 substrate and BPA. We first prepared a warranty agent, comprising three agents altogether. Reagent A:4.5g of p-aminobenzenesulfonic acid was dissolved in 500mL of ultrapure water, and 5mL of 12M hydrochloric acid was added thereto and stirred uniformly. Reagent B:0.5g of sodium nitrite was dissolved in 9.5mL of ultrapure water. Reagent C:1g of anhydrous sodium carbonate was dissolved in 9mL of ultrapure water.
Preparation of BPA alcoholic solution: 0.0228g of BPA powder was weighed and dissolved in 100mL of alcohol to give 10 -4 M of PBA solution (other concentrations obtained by dilution). Reagent a, reagent B, reagent C and BPA solution were formulated as coupling reagents in a 1:1:1:2 volume ratio.
25 Μl of coupling agent and an equal amount of MoS 2/Fe2O3 ethanol solution (10 -4 M) were instilled into an aluminum pan for SERS testing. The SERS test conditions were 514.5nmAr + lasers with a laser power of 80mW, an attenuation of 50%, an exposure time of 30s, and 2 scans per spectrum. As can be seen from fig. 3, the detection limit is as low as 10 -9 M, which indicates that the sample of the present invention has high SERS detection sensitivity.
Application example 2
In the embodiment, the concentration of BPA to be subjected to photocatalytic degradation is 0.01g/L, and the treatment process is as follows:
The BPA waste liquid with the concentration of 0.01g/L is taken as a treatment object to carry out photocatalysis degradation. 0.05g of MoS 2/Fe2O3 catalyst was dispersed in a 100ml aqueous solution of 0.001g BPA. Before photocatalytic degradation, dark adsorption treatment is required to be carried out on the BPA waste liquid, and after a benefit device is built, the dark adsorption treatment is carried out for 10min.
The photodegradation test was then performed, and the test solution was kept magnetically stirred throughout the catalytic test. The mixed solution was irradiated under an ultraviolet lamp, and sample collection was performed every 10 min. After each acquisition, the MoS 2/Fe2O3 catalyst was separated from the BPA waste liquid by centrifugation for uv testing, as shown in fig. 4, with a degradation rate of BPA up to 91% in 50 min.
Application example 3
The MoS 2/Fe2O3 nanocomposite prepared in this embodiment can be recycled as SERS substrate, and the processing procedure is as follows:
The procedure of application example 1 was repeated except that the cyclic test was conducted using a BPA alcohol solution having a concentration of 10 -4 M as the treatment object during the test. Based on the magnetic properties of Fe 2O3, the uniformly dispersed MoS 2/Fe2O3 can be rapidly separated from the solution by means of an external magnet after SERS test, and aggregates can be formed within 22 s. And any harm of the sample remaining in the environment is avoided.
In this embodiment, experiments prove that the recovered MoS 2/Fe2O3 substrate still has high SERS activity and can be reused at least 5 times, as shown in fig. 5. The recycling can save a great deal of time and cost in practical application, and has important research value and good application prospect in the field of preparing environment-friendly materials.
As can be seen from the above examples, the MoS 2/Fe2O3 nanocomposite which is a target product prepared by the method can not only realize trace detection of BPA but also degrade the BPA under ultraviolet light, and has the advantage of recycling. The environment-friendly material is simple in preparation process and low in cost, is beneficial to large-scale production, lays a solid foundation for practical application in the future, and has wide application prospects in the fields of food safety, material science, environment monitoring and the like.
The foregoing detailed description of the embodiments and advantages of the invention will be presented in terms of a detailed description of the invention, and the invention is not intended to be limited to the particular embodiments disclosed, but rather is to be accorded the full scope of the invention as defined by the following claims.
Claims (5)
1. The preparation method of the environment-friendly molybdenum disulfide/ferric oxide nanocomposite is characterized by comprising the following steps of: the method comprises the following steps:
①、MoS2 Preparation of nanoflower: mixing 0.5 g H 4MoNa2O6 and 0.7 g CH 4N2 S in 70mL of ultrapure water, magnetically stirring for 20min to obtain a uniform solution, adding 0.5 g C 6H8O7·H2 O into the solution, stirring to completely dissolve, transferring the obtained mixed solution into an 80mL Teflon-lined autoclave, placing the autoclave in a drying oven, preserving at 220-240 ℃ for 22-24h, cooling to room temperature after the reaction is finished, repeatedly centrifuging and cleaning the reaction product with deionized water and ethanol for three times, and finally drying at 70 ℃ for 6h to obtain pure MoS 2 powder;
②、MoS2/Fe2O3 Preparation of nanocomposite: weighing 0.2 g of MoS 2 powder prepared in the step ①, 0.5 g g H 1 8FeN3O1 8 and 0.7 g H 2NCONH2, mixing and dissolving in 70mL of ultrapure water, dispersing 0.02g g C 18H29NaO3 S in the mixed solution, placing in a water bath kettle with the temperature of 60 ℃ for stirring for 30min, transferring the solution into an autoclave with the temperature of 80mL Teflon lining, placing in a drying oven with the temperature of 90 ℃ for preserving for 12h, repeatedly centrifuging and cleaning the reaction product with ultrapure water and ethanol for three times, and drying at the temperature of 70 ℃ for 6h to obtain the target product MoS 2/Fe2O3 nanocomposite.
2. The application of the molybdenum disulfide/ferric oxide nanocomposite prepared by the preparation method of the environment-friendly molybdenum disulfide/ferric oxide nanocomposite in the aspect of hypersensitive SERS detection of bisphenol A.
3. The application of the molybdenum disulfide/ferric oxide nanocomposite prepared by the preparation method of the environment-friendly molybdenum disulfide/ferric oxide nanocomposite in the aspect of hypersensitive SERS detection of bisphenol A, which is characterized in that: the MoS 2/Fe2O3 nano composite material is used as a SERS substrate for a trace detection experiment of BPA, and in the experiment, the coupling reaction of phenolic estrogen and a Baoli reagent is adopted to enhance the adhesive force between the MoS 2/Fe2O3 substrate and BPA molecules; method for sample preparation before SERS test: three reagent configuration Baoli reagents were first prepared, reagent A: 4.5 g of p-aminobenzenesulfonic acid is dissolved in 500mL of ultrapure water, 5mL of 12M hydrochloric acid is added, and the mixture is stirred uniformly, and reagent B: 0.5g sodium nitrite was dissolved in 9.5 mL ultrapure water, reagent C:1g of anhydrous sodium carbonate was dissolved in 9mL of ultrapure water, and then a BPA solution was prepared: 0.0228 g of BPA powder is weighed and dissolved in 100mL of alcohol to obtain 10-4M PBA solution, and other concentrations are obtained through dilution; preparing a reagent A, a reagent B, a reagent C and a BPA solution into a coupling reagent according to a volume ratio of 1:1:1:2; finally, 25 mu L of coupling agent and 10 -4 M of equivalent MoS 2/Fe2O3 ethanol solution are dripped into an aluminum plate for subsequent testing; SERS test conditions: the 514.5 nm laser has a power of 80mw and an exposure time of 30s, and the number of times is counted twice.
4. The application of the molybdenum disulfide/ferric oxide nanocomposite prepared by the preparation method of the environment-friendly molybdenum disulfide/ferric oxide nanocomposite in bisphenol A photocatalytic degradation.
5. The application of the molybdenum disulfide/ferric oxide nanocomposite prepared by the preparation method of the environment-friendly molybdenum disulfide/ferric oxide nanocomposite in bisphenol A photocatalytic degradation is characterized in that: the MoS 2/Fe2O3 nano composite material as a target product is used as a photocatalyst for a catalytic degradation experiment of BPA; photocatalytic experiments of BPA: 0.05 gMoS 2/Fe2O3 catalyst was dispersed in 100ml of aqueous solution prepared from 0.001 g BPA, the test solution was kept magnetically stirred throughout the catalytic test, the test solution was first adsorbed in the dark for 10min, then irradiated under an ultraviolet lamp, sample collection was performed every 10min, and after each collection, the catalyst was separated from the BPA solution by centrifugation for ultraviolet testing.
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