CN110918108A - MXene composite nano material and preparation method and application thereof - Google Patents
MXene composite nano material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 36
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 35
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 31
- 230000001699 photocatalysis Effects 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011248 coating agent Substances 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 16
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000010936 titanium Substances 0.000 claims abstract description 9
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims abstract description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims abstract description 6
- 229940012189 methyl orange Drugs 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 24
- 238000005507 spraying Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 15
- 239000000853 adhesive Substances 0.000 claims description 10
- 230000001070 adhesive effect Effects 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000000945 filler Substances 0.000 claims description 9
- 239000002105 nanoparticle Substances 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000002351 wastewater Substances 0.000 claims description 7
- 229910044991 metal oxide Inorganic materials 0.000 claims description 6
- 150000004706 metal oxides Chemical class 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical group [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004098 Tetracycline Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 5
- 229960003742 phenol Drugs 0.000 claims description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 5
- 229940043267 rhodamine b Drugs 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 5
- 229960002180 tetracycline Drugs 0.000 claims description 5
- 229930101283 tetracycline Natural products 0.000 claims description 5
- 235000019364 tetracycline Nutrition 0.000 claims description 5
- 150000003522 tetracyclines Chemical class 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical group [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002135 nanosheet Substances 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 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
- 239000000919 ceramic Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 12
- 239000010842 industrial wastewater Substances 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 abstract 2
- 238000010438 heat treatment Methods 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 9
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- 230000015556 catabolic process Effects 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
- 210000000056 organ Anatomy 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
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- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- 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
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention discloses an MXene composite nano material and a preparation method thereof. The composite nano material comprises the following components: 5-15% MoS23 to 10 percent of MXene and the balance of TiO2. The preparation method comprises the following steps: mixing Ti3AlC2Dissolving the aluminum alloy into a hydrofluoric acid solution with the concentration of 35-40%, removing an aluminum layer in the hydrofluoric acid solution by magnetic stirring, cleaning and centrifuging to remove the residual hydrofluoric acid solution, and drying overnight to obtain etched MXene; ultrasonically dispersing the mixture in water to form a dispersion, sequentially adding soluble molybdenum salt, hydroxylamine chloride, thiourea and a titanium source under magnetic stirring, stirring and addingAdding a surfactant, reacting for 16-32 hours at 170-200 ℃, cleaning, centrifuging, removing supernatant, and drying in vacuum. The photocatalytic coating can effectively degrade organic pollutants such as methyl orange and the like in industrial wastewater. The preparation method has the advantages of low cost, simple and easily-controlled production process and high product yield.
Description
Technical Field
The invention relates to the field of nano composite materials, in particular to an MXene composite nano material and a preparation method and application thereof.
Background
TiO2The TiO-based catalyst has the advantages of high oxidation efficiency, no toxicity, good light stability, low cost, environmental friendliness and the like, and is paid attention to by researchers, but the TiO-based catalyst is2The problems of high recombination rate of electron-hole pairs of the photocatalyst, low sunlight utilization rate and the like cause the photocatalyst to be difficult to apply to the field of photocatalysis on a large scale.
Novel two-dimensional materials such as MoS2MXene has proved to be an excellent photocatalytic cocatalyst due to the advantages of unique layered structure, high specific surface area, high conductivity, adjustable band gap and the like. Recent reports have confirmed MoS2Or MXene as cocatalyst for modifying TiO2Can effectively overcome the defects of the photocatalyst, thereby improving the photocatalytic performance of the photocatalyst. And MoS2Co-modification of TiO with MXene2MoS of (1)2/MXene/TiO2The ternary photocatalytic system and the application thereof in the degradation treatment of organic pollutants in industrial wastewater are not reported.
Disclosure of Invention
One of the purposes of the invention is to provide an MXene composite nanometer material. The specific technical scheme is as follows:
an MXene composite nano material comprises the following components in percentage by mass: 5-15% MoS23 to 10 percent of MXene and the balance of TiO2。
Preferably, the MXene is in a shape of nanosheet with a thickness of 200-2Is 20-50nm thick and is TiO2The particle size of (A) is 10-20 nm.
The invention also aims to provide a preparation method of the MXene composite nanometer material. The specific technical scheme is as follows:
a preparation method of MXene composite nanometer material comprises the following steps:
(1) etching of MXene
Mixing Ti3AlC2Dissolving the aluminum-containing solution into 35-40% hydrofluoric acid solution, magnetically stirring for 10-15 h to remove the aluminum layer, washing with water, centrifuging to remove the residual hydrofluoric acid solution, and drying at 70-90 DEG CObtaining etched MXene at night;
(2)MoS2/MXene/TiO2preparation of composite nano material
Weighing etched MXene, dispersing in water, performing ultrasonic treatment for more than 5min, performing magnetic stirring for 10-60min to form MXene dispersion liquid, sequentially adding soluble molybdenum salt, hydroxylamine chloride, thiourea and a titanium source into the MXene dispersion liquid, stirring for more than 10min, adding a surfactant, continuously stirring for more than 20min, reacting for 16-32 h at 170-200 ℃, alternately washing with water and absolute ethyl alcohol to be clean, centrifuging, removing a supernatant, and performing vacuum drying at 70-90 ℃ for more than 5h to obtain MoS2/MXene/TiO2Composite nanomaterial, namely the MXene composite nanomaterial; the mass ratios, namely the concentrations, of the etched MXene, the soluble molybdenum salt, the hydroxylamine chloride, the thiourea, the titanium source and the surfactant relative to water are respectively 0.5-1.2 g/L, 15-20 g/L, 10-20 g/L, 25-35 g/L, 4-50 g/L and 3-5 g/L.
Preferably, the soluble molybdenum salt is sodium molybdate or ammonium molybdate.
Preferably, the titanium source is tetrabutyl titanate or ammonium fluorotitanate.
Preferably, the surfactant is cetyltrimethylammonium bromide, polyethylene glycol or polyvinylpyrrolidone.
The invention also aims to provide application of the MXene composite nano material. The specific technical scheme is as follows:
an MXene composite nano material is applied to a photocatalytic coating.
A method for applying MXene composite nano material to photocatalytic coating comprises the following steps: mixing MoS2/MXene/TiO2Mixing the composite nano material with a nano metal oxide curing agent and a nano filler, ball-milling for 0.5-5 h, then dropwise adding an inorganic adhesive with the concentration of 1.25-15 g/L, and uniformly mixing to prepare a spraying slurry; spraying the spraying slurry on the surface of the pretreated base material under the process conditions that the spraying speed is 0.3-1.0 m/s and the air pressure is 0.3-1.0 MPa, then preserving heat for 5-10 min at 80-120 ℃, then preserving heat for 10-15 min at 220-300 ℃, and finally preserving heat for 400-450 DEG CPreserving heat for 30-40 min, cooling to room temperature along with the furnace, then washing to be clean with clean water, and airing to obtain MoS coated on the surface of the base material2/MXene/TiO2A composite photocatalytic coating; the MoS2/MXene/TiO2The mass ratio of the composite nano material to the nano metal oxide curing agent to the nano filler to the inorganic adhesive is 1: 0.4-1.6: 0.1-5: 0.25-3; the inorganic adhesive is silicate solution, borate solution or phosphate solution; the nano filler is aluminum powder and Al with the granularity of 100-200 nm2O3Powder or SiO2Pulverizing; the substrate is a glass, ceramic or metal material.
Preferably, the nano metal oxide curing agent is CuO nano particles, ZnO nano particles or MgO nano particles with the particle size of 50-100 nm; the inorganic adhesive is water-soluble sodium silicate solution, sodium borate solution or aluminum dihydrogen phosphate solution.
Preferably, the MoS is applied2/MXene/TiO2The composite photocatalytic coating is used for photocatalytic degradation of organic matters in wastewater, and is illuminated for 0.5-1h under the condition of visible light; the organic matter is rhodamine B, methyl orange, phenol or tetracycline.
The invention has the beneficial effects that:
the invention provides a MoS by adopting a two-step synthesis method2/MXene/TiO2Preparation of composite photocatalytic material by MoS2Co-modified TiO with MXene2So as to obtain the multifunctional nano composite material with high adsorption and photocatalytic performance, and the multifunctional nano composite material is applied to the adsorption and photocatalytic degradation treatment of organic pollutants in industrial wastewater.
MoS of the invention2/MXene/TiO2The degradation rate of the composite photocatalytic coating to rhodamine B in wastewater can reach more than 90 percent within 45 minutes; and the degradation rates of methyl orange, phenol and tetracycline in 1 hour are respectively over 90%, 80% and 70%. The preparation method has the advantages of low cost, simple and easily-controlled production process and high product yield, and is suitable for large-scale industrial production.
Drawings
FIG. 1 shows MoS obtained in examples 1 to 3 of the present invention2/MXene/TiO2CompoundingXRD pattern of the nanomaterial.
FIG. 2 in FIG. 2, FIG. 2a and FIG. 2b show MoS prepared by examples 1 to 3 of the present invention2/MXene/TiO2Scanning Electron Microscopy (SEM) images of the composite nanomaterials, and fig. 2c is a Transmission Electron Microscopy (TEM) image thereof.
Detailed Description
The present invention will be further described below by way of specific embodiments, and it is apparent from the technical knowledge that the present invention can be described by other means without departing from the technical features of the present invention, and therefore all changes within the scope of the present invention or the equivalent scope of the present invention are encompassed by the present invention.
Example 1
A preparation method of MXene composite nanometer material comprises the following steps:
(1) etching of MXene
Mixing 1g of Ti3AlC2Dissolving the powder into 15mL of hydrofluoric acid (HF) solution (the concentration is 35-40%), magnetically stirring for 12h to remove an aluminum layer, washing with deionized water for several times, centrifuging to remove the residual hydrofluoric acid solution, and drying at 80 ℃ overnight to obtain black powder, namely etched MXene. (2) MoS2/MXene/TiO2Preparation of composite nano material (MXene composite nano material)
34mg of etched MXene is weighed and dispersed in 50mL of deionized water, and the mixture is subjected to ultrasonic treatment for 10min and magnetic stirring for 20min by an ultrasonic cleaning machine to form a uniform and stable solution. Then, 0.88g of sodium molybdate (Na2MoO 4. multidot.2H2O), 0.725g of hydroxylamine chloride, 1.4g of thiourea (CH4NS2) and 1.6mL of tetrabutyl titanate were added to the MXene dispersion in this order, and stirred for 1 hour. 0.18g of cetyltrimethylammonium bromide (CTAB) was then added, stirring was continued for 30min, and the solution was then transferred to a 60mL stainless steel autoclave lined with polytetrafluoroethylene, placed in a forced draft oven at 180 ℃ and reacted for 24 h. And finally, after the reaction is finished, respectively washing the reaction product with deionized water and absolute ethyl alcohol for three times, centrifuging the reaction product, removing supernate, and drying the supernate in vacuum for 10 hours at 80 ℃ to obtain MoS2/MXene/TiO2A composite nanomaterial.
(3)MoS2/MXene/TiO2Preparation of composite photocatalytic coating
0.1g of MoS2/MXene/TiO2The preparation method comprises the following steps of (1) mixing a composite nano material, 0.1g of CuO nano particles (a curing agent, 50-100 nm) and 0.03g of aluminum powder (a filler, the particle size is 200nm), ball-milling for 1h, then measuring 20ml of water-soluble sodium silicate (5g/L and an inorganic adhesive) by a pipette, dropwise adding the mixture into the mixture, and uniformly stirring the mixture in a mortar to prepare spraying slurry; spraying the spraying slurry on the surface of the pretreated glass substrate under the process conditions of spraying speed of 0.5m/s and air pressure of 0.5MPa, then carrying out multistage heat treatment process treatment, firstly carrying out heat treatment at 120 ℃ for 5min, then carrying out heat treatment at 300 ℃ for 15min, finally carrying out heat treatment at 450 ℃ for 40min, cooling to room temperature along with a furnace, then washing in clean water for 5min, and airing to obtain MoS coated on the surface of glass2/MXene/TiO2And (3) a composite photocatalytic coating.
Example 2
A preparation method of MXene composite nanometer material comprises the following steps:
(1) etching of MXene
Mixing 1g of Ti3AlC2Dissolving the powder into 15mL of hydrofluoric acid (HF) solution (the concentration is 35-40%), magnetically stirring for 12h to remove an aluminum layer, washing with deionized water for several times, centrifuging to remove the residual hydrofluoric acid solution, and drying at 80 ℃ overnight to obtain black powder, namely etched MXene. (2) MoS2/MXene/TiO2Preparation of composite nano material (MXene composite nano material)
42mg of etched MXene is weighed and dispersed in 50mL of deionized water, and the mixture is subjected to ultrasonic treatment for 10min and magnetic stirring for 20min by using an ultrasonic cleaning machine to form a uniform and stable solution. Then, 0.88g of sodium molybdate (Na2MoO4 & 2H2O), 0.725g of hydroxylamine chloride, 1.4g of thiourea (CH4NS2) and 0.24g of ammonium fluorotitanate were added to the MXene dispersion in this order, followed by stirring for 1 hour. Then 0.2g of polyethylene glycol is added, stirring is continued for 30min, and then the solution is transferred into a 60mL stainless steel autoclave with a polytetrafluoroethylene lining, and the autoclave is placed in a blast type oven at the temperature of 180 ℃ for 24 h. And finally, after the reaction is finished, respectively washing the reaction product with deionized water and absolute ethyl alcohol for three times, centrifuging the reaction product, removing supernate, and drying the supernate in vacuum for 10 hours at 80 ℃ to obtain MoS2/MXene/TiO2A composite nanomaterial.
(3)MoS2/MXene/TiO2Preparation of composite photocatalytic coating
0.1g of MoS2/MXene/TiO2Composite nanometer material, 0.16g ZnO nanometer particle (curing agent, 50-100 nm), 0.5g Al2O3(the filler has the granularity of 100nm) is ball-milled for 1h, then 20ml of sodium borate solution (15g/L, inorganic binder) is measured by a pipette and added into the mixture drop by drop, and the mixture in a mortar is uniformly stirred to prepare spraying slurry; spraying the spraying slurry on the surface of the pretreated glass substrate under the process conditions of spraying speed of 0.5m/s and air pressure of 0.5MPa, then carrying out multistage heat treatment process treatment, firstly carrying out heat treatment at 80 ℃ for 10min, then carrying out heat treatment at 220 ℃ for 10min, finally carrying out heat treatment at 400 ℃ for 30min, cooling to room temperature along with a furnace, then washing in pure water for 5min, and airing to obtain the carbon nitride/zinc sulfide composite photocatalytic coating coated on the surface of the glass.
Example 3
A preparation method of MXene composite nanometer material comprises the following steps:
(1) etching of MXene
Mixing 1g of Ti3AlC2Dissolving the powder into 15mL of hydrofluoric acid (HF) solution (the concentration is 35-40%), magnetically stirring for 12h to remove an aluminum layer, washing with deionized water for several times, centrifuging to remove the residual hydrofluoric acid solution, and drying at 80 ℃ overnight to obtain black powder, namely etched MXene. (2) MoS2/MXene/TiO2Preparation of composite nano material (MXene composite nano material)
54mg of etched MXene is weighed and dispersed in 50mL of deionized water, and the mixture is subjected to ultrasonic treatment for 10min and magnetic stirring for 20min by using an ultrasonic cleaning machine to form a uniform and stable solution. Then, 0.88g of sodium molybdate (Na2MoO 4. multidot.2H2O), 0.725g of hydroxylamine chloride, 1.4g of thiourea (CH4NS2) and 2.4mL of tetrabutyl titanate were added to the MXene dispersion in this order, and the mixture was stirred for 1 hour. Then 0.18g of polyvinylpyrrolidone (PVP) is added, stirring is continued for 30min, then the solution is transferred into a 60mL stainless steel autoclave with a polytetrafluoroethylene lining, the autoclave is placed in a blast type oven at 180 ℃, and the reaction time is 24h. And finally, after the reaction is finished, respectively washing the reaction product with deionized water and absolute ethyl alcohol for three times, centrifuging the reaction product, removing supernate, and drying the supernate in vacuum for 10 hours at 80 ℃ to obtain MoS2/MXene/TiO2A composite nanomaterial.
(3)MoS2/MXene/TiO2Preparation of composite photocatalytic coating
0.1g of MoS2/MXene/TiO2Composite nano material, 0.04g MgO nano particles (curing agent, 50-100 nm), 0.01g SiO2Ball milling for 1h (filler, granularity of 100nm), then adding 20ml of aluminum dihydrogen phosphate solution (1.25g/L, inorganic adhesive) measured by a pipette into the mixture drop by drop, and uniformly stirring the mixture in a mortar to prepare spraying slurry; spraying the spraying slurry on the surface of the pretreated glass substrate under the process conditions of spraying speed of 0.5m/s and air pressure of 0.5MPa, then carrying out multistage heat treatment process treatment, firstly carrying out heat treatment at 80 ℃ for 10min, then carrying out heat treatment at 220 ℃ for 10min, finally carrying out heat treatment at 400 ℃ for 30min, cooling to room temperature along with a furnace, then washing in clean water for 5min, and airing to obtain MoS coated on the surface of glass2/MXene/TiO2And (3) a composite photocatalytic coating.
Example 4 test analysis
(1) Microscopic morphology test analysis
FIG. 1 shows MoS obtained in examples 1 to 32/MXene/TiO2XRD pattern of composite nanomaterial. As can be seen, MXene (Ti)3AlC2) The sample has characteristic peaks at 18.02 degrees, 27.46 degrees, 36.02 degrees, 41.82 degrees and 60.64 degrees, and the characteristic peaks respectively correspond to diffraction peaks of MXene on (004), (006), (101), (105) and (110) crystal planes. Pure TiO2The diffraction peaks of the sample at 25.38 degrees, 37.8 degrees and 48.08 degrees respectively correspond to the (101), (004) and (200) crystal planes of the titanium dioxide. MoS2The XRD spectrum of the sample has characteristic peaks at the positions of 17.26 degrees, 32.46 degrees and 57.9 degrees, which respectively correspond to MoS2Diffraction peaks of (002), (100) and (110) crystal planes of (A). Three-phase MoS2/MXene/TiO2MXene and TiO can be observed in the XRD pattern2And MoS2The characteristic peaks of (A) indicate MXene and TiO2And MoS2A complex is formed during the hydrothermal process.
FIGS. 2a and 2b show MoS obtained in examples 1 to 32/MXene/TiO2Scanning Electron Microscopy (SEM) images of the composite nanomaterials, and fig. 2c is a Transmission Electron Microscopy (TEM) image thereof. FIG. 2a clearly shows the characteristic "organ" structure of MXene with multi-layer morphology, illustrating MAX (Ti)3AlC2) Under the stripping of hydrofluoric acid, interlayer aluminum atoms are removed, and the formed loose regular-shaped layered structure shows a typical MXene morphology. The flower-like MoS can be seen very visually in FIG. 2b2The nano-sheet is loaded on the MXene sheet layer, and the characteristic sheet layer morphology of MXene is kept, which shows that the molybdenum disulfide nano-sheet is more uniformly loaded on each single sheet layer of MXene. While TiO is clearly visible in FIG. 2c2The nano particles grow on MXene/TiO2The surface of the sheet layer.
(2) Photocatalytic performance test analysis
In order to examine the actual effect of the photocatalytic coating on degrading organic matters in the wastewater, the invention adopts an Shimadzu ultraviolet-visible spectrophotometer (UV2550) to measure the content of organic dye or antibiotic in the wastewater, specifically, an organic dye solution with a certain concentration is prepared, and then MoS prepared in the invention examples 1-3 is added2/MXene/TiO2The composite photocatalytic coating material is placed in wastewater, the pH value is 7, the magnetic stirring speed is 200r/min, an ultraviolet-visible spectrophotometer is adopted to test the degradation efficiency of the photocatalytic material under the visible light condition, the maximum absorption value is recorded every 15min, so that the photocatalytic degradation efficiency of the composite photocatalytic coating can be calculated, and the organic matter solubility is 10 ppm. Specific data are shown in tables 1 and 2:
TABLE 1 MoS2/MXene/TiO2Degradation rate (%) -of composite photocatalytic coating for photocatalytic degradation of rhodamine B
TABLE 2 MoS2/MXene/TiO2Degradation rate (%, illumination time 1h) of composite photocatalytic coating photocatalytic degradation of methyl orange, phenol and tetracycline
As can be seen from Table 1, the MoS of the present invention2/MXene/TiO2The degradation rate of the composite photocatalytic coating to rhodamine B in wastewater can reach more than 90 percent within 45 minutes; and the degradation rates of methyl orange, phenol and tetracycline in 1 hour are respectively over 90%, 80% and 70%.
Claims (10)
1. The MXene composite nanometer material is characterized by comprising the following components in percentage by mass: 5-15% MoS23 to 10 percent of MXene and the balance of TiO2。
2. The MXene composite nanomaterial of claim 1, wherein the MXene is in the shape of nanosheet with a thickness of 200-500nm, MoS2Is 20-50nm thick and is TiO2The particle size of (A) is 10-20 nm.
3. A method for preparing the MXene composite nanomaterial of claim 1 or 2, comprising the steps of:
(1) etching of MXene
Mixing Ti3AlC2Dissolving the aluminum alloy into a hydrofluoric acid solution with the concentration of 35-40%, magnetically stirring for 10-15 hours to remove an aluminum layer, washing with water, centrifuging to remove the residual hydrofluoric acid solution, and drying at 70-90 ℃ overnight to obtain etched MXene;
(2)MoS2/MXene/TiO2preparation of composite nano material
Weighing etched MXene, dispersing in water, performing ultrasonic treatment for more than 5min, performing magnetic stirring for 10-60min to form MXene dispersion liquid, sequentially adding soluble molybdenum salt, hydroxylamine chloride, thiourea and a titanium source into the MXene dispersion liquid, stirring for more than 10min, adding a surfactant, continuously stirring for more than 20min, reacting for 16-32 h at 170-200 ℃, alternately washing with water and absolute ethyl alcohol to be clean, centrifuging, removing a supernatant, and performing vacuum drying at 70-90 ℃ for more than 5h to obtain MoS2/MXene/TiO2Composite nanomaterial, namely the MXene composite nanomaterial; the mass ratios, namely the concentrations, of the etched MXene, the soluble molybdenum salt, the hydroxylamine chloride, the thiourea, the titanium source and the surfactant relative to water are respectively 0.5-1.2 g/L, 15-20 g/L, 10-20 g/L, 25-35 g/L, 4-50 g/L and 3-5 g/L.
4. The method of claim 3, wherein the soluble molybdenum salt is sodium molybdate or ammonium molybdate.
5. The method of claim 3, wherein the titanium source is tetrabutyl titanate or ammonium fluorotitanate.
6. The method for preparing MXene composite nanomaterial according to claim 3, wherein the surfactant is cetyltrimethylammonium bromide, polyethylene glycol or polyvinylpyrrolidone.
7. An MXene composite nanomaterial as defined in claim 1 or 2 applied to a photocatalytic coating.
8. A method according to claim 7, characterized in that it comprises the following steps: mixing MoS2/MXene/TiO2Mixing the composite nano material with a nano metal oxide curing agent and a nano filler, ball-milling for 0.5-5 h, then dropwise adding an inorganic adhesive with the concentration of 1.25-15 g/L, and uniformly mixing to prepare a spraying slurry; spraying the spraying slurry on the surface of the pretreated base material under the process conditions that the spraying speed is 0.3-1.0 m/s and the air pressure is 0.3-1.0 MPa, then preserving heat at 80-120 ℃ for 5-10 min, then preserving heat at 220-300 ℃ for 10-15 min, finally preserving heat at 400-450 ℃ for 30-40 min, cooling to room temperature along with a furnace, then washing with clean water until the temperature is clean, and airing to obtain MoS coated on the surface of the base material2/MXene/TiO2A composite photocatalytic coating; the MoS2/MXene/TiO2A composite nano material,The mass ratio of the nano metal oxide curing agent to the nano filler to the inorganic adhesive is 1: 0.4-1.6: 0.1-5: 0.25-3; the inorganic adhesive is silicate solution, borate solution or phosphate solution; the nano filler is aluminum powder and Al with the granularity of 100-200 nm2O3Powder or SiO2Pulverizing; the substrate is a glass, ceramic or metal material.
9. The method of claim 8, wherein the nano metal oxide curing agent is CuO nanoparticles, ZnO nanoparticles or MgO nanoparticles having a particle size of 50 to 100 nm; the inorganic adhesive is water-soluble sodium silicate solution, sodium borate solution or aluminum dihydrogen phosphate solution.
10. Method for the application according to claim 8, characterized in that said MoS is applied2/MXene/TiO2The composite photocatalytic coating is used for photocatalytic degradation of organic matters in wastewater, and is illuminated for 0.5-1h under the condition of visible light; the organic matter is rhodamine B, methyl orange, phenol or tetracycline.
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