CN114804206A - Molybdenum sulfide nano material and preparation method and application thereof - Google Patents
Molybdenum sulfide nano material and preparation method and application thereof Download PDFInfo
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- CN114804206A CN114804206A CN202210338595.6A CN202210338595A CN114804206A CN 114804206 A CN114804206 A CN 114804206A CN 202210338595 A CN202210338595 A CN 202210338595A CN 114804206 A CN114804206 A CN 114804206A
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- molybdenum sulfide
- molybdenum
- nano material
- antibiotic
- nanomaterial
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title description 10
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 40
- 229960005404 sulfamethoxazole Drugs 0.000 claims abstract description 23
- JLKIGFTWXXRPMT-UHFFFAOYSA-N sulphamethoxazole Chemical compound O1C(C)=CC(NS(=O)(=O)C=2C=CC(N)=CC=2)=N1 JLKIGFTWXXRPMT-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002135 nanosheet Substances 0.000 claims abstract description 19
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 17
- 230000000593 degrading effect Effects 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 7
- 229910052802 copper Inorganic materials 0.000 claims abstract description 7
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 23
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 18
- 230000003115 biocidal effect Effects 0.000 claims description 17
- 230000015556 catabolic process Effects 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 238000006731 degradation reaction Methods 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 11
- 229910052750 molybdenum Inorganic materials 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 239000011733 molybdenum Substances 0.000 claims description 10
- 239000003463 adsorbent Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 238000004729 solvothermal method Methods 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 7
- 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 claims description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 3
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 3
- 239000011609 ammonium molybdate Substances 0.000 claims description 3
- 229940010552 ammonium molybdate Drugs 0.000 claims description 3
- XYXNTHIYBIDHGM-UHFFFAOYSA-N ammonium thiosulfate Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=S XYXNTHIYBIDHGM-UHFFFAOYSA-N 0.000 claims description 3
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- 238000003911 water pollution Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 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 compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 2
- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical compound [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 claims description 2
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 2
- 239000011229 interlayer Substances 0.000 abstract description 14
- 229940088710 antibiotic agent Drugs 0.000 abstract description 13
- 238000001179 sorption measurement Methods 0.000 description 27
- 238000003917 TEM image Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- -1 biochar Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 125000004434 sulfur atom Chemical group 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229910052745 lead Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000976924 Inca Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000003920 environmental process Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- ZSDSQXJSNMTJDA-UHFFFAOYSA-N trifluralin Chemical compound CCCN(CCC)C1=C([N+]([O-])=O)C=C(C(F)(F)F)C=C1[N+]([O-])=O ZSDSQXJSNMTJDA-UHFFFAOYSA-N 0.000 description 1
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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
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0218—Compounds of Cr, Mo, W
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- 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
- C02F1/722—Oxidation by peroxides
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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Abstract
The invention discloses sulfurThe molybdenum sulfide nano material is assembled by molybdenum sulfide nano sheets; the maximum distance between two adjacent molybdenum sulfide nanosheets is greater than 0.6 nm; the composition molecule of the molybdenum sulfide nanosheet is MoS x X is 1.2 to 2.3; the specific surface area of the nano material is 3.5-18 m 2 (ii) in terms of/g. The molybdenum sulfide nano material has larger specific surface area and wider interlayer spacing, can provide more active sites for adsorbing heavy metals and degrading antibiotics, and can adsorb heavy metals including Pd, Cu and Cd and degrade antibiotics including sulfamethoxazole simultaneously.
Description
Technical Field
The invention relates to the field of materials, in particular to a molybdenum sulfide nano material and a preparation method and application thereof.
Background
In recent years, the treatment of heavy metal and antibiotic combined pollution in water bodies is receiving great attention. Heavy metals, as a toxic and non-degradable elemental species, are easily concentrated in the environment and are difficult to remove from ecosystems through natural environmental processes. Based on this, an inexpensive and simple efficient adsorption method has proven to be one of the most promising methods for removing heavy metals. And the antibiotic is taken as a novel pollutant, and the adsorption treatment only transfers the medium and cannot fundamentally remove the antibiotic. Further, the best treatment of antibiotics is to degrade into carbon dioxide and water, thereby minimizing its environmental impact. Therefore, many materials based on adsorption or advanced oxidation principles have been developed and applied to the removal of heavy metals or antibiotics, such as biochar, carbon nanotubes, carbon nitride, MOFs, and the like. Wherein MoS 2 As one of two-dimensional transition metal sulfides, the metal sulfide has wide application in a plurality of fields, and MoS is also applied to some researchers 2 For treatment of heavy metals, but existing MoS 2 The material can only treat single heavy metal, can not simultaneously adsorb multiple heavy metals, and the water body pollution has multiple heavy metal pollution, which greatly limits MoS 2 Application in water treatment.
Currently for two-dimensional MoS 2 The synthesis method of the nano-sheet mainly comprises a stripping method (physical and chemical) and a hydrothermal synthesis methodAnd a template method, but the mechanical stripping method has low efficiency, the chemical stripping method has harsh operating environment and more limitations, and the yield of the two methods is extremely low. In contrast, the hydrothermal synthesis method is simple to operate and has the potential of large-scale production.
Disclosure of Invention
In order to overcome the problems of the prior art, the invention provides a molybdenum sulfide nano material.
The second purpose of the invention is to provide a preparation method of the molybdenum sulfide nano material.
The invention also aims to provide a heavy metal adsorbent.
The fourth purpose of the invention is to provide an antibiotic degrading agent.
The fifth purpose of the invention is to provide a using method of the antibiotic degrading agent.
The invention also aims to provide the application of the molybdenum sulfide nano material in water pollution treatment.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the invention provides a molybdenum sulfide nano material, wherein the nano material is assembled by molybdenum sulfide nano sheets; the maximum distance between two adjacent molybdenum sulfide nanosheets is greater than 0.6 nm; the composition molecule of the molybdenum sulfide nanosheet is MoS x X is 1.2 to 2.3; the specific surface area of the nano material is 3.5-18 m 2 /g。
Preferably, the specific surface area of the nano material is 10-18 m 2 (ii)/g; further preferably, the specific surface area of the nano material is 10.9-17.8 m 2 /g。
Preferably, the composition molecule of the molybdenum sulfide nanosheet is MoS x X is 2-2.3; further preferably, the composition molecule of the molybdenum sulfide nanosheet is MoS x And x is 2.2 to 2.3.
Preferably, the molybdenum sulfide nanosheets are petal-shaped; the thickness of the molybdenum sulfide nanosheet is 0.01-2 nm.
The second aspect of the present invention provides a method for preparing the molybdenum sulfide nano material provided by the first aspect of the present invention, comprising the following steps: and reacting the molybdenum source and the sulfur source by adopting a solvothermal method to prepare the molybdenum sulfide nano material.
Preferably, the ratio of the molar weight of molybdenum atoms in the molybdenum source to the molar weight of sulfur in the sulfur source is 1: 2-2.2; further preferably, the ratio of the molar amount of molybdenum atoms in the molybdenum source to the molar amount of sulfur in the sulfur source is 1: 2.15.
Preferably, the molybdenum source comprises at least one of ammonium molybdate, ammonium molybdate tetrahydrate, sodium molybdate, potassium molybdate, ammonium paramolybdate, sodium paramolybdate, potassium paramolybdate, molybdenum trioxide; further preferably, the molybdenum source comprises at least one of ammonium molybdate, ammonium molybdate tetrahydrate.
Preferably, the sulfur source comprises at least one of thioacetamide, thiourea, ammonium sulfide, sodium sulfide, potassium sulfide, carbon disulfide, sodium thiosulfate, potassium thiosulfate, ammonium thiosulfate; further preferably, the sulfur source comprises at least one of thiourea, sodium thiosulfate, potassium thiosulfate, ammonium thiosulfate.
Preferably, the solvent comprises at least one of water, a water/ethanol mixture and ethanol.
Preferably, the water/ethanol mixed solution is a mixed solution of water and ethanol in any proportion; more preferably, in the water/ethanol mixed solution, the volume ratio of water to ethanol is 1: (1-20); still more preferably, in the water/ethanol mixed solution, the volume ratio of water to ethanol is 1: (5-10); more preferably, in the water/ethanol mixed solution, the volume ratio of water to ethanol is 1:5 or 1: 10.
preferably, the solvothermal reaction is specifically: mixing a sulfur source, a molybdenum source and a solvent, and then reacting for 10-24 hours at 180-240 ℃.
Preferably, the mixing step employs at least one of mechanical agitation mixing, ultrasonic mixing.
Preferably, the mixing time is 20-60 min; further preferably, the mixing time is 30-50 min; still further preferably, the mixing time is 30-40 min.
Preferably, the heating rate of the solvothermal reaction is 1-10 ℃/min; further preferably, the heating rate of the solvothermal reaction is 3-8 ℃/min; still further preferably, the temperature rise rate of the solvothermal reaction is 5-8 ℃/min. The heating rate can affect the progress of the solvothermal reaction, if the heating rate is too high, the molybdenum source and the sulfur source react faster, the molybdenum sulfide nano material with a special structure in the invention cannot be formed, and if the heating rate is too low, the reaction time is prolonged, so that the production cost is increased.
The third aspect of the invention provides a heavy metal adsorbent, which comprises the molybdenum sulfide nano material provided by the first aspect of the invention.
Preferably, the heavy metal comprises Pd, Cu, Cd.
Preferably, the concentration of the heavy metal detectable by the heavy metal adsorbent is 10-300 mg/L.
Preferably, the concentration range of detectable Pd of the heavy metal adsorbent is: 100-300 mg/L.
Preferably, the concentration range of Cu detectable by the heavy metal adsorbent is: 20-80 mg/L.
Preferably, the concentration range of Cd detectable by the heavy metal adsorbent is: 10-30 mg/L.
Preferably, the concentration ratio of the molybdenum sulfide nano material to the heavy metal solution is (1-40): 1.
preferably, the concentration ratio of the molybdenum sulfide nano material to the pd solution is (1-4): 1.
preferably, the concentration ratio of the molybdenum sulfide nano material to the Cu solution is (5-20): 1.
preferably, the concentration ratio of the molybdenum sulfide nanometer material to the Cd solution is (10-40): 1.
preferably, the heavy metal adsorbent is used by the following method: mixing and reacting the molybdenum sulfide nano material with a heavy metal solution.
Preferably, the temperature of the mixing reaction is 20-40 ℃; further preferably, the temperature of the mixing reaction is 25-35 ℃.
Preferably, the mixing reaction time is 4-10 h; further preferably, the mixing reaction time is 5-8 h.
Preferably, the mixing reaction is carried out by shaking the shaking table.
Preferably, the rotating speed of the shaking table is 150-250 r/min; further preferably, the rotating speed of the shaking table is 180-220 r/min; still further preferably, the rotating speed of the shaking table is 180-200 r/min.
Preferably, the pH value of the mixing reaction is 5.5-6.5; further preferably, the pH of the mixing reaction is 6.
The fourth aspect of the invention provides an antibiotic degrading agent, which comprises the molybdenum sulfide nano material provided by the first aspect of the invention.
Preferably, the antibiotic comprises sulfamethoxazole.
A fifth aspect of the present invention provides a method of using the antibiotic-degrading agent provided in the fourth aspect of the present invention, comprising the steps of: mixing a solution to be degraded with the antibiotic degrading agent; or mixing the solution to be degraded with an antibiotic degradation agent and hydrogen peroxide.
The antibiotic degradation agent can react in the absence of hydrogen peroxide, and specifically comprises the following components: only the solution containing the antibiotics and the antibiotic degrading agent are mixed uniformly, and then the partial adsorption of the antibiotics in the solution can be realized.
The antibiotic degradation agent can react in the presence of hydrogen peroxide, and specifically comprises the following components: and uniformly mixing the solution to be degraded containing the antibiotics, the antibiotic degrading agent and hydrogen peroxide, and then quickly degrading the antibiotics in the solution to be degraded.
Preferably, the mixing time is 5min to 60 min; further preferably, the mixing time is 5min to 40 min.
Preferably, the mixing is carried out at a pH of 7.
Preferably, the mixing temperature is 20-40 ℃; further preferably, the mixing temperature is 25-35 ℃.
Preferably, the mixing step is performed by shaking the shaker.
Preferably, the rotating speed of the shaking table is 150-250 r/min; further preferably, the rotating speed of the shaking table is 180-220 r/min; still further preferably, the rotating speed of the shaking table is 180-200 r/min.
A sixth aspect of the invention provides the use of the molybdenum sulphide nanomaterial provided by the first aspect of the invention in water pollution treatment.
The invention has the beneficial effects that: the molybdenum sulfide nano material has larger specific surface area and wider interlayer spacing, can provide more active sites for adsorbing heavy metals and degrading antibiotics, and can adsorb heavy metals including Pd, Cu and Cd and degrade antibiotics including sulfamethoxazole simultaneously.
Secondly, the molybdenum sulfide nano material is synthesized by adopting a solvothermal method, the preparation method is simple, mass production can be realized, the cost is low, the production efficiency and the yield are high, the nano material assembled by the petal-shaped molybdenum sulfide nano sheets is finally synthesized by selecting appropriate reaction conditions of the molybdenum source-sulfur source ratio, the solvent and the like, in the preparation process, the interlayer spacing is furthest enlarged, the specific surface area is increased, more adsorption sites are exposed, and the molybdenum sulfide nano material with the capabilities of adsorbing heavy metals and degrading antibiotics is further synthesized.
In addition, the special molybdenum sulfide nano material structure is utilized to degrade antibiotics in water and adsorb heavy metals in water, so that the water treatment effect is better.
Drawings
FIG. 1 is an SEM image of the molybdenum sulfide nano-materials of examples 1-4.
FIG. 2 is a TEM image of the molybdenum sulfide nanomaterial of examples 1-4.
FIG. 3 is a TEM image of the interlayer spacing of the Mo sulfide nano material in examples 1-4.
FIG. 4 is an adsorption isotherm diagram of heavy metal Cd from the molybdenum sulfide nanomaterial of examples 1-4.
FIG. 5 is a graph showing the adsorption isotherm of the heavy metal Cu by the molybdenum sulfide nanomaterial of examples 1 to 4.
FIG. 6 is a temperature contour diagram of adsorption of heavy metal Pb by the molybdenum sulfide nanomaterial of examples 1-4.
FIG. 7 is a kinetic diagram of adsorption and degradation of SMZ by the molybdenum sulfide nano-materials prepared in examples 1-4.
FIG. 8 is a graph of the adsorption and degradation amounts of the molybdenum sulfide nanomaterials prepared in examples 1-4 to SMZ.
Detailed Description
Specific embodiments of the present invention are described in further detail below with reference to the figures and examples, but the practice and protection of the present invention is not limited thereto. It is noted that the following processes, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
The molybdenum sulfide nano material in the embodiment is prepared by the following preparation method, which specifically comprises the following steps:
the method comprises the following steps: a Mo sample containing 1.24g of ammonium molybdate tetrahydrate (NH4) was weighed 7 O 24 ·4H 2 O and 1.14g of thiourea (CH) 4 N 2 S) in a beaker; measuring 40mL of pure water, adding the pure water into a beaker, vigorously stirring the mixture for 30min by using a magnetic stirrer, and then carrying out ultrasonic treatment for 30min to form a uniform solution;
step two: transferring the uniform solution in the step one into a 100ml stainless steel autoclave with a polytetrafluoroethylene lining, raising the temperature to 200 ℃ at a speed of 6 ℃/min, and then keeping for 12 h.
Step three: after the reaction system is naturally cooled to room temperature, a 0.25 mu m filter membrane is used for suction filtration, deionized water and ethanol are used for washing for 3 times respectively, vacuum drying is carried out at 60 ℃, and the molybdenum sulfide nano material in the embodiment is prepared and sealed for storage.
Example 2
The molybdenum sulfide nano material in the embodiment is prepared by the following preparation method, which specifically comprises the following steps:
the method comprises the following steps: a Mo sample containing 1.24g of ammonium molybdate tetrahydrate (NH4) was weighed 7 O 24 ·4H 2 O and 1.14g of thiourea (CH) 4 N 2 S) in a beaker; measuring 40mL of ethanol-water mixed solution (the volume ratio of water to ethanol is 1:5), adding the mixed solution into a beaker, violently stirring the mixed solution for 30min by a magnetic stirrer, and then carrying out ultrasonic treatment for 30min to form uniform solution;
step two: transferring the uniform solution in the step one into a 100ml stainless steel autoclave with a polytetrafluoroethylene lining, raising the temperature to 200 ℃ at a speed of 6 ℃/min, and then keeping for 12 h.
Step three: after the reaction system is naturally cooled to room temperature, a 0.25 mu m filter membrane is used for suction filtration, deionized water and ethanol are used for washing for 3 times respectively, vacuum drying is carried out at 60 ℃, and the molybdenum sulfide nano material in the embodiment is prepared and sealed for storage.
Example 3
The molybdenum sulfide nano material in the embodiment is prepared by the following preparation method, which specifically comprises the following steps:
the method comprises the following steps: a Mo sample containing 1.24g of ammonium molybdate tetrahydrate (NH4) was weighed 7 O 24 ·4H 2 O and 1.14g of thiourea (CH) 4 N 2 S) in a beaker; measuring 40mL of ethanol-water mixed solution (the volume ratio of water to ethanol is 1:10), adding the mixed solution into a beaker, violently stirring the mixed solution for 30min by a magnetic stirrer, and then carrying out ultrasonic treatment for 30min to form uniform solution;
step two: transferring the uniform solution in the step one into a 100ml stainless steel autoclave with a polytetrafluoroethylene lining, raising the temperature to 200 ℃ at a speed of 6 ℃/min, and then keeping for 12 h.
Step three: after the reaction system is naturally cooled to room temperature, a 0.25 mu m filter membrane is used for suction filtration, deionized water and ethanol are used for washing for 3 times respectively, vacuum drying is carried out at 60 ℃, and the molybdenum sulfide nano material in the embodiment is prepared and sealed for storage.
Example 4
The molybdenum sulfide nano material in the embodiment is prepared by the following preparation method, which specifically comprises the following steps:
the method comprises the following steps: a Mo sample containing 1.24g of ammonium molybdate tetrahydrate (NH4) was weighed 7 O 24 ·4H 2 O and 1.14g of thiourea (CH) 4 N 2 S) in a beaker; measuring 40mL of pure ethanol solution, adding the pure ethanol solution into a beaker, violently stirring the mixture for 30min by a magnetic stirrer, and then carrying out ultrasonic treatment for 30min to form a uniform solution;
step two: transferring the uniform solution in the step one into a 100ml stainless steel autoclave with a polytetrafluoroethylene lining, raising the temperature to 200 ℃ at a speed of 6 ℃/min, and then keeping for 12 h.
Step three: after the reaction system is naturally cooled to room temperature, a 0.25 mu m filter membrane is used for suction filtration, deionized water and ethanol are used for washing for 3 times respectively, vacuum drying is carried out at 60 ℃, and the molybdenum sulfide nano material in the embodiment is prepared and sealed for storage.
Performance testing
(1) Topography testing
Scanning electron microscopes are adopted to respectively test the SEM images of the molybdenum sulfide nano materials in the embodiments 1-4, specifically as shown in FIG. 1, wherein FIG. 1(a) is the SEM image of the molybdenum sulfide nano material in the embodiment 1; FIG. 1(b) is an SEM image of a molybdenum sulfide nanomaterial in example 2; FIG. 1(c) is an SEM image of a molybdenum sulfide nanomaterial in example 3; fig. 1(d) is an SEM image of the molybdenum sulfide nanomaterial in example 4. As can be seen from fig. 1, the molybdenum sulfide nanomaterials in examples 1 to 4 are all assembled by stacking two-dimensional petal-shaped nanosheets.
A transmission electron microscope is adopted to respectively test a TEM image and a TEM image of an interlayer space of the molybdenum sulfide nano material in examples 1-4, specifically shown in FIG. 2 and FIG. 3, wherein FIG. 2(a) is the TEM image of the molybdenum sulfide nano material in example 1; FIG. 2(b) is a TEM image of the molybdenum sulfide nanomaterial in example 2; FIG. 2(c) is a TEM image of the molybdenum sulfide nanomaterial in example 3; fig. 2(d) is a TEM image of the molybdenum sulfide nanomaterial in example 4. FIG. 3(a) is a TEM image of the interlayer spacing of molybdenum sulfide nanomaterial in example 1; FIG. 3(b) is a TEM image of the interlayer spacing of the molybdenum sulfide nanomaterial in example 2; FIG. 3(c) is a TEM image of the interlayer spacing of molybdenum sulfide nanomaterial in example 3; FIG. 3(d) is a TEM image of the interlayer spacing of the molybdenum sulfide nanomaterial in example 4; as can be seen from fig. 2 and 3, the molybdenum sulfide nanomaterials in examples 1 to 4 all have a relatively obvious nanosheet layer structure, and the distance between two adjacent nanosheet layers is relatively large, and the layer distance is greater than 0.6 nm; wherein the interlayer spacing of the molybdenum sulfide nanomaterial in example 1 is 0.62 nm; the interlayer spacing of the molybdenum sulfide nanomaterial in example 2 was 0.64 nm; the interlayer spacing of the molybdenum sulfide nanomaterial in example 3 was 0.69 nm; the interlayer spacing of the molybdenum sulfide nanomaterial in example 4 was 0.67 nm.
(2) Specific surface area
The specific surface area of the molybdenum sulfide nano-materials in examples 1-4 was measured by using a specific surface area tester (Micromeritics TriStar II), and the specific test results are shown in the following Table 1:
TABLE 1 specific surface area of molybdenum sulfide nanomaterials from examples 1 to 4
As can be seen from the above Table 1, the specific surface area of the molybdenum sulfide nano material synthesized by using water as the solvent in the example 1 is the largest, and the value of the specific surface area is 17.60m 2 Example 3 the specific surface area of the molybdenum sulfide nano material synthesized by using the mixed solution of water and ethanol with the volume ratio of 1:10 as the solvent is 10.96m 2 The molybdenum sulfide nano material synthesized by the method has a large specific surface area.
(4) Atomic mole ratio
The average mole percentages of Mo atoms and S atoms in the molybdenum sulfide nanomaterials of examples 1-4 were respectively tested using EDS spectroscopy (INCA ENERGY 350), and the specific test results are shown in table 2 below:
TABLE 2 average mole percent of Mo and S atoms in the molybdenum sulfide nanomaterials of examples 1-4
As can be seen from table 2, the average mole percentage of Mo atoms and S atoms in the molybdenum sulfide nanomaterial synthesized in embodiments 1 to 4 of the present invention is 1: (1.25 to 2.27), the average molar percentage of Mo atoms and S atoms in the molybdenum sulfide nanomaterial in example 2 was 1:1.25, and the average molar percentage of Mo atoms and S atoms in the molybdenum sulfide nanomaterial in example 4 was 1:1.59, which revealed that: certain S defects exist in the molybdenum sulfide nano materials prepared in the examples 2 and 4.
(5) Adsorption property of heavy metal
Respectively adding 0.02g of the molybdenum sulfide nano-materials prepared in the embodiments 1-4 into different 100ml conical flasks, then adding 50ml of Cd, Pb and Cu solutions with different concentration gradients into the conical flasks, and adjusting the pH value of the solution to 6; wherein the concentration range of the Cd solution is 10-30mg/L, the concentration range of the Pb solution is 100-300mg/L, and the concentration range of the Cu solution is 20-80 mg/L; sealing the conical flask, putting the conical flask into a constant-temperature shaking table, reacting for 6 hours at the rotation speed of the shaking table of 180r/min at 25 ℃, determining the concentration of heavy metals in the residual solution by using an atomic absorption spectrophotometer, and then respectively drawing adsorption isotherms of the molybdenum sulfide nano material to the heavy metals Cd, Pb and Cu in the test examples 1-4, specifically referring to figures 4-6, wherein figure 4 is an adsorption isotherm diagram of the molybdenum sulfide nano material to the heavy metal Cd in the examples 1-4; FIG. 5 is a graph showing the adsorption isotherm of the molybdenum sulfide nanomaterial on the heavy metal Cu in examples 1 to 4; FIG. 6 is a temperature contour diagram of adsorption of heavy metal Pb by the molybdenum sulfide nanomaterial of examples 1-4. As can be seen from fig. 4 to 6, the adsorption effect of the molybdenum sulfide nanomaterial of the present invention on heavy metals is: pb > Cu > Cd, the actual maximum adsorption capacity to Cd, Pb and Cu was 30.5, 101.2 and 382.5mg/g respectively. In addition, as can be seen from fig. 4 to 6, the molybdenum sulfide nanomaterial in example 3 of the present invention, i.e., the system using the mixed solution of water and ethanol at a volume ratio of 1:10 as the solvent, exhibits a better adsorption tendency, while the pure ethanol solvent system in example 4 exhibits a stronger adsorption effect on Pb, which may be due to the fact that the molybdenum sulfide nanomaterial exhibits a stronger Pb reduction ability due to S atom defects.
(6) Degradation Properties of SMZ
Respectively test for no H 2 O 2 Adsorption system and activation H 2 O 2 The degradation system of the invention is the degradation performance of the molybdenum sulfide nano material prepared in the embodiment 1-4 on Sulfamethoxazole (SMZ). The specific test method comprises the following steps: (1) no H 2 O 2 When the adsorption system is adopted, 0.02g of molybdenum sulfide nano material and 50mL of SMZ (50mg/L) are added into a 100mL conical flask, and the pH value of the solution is 7; (2) activation of H 2 O 2 In a 100mL conical flask, 0.02g of molybdenum sulfide nanomaterial, 50mL of SMZ (50mg/L) and 0.05mL of H are added 2 O 2 A solution, the pH of the solution being 7; and then sealing the conical flask, putting the conical flask into a constant-temperature shaking table, setting the temperature at 25 ℃, rotating the shaking table at 180r/min, sampling every 30s, 1 mm and 5min, and sampling for 0.5h and 1h, and measuring the concentration of the residual SMZ by using high performance liquid chromatography. The kinetics of adsorption and degradation of SMZ for the molybdenum sulfide nanomaterials prepared in examples 1-4 are shown in FIG. 7, wherein the upper four curves in FIG. 7 are adsorption kinetics curves of examples 1-4 for SMZ, and the lower four curves in FIG. 7 are degradation kinetics curves of examples 1-4 for SMZ. The adsorption and degradation amounts of the molybdenum sulfide nano-materials prepared in the examples 1 to 4 to the SMZ at different times are shown in a graph in FIG. 8, wherein the upper four curves in FIG. 8 are the degradation amount curves of the examples 1 to 4 to the SMZ, and the lower four curves in FIG. 8 are the adsorption amount curves of the examples 1 to 4 to the SMZ. As can be seen from fig. 7 and 8, the molybdenum sulfide nanomaterial of the present invention exhibits a certain adsorption capacity on SMZ, but has a more significant degradation performance, and in addition, the degradation rate on SMZ is fast, so that the SMZ can be rapidly and effectively degraded within 5 min. Wherein, the adopted water in the embodiment 3: the mixed solution with the volume ratio of ethanol being 1:10 is a system with a solvent, the maximum removal amount of SMZ can reach 62.72mg/g, and the molybdenum sulfide nano material has the function of rapidly activating H 2 O 2 The ability to generate free radicals and thus degrade SMZ, while adsorption makes only a small contribution.
In summary, the molybdenum sulfide nano material in the invention hasObvious nano petal shape, large specific surface area and interlayer spacing, and has the functions of adsorbing heavy metal and quickly activating H 2 O 2 The ability of generating free radicals to degrade antibiotics has important application potential for removing heavy metal and antibiotic composite pollutants in environmental water. In addition, by combining the properties of the molybdenum sulfide nano-materials in the embodiments 1 to 4, it can be seen that the molybdenum sulfide nano-material in the embodiment 3 has more excellent overall properties.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the embodiments, and various changes can be made without departing from the gist of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. A molybdenum sulfide nano-material is characterized in that: the nano material is assembled by molybdenum sulfide nanosheets; the maximum distance between two adjacent molybdenum sulfide nanosheets is greater than 0.6 nm; the composition molecule of the molybdenum sulfide nanosheet is MoS x X is 1.2 to 2.3; the specific surface area of the nano material is 3.5-18 m 2 /g。
2. The molybdenum sulfide nanomaterial of claim 1, wherein: the molybdenum sulfide nanosheets are petal-shaped.
3. The method for preparing molybdenum sulfide nano-material according to claim 1 or 2, characterized in that: the method comprises the following steps: and reacting the molybdenum source and the sulfur source by adopting a solvothermal method to prepare the molybdenum sulfide nano material.
4. The method for preparing the molybdenum sulfide nano-material according to claim 3, wherein: the molybdenum source comprises at least one of ammonium molybdate, ammonium molybdate tetrahydrate, sodium molybdate, potassium molybdate, ammonium paramolybdate, sodium paramolybdate, potassium paramolybdate and molybdenum trioxide; the sulfur source comprises at least one of thioacetamide, thiourea, ammonium sulfide, sodium sulfide, potassium sulfide, carbon disulfide, sodium thiosulfate, potassium thiosulfate and ammonium thiosulfate; the solvent comprises at least one of water, water/ethanol mixed solution and ethanol.
5. A heavy metal adsorbent, characterized by: comprising the molybdenum sulfide nanomaterial of claim 1 or 2.
6. The heavy metal adsorbent according to claim 5, characterized in that: the heavy metals include Pd, Cu, Cd.
7. An antibiotic-degrading agent characterized by: comprising the molybdenum sulfide nanomaterial of claim 1 or 2.
8. The antibiotic-degrading agent according to claim 7, wherein: the antibiotic comprises sulfamethoxazole.
9. The method of using the antibiotic-degrading agent of claim 7 or 8, wherein: the method comprises the following steps: mixing a solution to be degraded with the antibiotic degrading agent; or mixing the solution to be degraded with an antibiotic degradation agent and hydrogen peroxide.
10. Use of the molybdenum sulphide nanomaterial of claim 1 or 2 in the treatment of water pollution.
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| CN117101598A (en) * | 2023-10-24 | 2023-11-24 | 南昌航空大学 | Preparation method of molybdenum-based adsorption material, and product and application thereof |
| CN117101598B (en) * | 2023-10-24 | 2024-03-15 | 南昌航空大学 | Preparation method of molybdenum-based adsorption material, and product and application thereof |
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