CN115709098A - Synthetic method and application of ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite - Google Patents
Synthetic method and application of ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite Download PDFInfo
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- ferroferric oxide
- molybdenum disulfide
- dodecyl sulfate
- sodium dodecyl
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- 238000010189 synthetic method Methods 0.000 title abstract description 4
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- LSQZJLSUYDQPKJ-NJBDSQKTSA-N amoxicillin Chemical compound C1([C@@H](N)C(=O)N[C@H]2[C@H]3SC([C@@H](N3C2=O)C(O)=O)(C)C)=CC=C(O)C=C1 LSQZJLSUYDQPKJ-NJBDSQKTSA-N 0.000 claims description 2
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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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Abstract
The invention relates to a synthetic method and application of a ferroferric oxide-molybdenum disulfide-lauryl sodium sulfate nano compound, wherein the preparation method comprises the following steps: weighing ferric trichloride hexahydrate, sodium acetate and polyethylene glycol, measuring a glycol solution, and uniformly stirring; then transferring the mixture to a high-pressure reaction kettle for reaction; separating the product, washing and drying to obtain a ferroferric oxide nano material; ferroferric oxide, thioacetamide and sodium molybdate di Shui Ke are dissolved in pure water and are stirred uniformly; transferring the mixed solution into a high-pressure reaction kettle for reaction; (separating the product, washing and drying to obtain the ferroferric oxide-molybdenum disulfide nano compound, then mixing the ferroferric oxide-molybdenum disulfide nano compound and sodium dodecyl sulfate in pure water according to the same mass proportion, carrying out ultrasonic treatment, separating the product, washing and drying to obtain the nano compound).
Description
Technical Field
The invention relates to a ferroferric oxide-molybdenum disulfide-lauryl sodium sulfate nano compound and a method for catalytically degrading antibiotics under visible light, belonging to the technical field of nano biology.
Background
With the improvement of living standard, the demand of human beings for meat, eggs and milk is continuously increased, and antibiotics such as tetracycline, sulfadiazine and terramycin are widely applied to livestock and poultry industry and aquaculture industry. The long-term residue of antibiotics in the environment can induce the proliferation of drug-resistant genes and drug-resistant bacteria to enhance the drug resistance of sensitive bacteria, and the drug-resistant genes can be continuously expanded and evolved in the environment, so that the effective dose of the antibiotics is continuously increased, and the effectiveness of common antibiotics is greatly reduced. Antibiotic residues pose a potential threat to the ecological environment and also pose a serious threat to human health. Residual antibiotics in the environment can be transferred from the environmental compartment to the drinking water source and, in addition, most antibiotics are poorly metabolized and, after absorption by the treated person or animal, the residual parent compound or metabolite thereof can eventually be discharged into the aqueous environment, posing significant environmental and public health risks. Thus, the removal of antibiotic residues from the environment has received considerable attention.
Spinel ferrite (NiFe) with super-strong magnetism and visible light response 2 O 4 , CoFe 2 O 4 , CdFe 2 O 4 Etc.) have been widely studied as photocatalysts. Molybdenum sulfide at the lower valence band site exhibits strong oxidation and hole-generating ability. Thus, molybdenum sulfide is a very potential magnetic separation visible light photocatalyst. To date, some molybdenum sulfide-based photocatalysts have been constructed. However, the photocatalytic molybdenum sulfide-based material has a low activity, poor electron conductivity and is severely limited by its low potentialThe charge recombination rate is high. The heterogeneous interface can accelerate the separation of hole and electron and reduce the recombination of charges, and the sodium dodecyl sulfate modification can improve the dispersion performance of the compound and the effective site combined with the substrate. In the work, the ferroferric oxide-molybdenum disulfide-lauryl sodium sulfate composite material is prepared by a hydrothermal ultrasonic method. The existence of ferroferric oxide and sodium dodecyl sulfate effectively improves the light absorption of molybdenum sulfide, and has higher efficiency of catalyzing and degrading antibiotics under visible light.
Disclosure of Invention
The invention aims to solve the problems, and provides a synthetic method and application of a ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound, namely the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound and a method for catalytically degrading antibiotics under visible light.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite is characterized in that the synthesis method comprises the following steps:
(1) Weighing 1.4 to 1.6 grams of ferric trichloride hexahydrate, 2.0 to 2.2 grams of sodium acetate and 0.9 to 1.1 grams of polyethylene glycol, measuring 40ml of ethylene glycol solution, and uniformly stirring to obtain a mixed solution;
(2) Transferring the mixed solution obtained in the step (1) into a high-pressure reaction kettle, and reacting for several hours at 160 to 200 ℃;
(3) Separating the product obtained in the step (2), washing and drying to obtain a ferroferric oxide nano material;
(4) Respectively weighing 0.1 to 0.5 g of ferroferric oxide obtained in the step (3), 0.2 to 0.4 g of thioacetamide and 0.1 to 0.3 g of sodium molybdate dihydrate, dissolving in deionized water, and uniformly stirring;
(5) Transferring the mixed solution in the step (4) into a high-pressure reaction kettle, and reacting for several hours at the temperature of 170 to 200 ℃;
(6) Separating the product obtained in the step (5), washing and drying to obtain a ferroferric oxide-molybdenum disulfide nano compound;
(7) Mixing the ferroferric oxide-molybdenum disulfide nano compound obtained in the step (6) and sodium dodecyl sulfate in the deionized water according to the same mass ratio, and performing ultrasonic treatment;
(8) And (5) separating the product obtained in the step (7), washing and drying to obtain the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound.
In the step (2), the reaction time is 15 to 20 hours.
In the step (3), the centrifugal rotation speed of the solution is 6000 to 9000 rpm, and the centrifugal time is 10 to 30 minutes; the drying temperature is 60 to 80 ℃, and the drying time is 8 to 12 hours.
In the step (4), the stirring time is 20 to 40 minutes.
In the step (5), the reaction time is 15 to 25 hours.
In the step (6), the centrifugation speed is 5000 to 10000 r/min, the centrifugation time is 5 to 20 minutes, the drying temperature is 50 to 80 ℃, and the time is 4~8 hours.
A method for degrading antibiotics by ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound under the catalysis of visible light is characterized in that the detection operation process is as follows:
a) Weighing 3~9 mg tetracycline hydrochloride, adding into deionized water, and stirring uniformly;
b) Weighing 10 to 30 milligrams of ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound, and adding the nano compound into the solution obtained in the step a);
c) Placing the mixed solution obtained in the step b) into a photocatalysis reaction instrument, and magnetically stirring and uniformly dispersing in the dark;
d) A xenon lamp light source with an ultraviolet filter is turned on, and a condensation circulating water system is turned on, so that the temperature is stable;
e) Extracting reaction suspension in a given irradiation time interval, and filtering through a filter membrane to remove particles;
f) Putting the liquid obtained in the step e) into an ultraviolet-visible spectrophotometer to read under a specific wavelength;
g) And f), obtaining the efficiency of degrading the antibiotic by the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound according to the data obtained in the step f).
In the step a), the amount of deionized water is 30 to 70 milliliters;
in the step c), the magnetic stirring speed is 600 to 1000rpm;
in the step d), the xenon lamp light source power is 200 to 500W, and the reaction temperature is 15 to 30 ℃;
in the step e), the irradiation time interval is 15 to 45 minutes, 3~8 milliliters of reaction suspension is extracted, and the aperture size of a filter membrane is 0.1 to 0.3 micrometer;
in the step f), setting the wavelength of the ultraviolet-visible spectrophotometer to be 300-700 nm.
The antibiotics include but are not limited to tetracycline, ciprofloxacin, amoxicillin, sulfadiazine.
Compared with the prior art, the invention has the following beneficial effects:
1. the too high or too low dosage of the ferroferric oxide in the step (4) is not beneficial to photocatalytic degradation of antibiotics, and the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound prepared by the invention has the advantages that: has excellent photocatalytic degradation performance.
2. And (3) sealing the mixed solution obtained in the step (5) in a high-pressure reaction kettle, generating high pressure in the reaction kettle along with the temperature rise to 170-200 ℃, fully dispersing thioacetamide and sodium molybdate in an aqueous solution under a high-temperature and high-pressure physical and chemical environment, and ensuring that incomplete vulcanization can form a ferroferric oxide/molybdenum disulfide heterostructure after reaction for 15-25 hours, so that more reaction sites are obtained, and the charge transmission performance is improved.
3. In the step a) and the step b), the addition amount of the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound is about 25 mg/50 ml, and the photocatalytic degradation efficiency of the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound on tetracycline is highest.
The method comprises the following steps: further mixing ferric trichloride hexahydrate, sodium acetate, polyethylene glycol and glycol solution under magnetic stirring; then transferring the prepared solution into a high-pressure autoclave reaction kettle, continuously reacting for a certain time, and cooling to room temperature; centrifuging for many times and washing with deionized water and ethanol; and drying overnight to obtain ferroferric oxide.
Preparing aqueous solution of thioacetamide and sodium molybdate dihydrate, and mixing ferroferric oxide therein; transferring the obtained mixed solution into a high-pressure kettle for reaction; after centrifugal separation, washing the mixture for many times by using ethanol and deionized water; drying to obtain a finished product of ferroferric oxide-molybdenum disulfide;
mixing ferroferric oxide-molybdenum disulfide and sodium dodecyl sulfate in water according to the same mass ratio, carrying out ultrasonic treatment for several hours, and washing and drying to obtain the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite. And dispersing the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound in a mixed solution of deionized water and antibiotics by magnetic stirring, and turning on a xenon lamp with an ultraviolet filter. The result proves that under visible light, the ferroferric oxide-molybdenum disulfide-lauryl sodium sulfate nano compound has improved charge transfer and separation efficiency and improved photocatalytic antibiotic degradation efficiency.
According to the invention, the ferroferric oxide-molybdenum disulfide-lauryl sodium sulfate composite material is prepared by adopting a hydrothermal ultrasonic method, and the existence of the ferroferric oxide and the lauryl sodium sulfate effectively improves the light absorption of molybdenum sulfide, so that the composite material has higher efficiency of catalyzing and degrading antibiotics under visible light. Due to the harm of antibiotics, the use of antibiotics is limited or reduced in more and more fields at present, and the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite nano material has high efficiency of catalyzing and degrading the antibiotics under visible light, so that the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite nano material has wide application prospect in degrading the antibiotics in the environment.
Drawings
Fig. 1 is a scanning transmission electron microscope image of the ferriferrous oxide-molybdenum disulfide-sodium dodecyl sulfate composite of example 1 of the present invention.
FIG. 2 is an X-ray diffraction diagram of a ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate compound in example 2 of the present invention.
Fig. 3 is a graph of tetracycline degradation efficiency of the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite in example 3 of the present invention under visible light.
Detailed Description
The preparation of the ferriferrous oxide-molybdenum disulfide-sodium dodecyl sulfate composite is further illustrated by the following specific examples.
Example 1:
FIG. 1 is a scanning transmission electron microscope image of the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite prepared by the invention.
Example 2:
The crystal structure of the obtained ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound is shown in figure 2, and the compound can be determined to be composed of ferroferric oxide, molybdenum disulfide and sodium dodecyl sulfate.
Example 3:
25 mg of the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound prepared in the example 2 is put into 50 ml of tetracycline hydrochloride (25 ppm) solution, magnetic stirring is carried out for 30 minutes in the dark, after adsorption and desorption balance is achieved, a xenon lamp light source with an ultraviolet filter (more than 420 nm) is turned on, samples are taken for 5 ml within two hours at intervals of half an hour, and after filtration, the degradation performance is detected by an ultraviolet visible spectrophotometer at 357nm, wherein the degradation performance is shown in figure 3.
As can be seen in fig. 3: the efficiency of the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nanocomposite for photocatalytic degradation of tetracycline hydrochloride is about 92.4%. Compared with other photocatalytic composite materials, the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite has relatively high efficiency under visible light.
Claims (9)
1. The ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite is characterized in that the synthesis method comprises the following steps:
(1) Weighing 1.4 to 1.6 grams of ferric trichloride hexahydrate, 2.0 to 2.2 grams of sodium acetate and 0.9 to 1.1 grams of polyethylene glycol, measuring 40ml of ethylene glycol solution, and uniformly stirring to obtain a mixed solution;
(2) Transferring the mixed solution obtained in the step (1) into a high-pressure reaction kettle, and reacting for several hours at 160 to 200 ℃;
(3) Separating the product obtained in the step (2), washing and drying to obtain a ferroferric oxide nano material;
(4) Respectively weighing 0.1 to 0.5 g of ferroferric oxide, 0.2 to 0.4 g of thioacetamide and 0.1 to 0.3 g of sodium molybdate dihydrate which are obtained in the step (3), dissolving in deionized water, and uniformly stirring;
(5) Transferring the mixed solution in the step (4) into a high-pressure reaction kettle, and reacting for several hours at the temperature of 170 to 200 ℃;
(6) Separating the product obtained in the step (5), washing and drying to obtain a ferroferric oxide-molybdenum disulfide nano compound;
(7) Mixing the ferroferric oxide-molybdenum disulfide nano compound obtained in the step (6) and sodium dodecyl sulfate in pure water according to the same mass ratio, and performing ultrasonic treatment;
(8) And (5) separating the product obtained in the step (7), washing and drying to obtain the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite.
2. The ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite according to claim 1, which is characterized in that: in the step (2), the reaction time is 15 to 20 hours.
3. The ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite according to claim 1, which is characterized in that: in the step (3), the centrifugal rotation speed of the solution is 6000 to 9000 r/min, and the centrifugal time is 10 to 30 minutes; the drying temperature is 60 to 80 ℃, and the drying time is 8 to 12 hours.
4. The ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite according to claim 1, which is characterized in that: in the step (4), the stirring time is 20 to 40 minutes.
5. The ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite according to claim 1, which is characterized in that: in the step (5), the reaction time is 15 to 25 hours.
6. The ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano composite according to claim 1, which is characterized in that: in the step (6), the centrifugal rotation speed is 5000 to 10000 rpm, the centrifugal time is 5 to 20 minutes, the drying temperature is 50 to 80 ℃, and the time is 4~8 hours.
7. The method for catalytically degrading antibiotics by ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound under visible light as claimed in any one of claims 1 to 6, which is characterized in that the detection operation process is as follows:
a) Weighing 3~9 mg tetracycline hydrochloride, adding into deionized water, and stirring uniformly;
b) Weighing 10 to 30 milligrams of ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound, and adding the nano compound into the solution obtained in the step a);
c) Placing the mixed solution obtained in the step b) into a photocatalysis reaction instrument, and magnetically stirring and uniformly dispersing in the dark;
d) A xenon lamp light source with an ultraviolet filter is turned on, and a condensation circulating water system is turned on, so that the temperature is stable;
e) Extracting reaction suspension in a given irradiation time interval, and filtering through a filter membrane to remove particles;
f) Putting the liquid obtained in the step e) into an ultraviolet-visible spectrophotometer to read under a specific wavelength;
g) And f), obtaining the efficiency of degrading the antibiotic by the ferroferric oxide-molybdenum disulfide-sodium dodecyl sulfate nano compound according to the data obtained in the step f).
8. The method of claim 7, wherein:
in the step a), the amount of deionized water is 30 to 70 milliliters;
in the step c), the magnetic stirring speed is 600 to 1000rpm;
in the step d), the power of a xenon lamp light source is 200 to 500W, and the reaction temperature is 15 to 30 ℃;
in the step e), the irradiation time interval is 15 to 45 minutes, 3~8 ml of reaction suspension is extracted, and the aperture size of the filter membrane is 0.1 to 0.3 micron;
in the step f), the wavelength of the ultraviolet-visible spectrophotometer is set to be 300-700 nm.
9. The method of claim 7, wherein: the antibiotics include but are not limited to tetracycline, ciprofloxacin, amoxicillin, sulfadiazine.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104941667A (en) * | 2015-05-20 | 2015-09-30 | 扬州大学 | Petal-shaped magnetic ferric oxide molybdenum sulfide compound and preparation method thereof |
| CN105776349A (en) * | 2016-03-14 | 2016-07-20 | 金堆城钼业股份有限公司 | Preparation method of layered MoS2-Fe3O4 nanocomposite |
| CN109589994A (en) * | 2018-12-28 | 2019-04-09 | 福建江夏学院 | A kind of molybdenum disulfide-carbon nanotube optic catalytic composite material and its synthetic method |
| CN109806889A (en) * | 2019-02-25 | 2019-05-28 | 宁夏大学 | A kind of molybdenum disulfide/ferroferric oxide magnetic nano composite material and preparation method and application |
| CN114392355A (en) * | 2022-01-22 | 2022-04-26 | 扬州大学 | Fe3O4@MoS2Preparation method and application of @ SDS composite nano material |
-
2022
- 2022-11-30 CN CN202211513369.3A patent/CN115709098A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104941667A (en) * | 2015-05-20 | 2015-09-30 | 扬州大学 | Petal-shaped magnetic ferric oxide molybdenum sulfide compound and preparation method thereof |
| CN105776349A (en) * | 2016-03-14 | 2016-07-20 | 金堆城钼业股份有限公司 | Preparation method of layered MoS2-Fe3O4 nanocomposite |
| CN109589994A (en) * | 2018-12-28 | 2019-04-09 | 福建江夏学院 | A kind of molybdenum disulfide-carbon nanotube optic catalytic composite material and its synthetic method |
| CN109806889A (en) * | 2019-02-25 | 2019-05-28 | 宁夏大学 | A kind of molybdenum disulfide/ferroferric oxide magnetic nano composite material and preparation method and application |
| CN114392355A (en) * | 2022-01-22 | 2022-04-26 | 扬州大学 | Fe3O4@MoS2Preparation method and application of @ SDS composite nano material |
Non-Patent Citations (1)
| Title |
|---|
| XIAOZI LIN ET AL.: "Magnetically Recyclable MoS2/Fe3O4 Hybrid Composite as Visible Light Responsive Photocatalyst with Enhanced Photocatalytic Performance", 《ACS SUSTAINABLE CHEM. ENG.》, vol. 7, pages 4 - 5 * |
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