CN113716671B - Method for treating wastewater based on 1T-phase nano molybdenum disulfide and preparation method of 1T-phase nano molybdenum disulfide - Google Patents
Method for treating wastewater based on 1T-phase nano molybdenum disulfide and preparation method of 1T-phase nano molybdenum disulfide Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 87
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000002351 wastewater Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims description 16
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 16
- 239000012043 crude product Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000013067 intermediate product Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- FHHJDRFHHWUPDG-UHFFFAOYSA-L peroxysulfate(2-) Chemical compound [O-]OS([O-])(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-L 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical group [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 230000000593 degrading effect Effects 0.000 abstract description 29
- 238000006731 degradation reaction Methods 0.000 abstract description 24
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- 230000000694 effects Effects 0.000 abstract description 7
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- 230000003213 activating effect Effects 0.000 abstract description 2
- 238000004729 solvothermal method Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 38
- 239000005906 Imidacloprid Substances 0.000 description 24
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 24
- 229940056881 imidacloprid Drugs 0.000 description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- 239000008367 deionised water Substances 0.000 description 19
- 229910021641 deionized water Inorganic materials 0.000 description 19
- 239000000243 solution Substances 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 11
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
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- 238000012360 testing method Methods 0.000 description 8
- 239000012425 OXONE® Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 description 7
- 238000010791 quenching Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- -1 sulfate radical Chemical class 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 5
- 238000001994 activation Methods 0.000 description 4
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- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
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- 229910052723 transition metal Inorganic materials 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 description 2
- 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 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- PGOOBECODWQEAB-UHFFFAOYSA-N (E)-clothianidin Chemical compound [O-][N+](=O)\N=C(/NC)NCC1=CN=C(Cl)S1 PGOOBECODWQEAB-UHFFFAOYSA-N 0.000 description 1
- HOKKPVIRMVDYPB-UVTDQMKNSA-N (Z)-thiacloprid Chemical compound C1=NC(Cl)=CC=C1CN1C(=N/C#N)/SCC1 HOKKPVIRMVDYPB-UVTDQMKNSA-N 0.000 description 1
- 239000005888 Clothianidin Substances 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical class [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000005940 Thiacloprid Substances 0.000 description 1
- 239000005941 Thiamethoxam Substances 0.000 description 1
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052750 molybdenum Chemical class 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000033458 reproduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 150000003463 sulfur Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
- NWWZPOKUUAIXIW-FLIBITNWSA-N thiamethoxam Chemical compound [O-][N+](=O)\N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-FLIBITNWSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
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- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- 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
- C02F2101/306—Pesticides
-
- 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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- General Physics & Mathematics (AREA)
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- Crystallography & Structural Chemistry (AREA)
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Abstract
The invention relates to a method for treating wastewater based on 1T-phase nano molybdenum disulfide, which comprises the following steps: and (3) blending the 1T-phase nano molybdenum disulfide in persulfate, and putting the mixture into the wastewater for stirring. The invention also relates to a method for treating wastewater based on the 1T-phase nano molybdenum disulfide. The 1T-phase nano molybdenum disulfide with higher purity is prepared by simple, controllable and low-cost solvothermal reaction; the 1T-phase nano molybdenum disulfide disclosed by the invention has higher active site exposure and better electron transfer performance, and has higher efficiency for activating persulfate to generate sulfate radicals, so that the 1T-phase nano molybdenum disulfide is more beneficial to degrading organic matters in wastewater, including neonicotinoid pesticides difficult to degrade by conventional means; preferably, the 1T-phase nano molybdenum disulfide has a high degradation effect on organic matters in wastewater under a low pH condition (pH = 1-3).
Description
Technical Field
The invention belongs to the field of environmental protection, and particularly relates to a method for treating wastewater based on 1T-phase nano molybdenum disulfide and a preparation method of the 1T-phase nano molybdenum disulfide.
Background
In recent years, due to rapid development of intensive agriculture and continuous progress of chemical production technology, the usage amount of pesticides is greatly increased, and most of the pesticides enter natural water bodies through irrigation and precipitation except that a small amount of pesticides are absorbed by crops, so that a large amount of wastewater containing dangerous organic matters exists in the nature. However, many pesticides used in modern agriculture mostly contain heterocyclic structures, such as neonicotinoid pesticides, which have stable chemical structures, are difficult to degrade in natural environments, enter human bodies along with drinking water and food, have persistence, mobility and bioaccumulation, and have potential toxic effects on endocrine, respiration, reproduction, nervous systems and the like of human beings and other organisms.
As a method capable of effectively degrading organic pollutants in water, the advanced oxidation technology has been widely researched and applied all over the world (Current Pollution Reports,2015,1 (3): 167-176). The Fenton oxidation technology based on hydroxyl free radicals OH is most applied in the advanced oxidation technology, but a large amount of iron salt is needed in the Fenton oxidation technology, so a large amount of iron mud is generated in the reaction process, and the risk of secondary pollution is increased; furthermore, the half-life of the hydroxyl radical. OH, the major active oxygen species generated in Fenton's oxidation technology, is short, typically less than 1 μ s, and thus the efficiency of contaminant degradation in the system is very limited (Chemical Engineering Journal,2020, 381; compared with the Fenton oxidation technology, the sulfate radical generated in the persulfate oxidation technology has higher oxidation-reduction potential (2.5-3.1 eV), and the half-life period of the sulfate radical is 30-40 mus, so that the oxidative degradation reaction can be more effectively carried out, and no secondary pollution is generated. The activation mode of the persulfate oxidation method comprises physical methods such as photoactivation, ultrasonic activation, thermal activation and the like, and homogeneous activation technologies such as various transition metal salts, but the homogeneous activation technologies face the problems of difficult recovery and reutilization and secondary pollution to a system (Applied Catalysis B: environmental,2019, 242.
Therefore, in order to overcome the above disadvantages, a technical solution is needed to solve the problem of how to degrade the organic matters in the wastewater.
Disclosure of Invention
In recent years, heterogeneous persulfate oxidation technologies based on various environmental energy supply materials, such as transition metal sulfides, transition metal oxides, bimetallic framework materials, doped compounds, and the like, have been the focus of research. Among the many environmentally energized materials, molybdenum disulfide is of great interest as a typical transition metal sulfide. The nanometer molybdenum disulfide has many excellent physical, optical and electrical properties, and has been researched and applied in the fields of photoelectric components, energy storage and catalysis. Because the lamella of the nano molybdenum disulfide is stripped into a single layer or a few layers, a large number of active sites are exposed, and the nano molybdenum disulfide has excellent catalytic property.
According to the stacking order and the coordination of Mo atoms, the molybdenum disulfide can form three forms of bulk crystal structures, namely a 2H phase with a hexagonal structure, a 3R phase with an orthorhombic hexahedral structure and a 1T phase with a regular octahedral structure, wherein the 1T phase molybdenum disulfide and the 3R phase molybdenum disulfide both belong to a metastable state, and the 2H phase molybdenum disulfide belongs to a stable state, so that the most commonly existing molybdenum disulfide is the 2H phase in nature. In addition, the valence electrons of the molybdenum disulfide of the 2H phase and the 3R phase fill the dz2 orbital in a spin-opposed manner; in the 1T phase molybdenum disulfide, an octahedral coordination structure of a sulfur atom and a molybdenum atom enables vacant orbitals to exist near a Fermi level, so that the 2H phase and the 3R phase belong to a semiconductor phase, and the 1T phase belongs to a metal phase, so that the 1T phase molybdenum disulfide has more excellent conductivity and catalytic activity.
The 1T phase is used as a crystal structure of the molybdenum disulfide, has good conductivity similar to that of pure metal, and is more beneficial to electron transfer, but the 1T phase nano molybdenum disulfide is metastable and almost does not exist in natural environment, so the invention discloses a method for synthesizing the 1T phase nano molybdenum disulfide used as a catalyst of heterogeneous persulfate, and degrading waste water containing organic matters, particularly organic pesticide sewage.
One purpose of the invention is to provide a method for treating wastewater based on 1T-phase nano molybdenum disulfide, which comprises the following steps:
and (3) blending the 1T-phase nano molybdenum disulfide in persulfate, and putting into the wastewater for stirring.
The organic matters in the wastewater can not only comprise common easily degradable bisphenol A, antibiotics and other organic pollutants; and may include polychlorinated biphenyls which are hardly degraded. The technical scheme of the invention also has obvious degradation effect on neonicotinoid pesticides such as imidacloprid and the like which are difficult to degrade in the traditional process.
Further, the persulfate is selected from one of peroxymonosulfate, peroxydisulfate, or a mixture thereof.
Further, the stirring was performed in a light-shielded environment.
Further, the addition amount of the 1T-phase nano molybdenum disulfide accounts for 0.05-0.5g/L of the wastewater; the addition amount of the persulfate accounts for 1.5-12mmol/L of the wastewater.
Further, the pH of the wastewater is 1-3.
Another object of the present invention is to provide the method for preparing 1T-phase nano molybdenum disulfide, wherein the method for preparing 1T-phase nano molybdenum disulfide comprises the following steps:
s1, mixing a sulfur-containing compound and molybdate to form a solution;
s2, heating the solution for reaction to obtain an intermediate product;
s3, centrifuging the intermediate product, taking the precipitate, washing and drying to obtain a solid;
s4, adding the solid into an organic solvent for dispersion, and then heating for reaction to obtain a crude product;
s5, centrifuging the crude product, taking the precipitate, washing and drying to obtain the product.
Further, in S2, the heating temperature is 180-200 ℃; in S4, the heating temperature is 200-220 ℃.
Further, the sulfur-containing compound is selected from thiourea or thioacetamide, and the molybdate is selected from sodium molybdate or ammonium molybdate.
Further, the organic solvent is selected from one or more of methanol, ethanol, propanol and butanol.
Further, the method adopted by the dispersion is ultrasound.
The invention has the following beneficial effects:
1. the technical means disclosed by the invention prepares the 1T-phase nano molybdenum disulfide with higher purity through simple, controllable and low-cost solvothermal reaction;
2. the 1T-phase nano molybdenum disulfide disclosed by the invention has higher active site exposure and better electron transfer performance, and has higher efficiency for activating persulfate to generate sulfate radicals, so that the 1T-phase nano molybdenum disulfide is more beneficial to degrading organic matters in wastewater, including neonicotinoid pesticides difficult to degrade by conventional means.
3. Preferably, the 1T-phase nano molybdenum disulfide has a high degradation effect on organic matters in wastewater under a low pH condition (pH = 1-3).
Drawings
FIG. 1 shows a scanning electron microscope image of 1T phase nano molybdenum disulfide in example 1;
FIG. 2 is a graph showing a comparison of Raman spectra of 1T phase nano-molybdenum disulfide in example 1 and 2H phase nano-molybdenum disulfide in comparative example 1;
FIG. 3 is a graph showing the degradation performance of the samples of example 1 and comparative examples 1 to 5 in test example 1 with respect to organic matters in wastewater;
FIG. 4 is a graph showing the degradation performance of the samples of example 1 and comparative examples 6 to 9 in test example 2 with respect to organic matters in wastewater;
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are listed. The starting materials, reactions and work-up procedures which are given in the examples are, unless otherwise stated, those which are customary on the market and are known to the person skilled in the art.
The frequency used by the ultrasound of the embodiment of the invention is 40KHz;
the 2H-phase nano molybdenum disulfide disclosed by the embodiment of the invention is prepared by a hydrothermal reaction in a laboratory in Journal of hazardous Materials 394 (2020) 122525;
the molybdenum disulfide of the micron-sized particles is purchased from Shanghai Michelin Biochemical technology Co., ltd, and has the model of AR,99 percent and less than 2 mu m.
Example 1
A preparation method of 1T phase nano molybdenum disulfide comprises the following steps:
s1, 1mmol of ammonium paramolybdate tetrahydrate ((NH) 4 ) 6 Mo 7 O 24 ·4H 2 O), with 30mmol of thiourea (CS (NH) 2 ) 2 ) Dissolving in 35ml of deionized water, and stirring for 30min to form a solution;
s2, transferring the solution into a high-pressure reaction kettle with the capacity of 200ml and a PPL material lining, heating for 24 hours at 180 ℃, and then cooling to room temperature to obtain an intermediate product;
s3, centrifuging the intermediate product at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate by using deionized water and ethanol, and performing vacuum drying at the temperature of 60 ℃ to obtain a solid;
s4, adding the solid into absolute ethyl alcohol, performing ultrasonic dispersion treatment for 30min, and then transferring the solid into a reaction kettle at 200 ℃ to react for 8h to obtain a crude product;
s5, centrifuging the crude product at the rotating speed of 4000rpm to obtain a precipitate, washing with deionized water, and drying in vacuum at 100 ℃ to obtain the product 1T-phase nano molybdenum disulfide.
Fig. 1 shows a scanning electron microscope image of 1T-phase nano molybdenum disulfide, and it can be seen from the image that 1T-phase nano molybdenum disulfide is in a typical nano flower shape and is agglomerated to a certain extent, which indicates that the size of the synthesized molybdenum disulfide reaches the nano level.
The method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide comprises the following steps:
s1, preparing organic wastewater by using deionized water and imidacloprid stock solution with the concentration of 100ppm in a reagent bottle with the capacity of 500 ml. The amounts of the deionized water and the imidacloprid stock solution are 180mL and 20mL respectively, namely the concentration of the imidacloprid is diluted by 10 times, the concentration of the imidacloprid participating in the degradation reaction is 10ppm, and the pH value of the wastewater containing organic matters is adjusted to 3;
s2, 0.01g of 1T-phase nano molybdenum disulfide and 1.2mmol of potassium monopersulfate are put into 200ml of the waste water of the organic matters to obtain a mixture. And stirring the mixture at the rotating speed of 600rpm under the conditions of normal temperature and light protection, thereby degrading organic matters in the wastewater.
Example 2
A preparation method of 1T-phase nano molybdenum disulfide comprises the following steps:
s1, adding 2mmol of ammonium molybdate tetrahydrate ((NH) 4 ) 6 Mo 7 O 24 ·4H 2 O), with 20mmol of thioacetamide (CH) 3 CSNH 2 ) Dissolving in 35ml of deionized water, and stirring for 30min to form a solution;
s2, transferring the solution into a high-pressure reaction kettle which has the capacity of 200ml and is made of PPL material as a lining, heating for 20 hours at 185 ℃, and then cooling to room temperature to obtain an intermediate product;
s3, centrifuging the intermediate product at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate by using deionized water and ethanol, and performing vacuum drying at the temperature of 60 ℃ to obtain a solid;
s4, adding the solid into absolute ethyl alcohol, performing ultrasonic dispersion treatment for 30min, and then transferring the solid into a reaction kettle at 210 ℃ for reaction for 9h to obtain a crude product;
s5, centrifuging the crude product at the rotating speed of 4000rpm to obtain a precipitate, washing with deionized water, and drying in vacuum at 100 ℃ to obtain the product 1T-phase nano molybdenum disulfide.
The method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide comprises the following steps:
s1, preparing organic wastewater by using deionized water and thiamethoxam stock solution with the concentration of 50ppm in a reagent bottle with the capacity of 500 ml. The amounts of the deionized water and the imidacloprid stock solution are respectively 360mL and 40mL, namely the concentration of the imidacloprid is diluted by 10 times, the concentration of the imidacloprid participating in the degradation reaction is 5ppm, and the pH value of the wastewater containing organic matters is adjusted to 3;
s2, 0.02g of 1T-phase nano molybdenum disulfide and 2.4mmol of potassium peroxodisulfate are put into 400ml of waste water of the organic matters to obtain a mixture. And stirring the mixture at the rotating speed of 600rpm under the conditions of normal temperature and light protection, thereby degrading the organic matters in the wastewater.
Example 3
A preparation method of 1T-phase nano molybdenum disulfide comprises the following steps:
s1, adding 2mmol of sodium molybdateDihydrate (Na) 2 MoO 4 ·2H 2 O), with 6mmol of thiourea (CS (NH) 2 ) 2 ) Dissolving in 35ml of deionized water, and stirring for 30min to form a solution;
s2, transferring the solution into a high-pressure reaction kettle with the capacity of 200ml and a PPL material lining, heating for 21h at 190 ℃, and then cooling to room temperature to obtain an intermediate product;
s3, centrifuging the intermediate product at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate by using deionized water and ethanol, and performing vacuum drying at the temperature of 60 ℃ to obtain a solid;
s4, adding the solid into absolute ethyl alcohol, performing ultrasonic dispersion treatment for 30min, and then transferring the solid into a reaction kettle at 220 ℃ for reaction for 10h to obtain a crude product;
s5, centrifuging the crude product at the rotating speed of 4000rpm to obtain a precipitate, washing with deionized water, and drying in vacuum at 100 ℃ to obtain the product 1T-phase nano molybdenum disulfide.
The method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide comprises the following steps:
s1, preparing organic wastewater by using deionized water and thiacloprid stock solution with the concentration of 200ppm in a reagent bottle with the capacity of 500 ml. The amounts of the deionized water and the imidacloprid stock solution are 270mL and 30mL respectively, namely the concentration of the imidacloprid is diluted by 10 times, the concentration of the imidacloprid participating in the degradation reaction is 20ppm, and the pH value of the wastewater containing organic matters is adjusted to 3;
s2, 0.05g of 1T-phase nano molybdenum disulfide and 6mmol of potassium monopersulfate are put into 200ml of the waste water of the organic matters to obtain a mixture. And stirring the mixture at the rotating speed of 500rpm under the condition of normal temperature and light protection, thereby degrading the organic matters in the wastewater.
Example 4
A preparation method of 1T-phase nano molybdenum disulfide comprises the following steps:
s1, adding 3mmol of sodium molybdate dihydrate (Na) 2 MoO 4 ·2H 2 O), with 10mmol of thioacetamide (CH) 3 CSNH 2 ) Dissolved in 35ml of deionized waterStirring in water for 30min to obtain solution;
s2, transferring the solution into a high-pressure reaction kettle with the capacity of 200ml and a PPL material lining, heating for 22h at the temperature of 200 ℃, and then cooling to room temperature to obtain an intermediate product;
s3, centrifuging the intermediate product at the rotating speed of 4000rpm to obtain a precipitate, washing the precipitate by using deionized water and ethanol, and performing vacuum drying at the temperature of 60 ℃ to obtain a solid;
s4, adding the solid into absolute ethyl alcohol, performing ultrasonic dispersion treatment for 30min, and then transferring the solid into a reaction kettle at 220 ℃ for reaction for 11h to obtain a crude product;
s5, centrifuging the crude product at the rotating speed of 4000rpm to obtain a precipitate, washing with deionized water, and drying in vacuum at 100 ℃ to obtain the product 1T-phase nano molybdenum disulfide.
The method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide comprises the following steps:
s1, preparing organic wastewater by using deionized water and clothianidin stock solution with the concentration of 100ppm in a reagent bottle with the capacity of 500 ml. The amounts of the deionized water and the imidacloprid stock solution are 190mL and 10mL respectively, namely the concentration of the imidacloprid is diluted by 10 times, the concentration of the imidacloprid participating in the degradation reaction is 5ppm, and the pH value of the wastewater containing organic matters is adjusted to 3;
s2, 0.1g of 1T-phase nano molybdenum disulfide and 12mmol of potassium peroxodisulfate are put into 200ml of the waste water of the organic matters to obtain a mixture. And stirring the mixture at the rotating speed of 400rpm under the conditions of normal temperature and light protection, thereby degrading the organic matters in the wastewater.
Comparative example 1
The preparation method of the comparative example 1 is the same as that of the example 1 and the method for degrading organic matters in wastewater, and the only difference is that the 1T phase nano molybdenum disulfide in the comparative example 1 is replaced by 2H phase nano molybdenum disulfide with equal amount of substances.
Figure 2 shows a comparison of raman spectra of 1T phase nano molybdenum disulfide in example 1 and 2H phase nano molybdenum disulfide in comparative example 1. As can be seen from the figure, the 1T-phase nano molybdenum disulfide prepared in example 1 has a typical characteristic peak at a corresponding wavelength, and is obviously different from the 2H-phase nano molybdenum disulfide prepared in comparative example 1, which indicates that the 1T-phase nano molybdenum disulfide prepared in example 1 is successfully prepared.
Comparative example 2
Comparative example 2 is the same as example 1 in both the preparation method and the method for degrading organic matters in wastewater, and the only difference is that the 1T phase nano molybdenum disulfide described in comparative example 2 is replaced by micron-sized particles of molybdenum disulfide in equal amount.
Comparative example 3
The comparative example 3 is the same as the preparation method of the example 1 and the method for degrading organic matters in wastewater, and the only difference is that the method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide described in the comparative example 3 does not contain the 1T-phase nano molybdenum disulfide.
Comparative example 4
The comparative example 4 is the same as the preparation method of the example 1 and the method for degrading the organic matters in the wastewater, and the only difference is that the method for degrading the organic matters in the wastewater by using the 1T-phase nano molybdenum disulfide described in the comparative example 4 does not contain potassium monopersulfate.
Comparative example 5
Comparative example 5 is a blank control, i.e. with only organic-containing wastewater.
Comparative example 6
Comparative example 6 is the same as example 1 in both the preparation method and the method of degrading organic substances in wastewater, with the only difference that,
in the method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide described in the comparative example 6, the pH value of the wastewater containing the organic matters is adjusted to 5.
Comparative example 7
Comparative example 7 is the same as example 1 in both the preparation method and the method of degrading organic substances in wastewater, with the only difference that,
in the method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide described in the comparative example 7, the pH value of the wastewater containing the organic matters is adjusted to 7.
Comparative example 8
Comparative example 8 is the same as example 1 in both the preparation method and the method of degrading organic substances in wastewater, with the only difference that,
in the method for degrading organic matters in wastewater by using the 1T-phase nano molybdenum disulfide as described in the comparative example 8, the pH value of the wastewater containing the organic matters is adjusted to 9.
Comparative example 9
Comparative example 9 is the same as the preparation method of example 1 and the method for degrading organic matters in wastewater, and the only difference is that in the method for degrading organic matters in wastewater by using 1T-phase nano molybdenum disulfide described in comparative example 9, the pH value of wastewater containing organic matters is adjusted to 11.
Test example 1
In order to test the degradation performance of the samples of the above example 1, and comparative examples 1 to 5 on organic matters in wastewater, the following test experiments were made.
The real-time monitoring of step S2 in the process of degrading organics in wastewater in example 1 and comparative examples 1-5 was performed by: sampling the mixture by a liquid-moving machine at the reaction time of 0, 1, 5, 15, 30, 60, 90, 120, 150 and 180 min; then methanol is used as a free radical quenching agent and added into the sample to quench the reaction; then diluting the sample by 10 times with ultrapure water, filtering by using a 0.22 mu m filter head, and adding methanol serving as a free radical quencher into the sample to quench the reaction; and finally, carrying out quantitative analysis on the degraded sample by using a liquid chromatography-mass spectrometer.
The results are shown in FIG. 3. As can be seen from FIG. 3, in example 1, due to the use of 1T-phase nano molybdenum disulfide, after mixing potassium monopersulfate, the degradation performance of imidacloprid, which is an organic substance in wastewater, is very significant. The relevant data are shown in table 1.
It should be noted that, the degradation rate formula is: eta =1- (C) t /C 0 )
Wherein: eta-degradation rate
C t -concentration of Imidacloprid in the Water sample at time t (mg/L)
C 0 -concentration of Imidacloprid in Water sample at time 0Degree, i.e. initial concentration of imidacloprid in the water sample (mg/L)
As can be seen from the above table, when the degradation reaction proceeded for 180min, the imidacloprid concentration in the wastewater added with the sample of example 1 was reduced to below 270ppb, the degradation rate reached above 70%, and the degradation effect was significant. In the wastewater of the comparative examples 1 to 5, the imidacloprid concentration is still high, which shows that the samples of the comparative examples 1 to 5 have very little degradation performance on the imidacloprid.
Test example 2
In order to test the degradation performance of the samples of the above example 1, and comparative examples 6 to 9 on the organic matter in wastewater, the following test experiments were conducted.
The real-time monitoring of step S2 of the method for degrading organic substances in wastewater section of example 1 and comparative examples 6 to 9 was carried out by: sampling the mixture by a liquid-moving machine at the reaction time of 0, 1, 5, 15, 30, 60, 90, 120, 150 and 180 min; then methanol is used as a free radical quenching agent and added into the sample to quench the reaction; then diluting the sample by 10 times with ultrapure water, filtering by using a 0.22 mu m filter head, and adding methanol serving as a free radical quenching agent into the sample to quench the reaction; and finally, carrying out quantitative analysis on the degraded sample by using a liquid chromatography-mass spectrometer.
The results are shown in FIG. 4. As can be seen from fig. 4, in example 1, because 1T-phase nano molybdenum disulfide is used, and after potassium monopersulfate is mixed, and the pH is 3, the degradation performance of the organic imidacloprid in the wastewater is very significant. The relevant data are shown in table 2.
TABLE 2 degradation Rate data for Imidacloprid for the samples of example 1, comparative examples 6-9
As can be seen from the above table, when the pH is in a strongly acidic condition of 3, the sample has a good effect of degrading in wastewater; as the pH value is increased, the degradation performance is poorer and poorer, and the alkaline environment can cause the degradation effect to be poorer.
The main reason is that the acidic condition is more favorable for promoting the dissociation of the added 1T-phase nano molybdenum disulfide in the wastewater to form naked Mo (IV), then the active unsaturated Mo (IV) 4d orbit transfers electrons to potassium monopersulfate to destroy-O-O-bonds to form sulfate radical SO-4 and Mo (V), mo (V) further transfers electrons to potassium monopersulfate to generate SO-4 and Mo (VI), and further the degradation effect of the system on imidacloprid is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.
Claims (4)
1. A method for treating wastewater based on 1T-phase nano molybdenum disulfide is characterized by comprising the following steps:
blending 1T-phase nano molybdenum disulfide and persulfate, and putting into the wastewater for stirring;
the pH value of the wastewater is 1-3;
the preparation method of the 1T-phase nano molybdenum disulfide comprises the following steps:
s1, forming a solution by using a sulfur-containing compound and molybdate;
s2, heating the solution for reaction to obtain an intermediate product;
s3, centrifuging the intermediate product, taking the precipitate, washing and drying to obtain a solid;
s4, adding the solid into an organic solvent for dispersion, and then heating for reaction to obtain a crude product;
s5, centrifuging the crude product, taking the precipitate, washing and drying to obtain a product;
the stirring is carried out in a dark environment;
in S2, the heating temperature is 180-200 ℃; in S4, the heating temperature is 200-220 ℃;
the sulfur-containing compound is selected from thiourea or thioacetamide, and the molybdate is selected from sodium molybdate or ammonium molybdate.
2. The method for treating wastewater based on 1T-phase nano molybdenum disulfide according to claim 1, wherein the persulfate is selected from one of peroxymonosulfate and peroxydisulfate or a mixture thereof.
3. The method for treating wastewater based on 1T-phase nano molybdenum disulfide according to claim 1, wherein the addition amount of 1T-phase nano molybdenum disulfide accounts for 0.05-0.5g/L of the wastewater; the addition amount of the persulfate accounts for 1.5-12mmol/L of the wastewater.
4. The method for treating wastewater based on 1T-phase nano molybdenum disulfide according to claim 1, wherein the organic solvent is selected from one or more of methanol, ethanol, propanol and butanol.
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