CN112871185B - SnO applied to sewage treatment 2 -MoS 2 Modified graphene aerogel and preparation method thereof - Google Patents
SnO applied to sewage treatment 2 -MoS 2 Modified graphene aerogel and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000004964 aerogel Substances 0.000 title claims abstract description 30
- 239000010865 sewage Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims description 7
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 40
- 239000002057 nanoflower Substances 0.000 claims abstract description 38
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920000962 poly(amidoamine) Polymers 0.000 claims abstract description 25
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 20
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 20
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 19
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 19
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 19
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001119 stannous chloride Substances 0.000 claims abstract description 19
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 19
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 19
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001257 hydrogen Chemical group 0.000 claims abstract description 5
- 229910052739 hydrogen Chemical group 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 239000002904 solvent Substances 0.000 claims description 54
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 51
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 45
- 239000008367 deionised water Substances 0.000 claims description 39
- 229910021641 deionized water Inorganic materials 0.000 claims description 39
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 15
- 229910001887 tin oxide Inorganic materials 0.000 claims description 15
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 14
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 230000004048 modification Effects 0.000 claims description 10
- 238000012986 modification Methods 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 238000005576 amination reaction Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 229910006404 SnO 2 Inorganic materials 0.000 abstract description 22
- 239000000975 dye Substances 0.000 abstract description 11
- 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 abstract description 9
- 229940012189 methyl orange Drugs 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 4
- 125000003277 amino group Chemical group 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 230000031700 light absorption Effects 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 abstract 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- -1 and at present Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 125000001153 fluoro group Chemical class F* 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- B01J27/02—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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/063—Polymers comprising a characteristic microstructure
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
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- B01J35/23—
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- B01J35/39—
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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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
-
- 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
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
-
- 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
-
- 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
Abstract
The invention relates to the technical field of water treatment and discloses SnO applied to sewage treatment 2 ‑MoS 2 Modified graphene aerogel is prepared by taking graphene, diethylenetriamine, N-methylene bisacrylamide, stannous chloride, sodium fluoride, thioacetamide and sodium molybdate as raw materials to obtain hyperbranched polyamidoamine functionalized graphene loaded MoS 2 Hollow sphere modified F-doped SnO 2 The nanoflower and hyperbranched polyamidoamine functionalized graphene has ultrahigh specific surface area, abundant amino groups and hydrogen bonds and a large number of cavity structures, is favorable for adsorbing more organic dyes such as methyl orange and the like, and promotes SnO by F doping 2 Red shift of absorption band edge, broadening light absorption range, moS 2 With SnO 2 The organic dye such as methyl orange and the like can be oxidized into small molecular substances by the superoxide anion and the hydroxyl radical with strong oxidizing property.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to SnO applied to sewage treatment 2 -MoS 2 Modified graphene aerogel and a preparation method thereof.
Background
At present, the variety of dyes all over 10 thousands of the world, the yield exceeds 700 million tons every year, and the production is still increasing, in the process of producing the dyes, the loss of the dyes and the discharge of printing and dyeing wastewater are often accompanied with the outflow of partial dyes, and in the process of printing and dyeing, the loss of the dyes and the discharge of printing and dyeing wastewater are also caused, so that serious environmental pollution is caused, especially, acid azo dyes such as methyl orange and the like which have stable chemical structure, strong oxidation resistance and toxicity and are difficult to degrade are directly discharged without being treated, so that an ecological system is seriously damaged, and further, the health of human beings is damaged.
The efficiency of the photocatalytic degradation method mainly depends on the selection of a photocatalyst, and at present, semiconductor photocatalytic materials such as ZnO and TiO are used 2 、WO 3 、SnO 2 The like have excellent photocatalytic performance and are widely applied to the fields of photocatalytic hydrogen production and degradation, wherein n-type semiconductor SnO 2 The material has the advantages of wide forbidden band width, low toxicity, high chemical stability, low cost, excellent photocatalytic activity and the like, is widely applied to the fields of gas sensing, lithium ion batteries, photocatalysis and the like, but has the advantages of easy recombination of photo-generated electrons and holes, low sunlight utilization rate, great restriction on the application range, modification treatment on the material is needed, and element doping can improve SnO 2 Overall performance of, and p-type semiconductor MoS 2 Has narrower forbidden bandwidth, better conductivity and excellent electrochemical and optical properties, is widely applied to the fields of lithium ion batteries, photocatalysis and the like, and is SnO 2 Compounding to obviously improve SnO 2 The graphene has the advantages of large specific surface area, good conductivity and the like, is widely applied to the fields of lithium ion batteries, photocatalysis, adsorption and the like, and can further improve the adsorption performance of the graphene on organic dyes such as methyl orange and the like through chemical modification.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides SnO applied to sewage treatment 2 -MoS 2 The modified graphene aerogel and the preparation method thereof solve the problem of SnO 2 The photo-generated electrons and holes of the photocatalyst are easy to recombine, the sunlight utilization rate is low, and the adsorption performance is poor.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: snO applied to sewage treatment 2 -MoS 2 Modified graphene aerogel, snO applied to sewage treatment 2 -MoS 2 The preparation method of the modified graphene aerogel comprises the following steps:
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, performing uniform ultrasonic dispersion, performing reaction, removing the solvent by rotary evaporation, washing with acetone, and drying to obtain hyperbranched polyamidoamine functionalized graphene;
(3) Adding a deionized water solvent and sodium hydroxide into a three-mouth bottle, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while performing ultrasonic treatment, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, uniformly dispersing by ultrasonic treatment, placing the mixture into a reaction kettle, performing hydrothermal reaction, cooling to room temperature, performing centrifugal separation, washing with deionized water and absolute ethyl alcohol, and drying to obtain fluorine-doped stannic oxide nanoflowers;
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped tin oxide nanoflower into a three-necked bottle, performing ultrasonic dispersion uniformly, performing hydrolysis reaction, adding ethanol to promote dispersion, precipitating a product by using dilute hydrochloric acid, performing centrifugal separation, washing the product by using deionized water, drying the product, putting the dried product into a tubular furnace, calcining the product, and cooling the product to room temperature to obtain molybdenum disulfide hollow sphere modified fluorine-doped tin oxide nanoflower;
(5) Adding a deionized water solvent, molybdenum disulfide hollow spheres for modifying fluorine-doped tin oxide nanoflowers and hyperbranched polyamidoamine functionalized graphene into a three-necked bottle, uniformly dispersing by ultrasonic waves, placing the three-necked bottle in a reaction kettle, carrying out hydrothermal reaction, and carrying out freeze drying to obtain the fluorine-doped tin oxide nanoflowers and the hyperbranched polyamidoamine functionalized grapheneSnO applied to sewage treatment 2 -MoS 2 Modifying the graphene aerogel.
Preferably, in the step (2), the mass ratio of diethylenetriamine to N, N-methylene bisacrylamide to aminated graphene is 10-20.
Preferably, the reaction condition in the step (2) is reflux reaction at 45-60 ℃ for 6-9h.
Preferably, in the step (3), the mass ratio of the sodium hydroxide, the stannous chloride, the sodium fluoride and the hexadecyl trimethyl ammonium bromide is 60-120.
Preferably, the hydrothermal reaction condition in the step (3) is hydrothermal reaction at 140-200 ℃ for 24-32h.
Preferably, the mass ratio of thioacetamide, sodium molybdate and fluorine-doped stannic oxide nanoflower in the step (4) is 40-70.
Preferably, the hydrolysis reaction in the step (4) is carried out at 85-100 ℃ for 6-12min.
Preferably, the calcination in step (4) is performed under the condition of 700-800 ℃ in a hydrogen atmosphere for 0.5-2h.
Preferably, the mass ratio of the molybdenum disulfide hollow sphere modified fluorine doped stannic oxide nanoflower to the hyperbranched polyamidoamine functionalized graphene in the step (5) is 3-6.
Preferably, the hydrothermal reaction condition in the step (5) is hydrothermal reaction at 160-200 ℃ for 8-15h.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
SnO applied to sewage treatment 2 -MoS 2 The modified graphene aerogel takes aminated graphene as a central point, amino and imino on aminated graphene and diethylenetriamine and double bonds on N, N-methylene-bisacrylamide undergo a Michelal addition reaction to obtain hyperbranched polyamidoamine functionalized graphene, and Sn is reacted in an alkaline environment 2+ Rapid hydrolysis to Sn (OH) 2 And further oxidized to form Sn (OH) 4 Further with OH - Reaction to form Sn (OH) 6 2- Hydrothermal reaction to produce SnO 2 Nanocrystalline is coagulated and nucleated, and further directionally grows to form SnO along the direction of acting force with reduced surface energy under the action of cetyl trimethyl ammonium bromide serving as a surfactant 2 Further, the nanosheets grow randomly in other directions to form SnO 2 Nanometer flower and sodium fluoride as doping source to obtain F-doped SnO 2 Nano flower, snO 2 The unique nano flower-shaped morphology has an ultra-high specific surface area, is favorable for exposing photocatalytic degradation active sites, and takes the nano flower-shaped morphology as a substrate to accelerate the hydrolysis of thioacetamide with hydrochloric acid and high temperature to generate H 2 S, further reacting with sodium molybdate to dope SnO with F 2 In-situ growth of MoS on nanoflower x Seed crystals further in MoS x Precipitation of MoS on seed crystals x Generating MoS x Spherical nanoparticles, calcined, moS x Generating MoS 2 And H 2 Obtaining MoS 2 Hollow sphere modified F-doped SnO 2 Nanoflower, moS 2 The special hollow spherical shape has super-high specific surface area, is beneficial to exposing more photocatalytic degradation active sites, and further takes hyperbranched polyamidoamine functionalized graphene as a carrier and MoS 2 Hollow sphere modified F-doped SnO 2 The nano flower is used as an active substance to obtain SnO applied to sewage treatment 2 -MoS 2 Modifying the graphene aerogel.
SnO applied to sewage treatment 2 -MoS 2 The hyperbranched polyamidoamine functionalized graphene has an ultrahigh specific surface area, is beneficial to exposing more adsorption active sites, contains abundant amino groups and hydrogen bonds in the molecular structure of hyperbranched polyamidoamine, further exposes more adsorption active sites, and simultaneously protonates abundant amino groups in a weak acid environment, so that the hyperbranched polyamidoamine has more positive charges, increases the electrostatic attraction with organic dyes such as methyl orange with negative charges, and the hyperbranched polyamidoamine has excellent hydrophilicity, and forms a large number of cavity structures in the process of forming the hyperbranched polyamidoamine by a Michelal addition reaction, and has a synergistic effect with the grapheneIs beneficial to adsorbing more organic dyes such as methyl orange and the like.
SnO applied to sewage treatment 2 -MoS 2 Modifying graphene aerogel, and doping F atoms into SnO 2 In the crystal lattice of (2), promoting SnO 2 The nanocrystals are grown so that SnO 2 Further increase the specific surface area of the catalyst and simultaneously make SnO 2 The absorption band edge red shift widens SnO 2 Absorption of light in the range of SnO 2 Utilization ratio of sunlight, p-type semiconductor MoS 2 With n-type semiconductors SnO 2 Forming a p-n heterojunction structure such that MoS 2 And SnO 2 The Fermi energy levels of the contact surfaces are the same, so that energy bands near the contact surfaces are dislocated to form an internal electric field, and under the action of the internal electric field, photoproduction electrons and holes are promoted to pass through the contact surfaces to be separated, so that SnO is enabled 2 Hole transfer to MoS in the valence band 2 On the price band, and MoS 2 Transfer of photo-generated electrons on conduction band from SnO 2 The separation of photo-generated electrons and holes is promoted on the conduction band, the photo-generated electrons react with oxygen to generate superoxide anions, the holes react with water to generate hydroxyl radicals, and the superoxide anions and the hydroxyl radicals with strong oxidizing property can oxidize organic dyes such as methyl orange and the like into small molecular substances.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: snO applied to sewage treatment 2 -MoS 2 Modified graphene aerogel applied to SnO of sewage treatment 2 -MoS 2 The preparation method of the modified graphene aerogel comprises the following steps:
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, wherein the mass ratio of the methanol solvent to the diethylenetriamine to the N, N-methylene bisacrylamide to the aminated graphene is 10-20;
(3) Adding a deionized water solvent and sodium hydroxide into a three-mouth bottle, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while performing ultrasonic treatment, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, wherein the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide is (60-100);
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped stannic oxide nanoflower into a three-neck flask, wherein the mass ratio of the deionized water solvent to the thioacetamide to the sodium molybdate to the fluorine-doped stannic oxide nanoflower is 40-70;
(5) Adding a deionized water solvent, molybdenum disulfide hollow spheres modified fluorine-doped tin oxide nanoflowers and hyperbranched polyamidoamine functionalized graphene into a three-mouth bottle, wherein the mass ratio of the two is 3-6, the two is uniformly dispersed by ultrasonic, placing the three-mouth bottle into a reaction kettle, carrying out hydrothermal reaction at 160-200 ℃ for 8-15h, and carrying out freeze drying to obtain SnO applied to sewage treatment 2 -MoS 2 Modifying the graphene aerogel.
Example 1
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, wherein the mass ratio of the methanol solvent to the diethylenetriamine to the N, N-methylene bisacrylamide to the aminated graphene is 10;
(3) Adding a deionized water solvent and sodium hydroxide into a three-neck flask, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while ultrasonically treating, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, wherein the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide is 60;
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped tin oxide nanoflower into a three-neck flask, wherein the mass ratio of the deionized water solvent to the thioacetamide to the sodium molybdate to the fluorine-doped tin oxide nanoflower is 40;
(5) Adding a deionized water solvent, molybdenum disulfide hollow spheres to modify fluorine-doped tin oxide nanoflowers and hyperbranched polyamidoamine functionalized graphene into a three-mouth bottle, wherein the mass ratio of the two is 3 2 -MoS 2 Modifying the graphene aerogel.
Example 2
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, wherein the mass ratio of the three is 13.5;
(3) Adding a deionized water solvent and sodium hydroxide into a three-mouth bottle, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while ultrasonically treating, adding sodium fluoride and a surfactant, namely cetyl trimethyl ammonium bromide, wherein the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide is (80);
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped tin oxide nanoflower into a three-necked bottle, wherein the mass ratio of the deionized water solvent to the thioacetamide to the sodium molybdate to the fluorine-doped tin oxide nanoflower is 50;
(5) Adding a deionized water solvent, molybdenum disulfide hollow sphere modified fluorine-doped stannic oxide nanoflower and hyperbranched polyamidoamine functionalized graphene into a three-necked flask, wherein the mass ratio of the two is 4 2 -MoS 2 Modifying the graphene aerogel.
Example 3
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, wherein the mass ratio of the methanol solvent to the diethylenetriamine to the N, N-methylene bisacrylamide to the aminated graphene is 17;
(3) Adding a deionized water solvent and sodium hydroxide into a three-mouth bottle, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while ultrasonically treating, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, wherein the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide is (100);
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped tin oxide nanoflower into a three-neck flask, wherein the mass ratio of the deionized water solvent to the thioacetamide to the sodium molybdate to the fluorine-doped tin oxide nanoflower is 60;
(5) Adding a deionized water solvent, molybdenum disulfide hollow sphere modified fluorine-doped stannic oxide nanoflower and hyperbranched polyamidoamine functionalized graphene into a three-neck flask, wherein the mass ratio of the two is 5 2 -MoS 2 Modifying the graphene aerogel.
Example 4
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, wherein the mass ratio of the methanol solvent to the diethylenetriamine to the N, N-methylene bisacrylamide to the aminated graphene is 20;
(3) Adding a deionized water solvent and sodium hydroxide into a three-neck flask, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while ultrasonically treating, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, wherein the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide is (120);
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped stannic oxide nanoflower into a three-neck flask, wherein the mass ratio of the deionized water solvent to the thioacetamide to the sodium molybdate to the fluorine-doped stannic oxide nanoflower is 70;
(5) Adding a deionized water solvent, molybdenum disulfide hollow spheres modified fluorine-doped stannic oxide nanoflower and hyperbranched polyamidoamine functionalized graphene into a three-necked bottle, wherein the mass ratio of the deionized water solvent to the molybdenum disulfide hollow spheres modified fluorine-doped stannic oxide nanoflower to the hyperbranched polyamidoamine functionalized graphene is 6 2 -MoS 2 Modifying the graphene aerogel.
Comparative example 1
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, wherein the mass ratio of the methanol solvent to the diethylenetriamine to the N, N-methylene bisacrylamide to the aminated graphene is 8;
(3) Adding a deionized water solvent and sodium hydroxide into a three-neck flask, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while ultrasonically treating, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, wherein the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide is 48;
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped tin oxide nanoflower into a three-neck flask, wherein the mass ratio of the deionized water solvent to the thioacetamide to the sodium molybdate to the fluorine-doped tin oxide nanoflower is 32;
(5) Adding a deionized water solvent, molybdenum disulfide hollow spheres modified fluorine-doped stannic oxide nanoflowers and hyperbranched polyamidoamine functionalized graphene into a three-necked flask, wherein the mass ratio of the deionized water solvent to the molybdenum disulfide hollow spheres modified fluorine-doped stannic oxide nanoflowers to the hyperbranched polyamidoamine functionalized graphene is 2.4, dispersing the mixture uniformly by ultrasonic, placing the mixture into a reaction kettle, carrying out hydrothermal reaction for 8 hours at 160 ℃, and carrying out freeze drying to obtain SnO applied to sewage treatment 2 -MoS 2 Modifying the graphene aerogel.
Comparative example 2
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding methanol solvent, diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a three-necked bottle, wherein the mass ratio of the methanol solvent to the diethylenetriamine to the N, N-methylene bisacrylamide to the aminated graphene is 24;
(3) Adding a deionized water solvent and sodium hydroxide into a three-neck flask, uniformly dispersing by ultrasonic treatment, dropwise adding a stannous chloride aqueous solution while ultrasonically treating, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, wherein the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide is 144;
(4) Adding a deionized water solvent, thioacetamide, sodium molybdate and fluorine-doped stannic oxide nanoflower into a three-neck flask, wherein the mass ratio of the deionized water solvent to the thioacetamide to the sodium molybdate to the fluorine-doped stannic oxide nanoflower is 84;
(5) Adding a deionized water solvent, molybdenum disulfide hollow spheres modified fluorine-doped stannic oxide nanoflowers and hyperbranched polyamidoamine functionalized graphene into a three-necked bottle, wherein the mass ratio of the deionized water solvent to the molybdenum disulfide hollow spheres modified fluorine-doped stannic oxide nanoflowers to the hyperbranched polyamidoamine functionalized graphene is 7.2, dispersing the mixture uniformly by ultrasonic, placing the mixture into a reaction kettle, carrying out hydrothermal reaction for 15 hours at 200 ℃, and carrying out freeze drying to obtain SnO applied to sewage treatment 2 -MoS 2 Modifying the graphene aerogel.
10mg of SnO applied to sewage treatment and obtained in example and comparative example and applied to sewage treatment were added to 50mL of methyl orange solution with a mass concentration of 20mg/L 2 -MoS 2 Modifying the graphene aerogel, uniformly dispersing, adjusting the pH value of the solution to 6, stirring for 90min at 25 ℃, centrifuging to remove solids to obtain a degraded solution, measuring the concentration of methyl orange in the solution by using an L5 type ultraviolet-visible spectrophotometer, and calculating the adsorption rate.
10mg of SnO applied to sewage treatment and obtained in example and comparative example and applied to sewage treatment were added to 50mL of methyl orange solution with a mass concentration of 20mg/L 2 -MoS 2 Modifying the graphene aerogel, uniformly dispersing, adjusting the pH value of the solution to 6, irradiating for 90min by using a 500W xenon lamp, centrifuging to remove solids to obtain a degraded solution, measuring the concentration of methyl orange in the solution by using an L5 type ultraviolet-visible spectrophotometer, and calculating the degradation rate.
Claims (6)
1. SnO applied to sewage treatment 2 -MoS 2 Modified graphiteOlefinic aerogel, characterized in that: snO applied to sewage treatment 2 -MoS 2 The preparation method of the modified graphene aerogel comprises the following steps:
(1) Carrying out amination modification on graphene by using diethylenetriamine to obtain aminated graphene;
(2) Adding diethylenetriamine, N-methylene bisacrylamide and aminated graphene into a methanol solvent according to the mass ratio of 10-20 to 15-30, performing ultrasonic dispersion uniformly, reacting, removing the solvent by rotary evaporation, washing and drying to obtain hyperbranched polyamidoamine functionalized graphene;
(3) Adding sodium hydroxide into a deionized water solvent, uniformly dispersing by ultrasonic, dropwise adding a stannous chloride aqueous solution while performing ultrasonic treatment, adding sodium fluoride and a surfactant cetyl trimethyl ammonium bromide, controlling the mass ratio of the sodium hydroxide to the stannous chloride to the sodium fluoride to the cetyl trimethyl ammonium bromide to be 60-120-1.5;
(4) Adding thioacetamide, sodium molybdate and fluorine-doped tin oxide nanoflower into a deionized water solvent according to the mass ratio of 40-70;
(5) Adding molybdenum disulfide hollow spheres with the mass ratio of 3-6 to modify fluorine-doped stannic oxide nanoflower and hyperbranched polyamidoamine functionalized graphene into a deionized water solvent, uniformly dispersing by ultrasonic waves, placing the mixture into a reaction kettle, carrying out hydrothermal reaction, and carrying out freeze drying to obtain SnO applied to sewage treatment 2 -MoS 2 Modifying the graphene aerogel.
2. SnO applied to sewage treatment according to claim 1 2 -MoS 2 Modified graphene aerogel is characterized in that: the reaction conditions in the step (2) are thatReflux reaction is carried out for 6 to 9 hours at the temperature of 45 to 60 ℃.
3. A SnO applied to sewage treatment according to claim 1 2 -MoS 2 Modified graphene aerogel, its characterized in that: the hydrothermal reaction condition in the step (3) is that the hydrothermal reaction is carried out for 24-32h at 140-200 ℃.
4. SnO applied to sewage treatment according to claim 1 2 -MoS 2 Modified graphene aerogel, its characterized in that: the hydrolysis reaction in the step (4) is carried out for 6-12min at 85-100 ℃.
5. SnO applied to sewage treatment according to claim 1 2 -MoS 2 Modified graphene aerogel, its characterized in that: the calcining condition in the step (4) is calcining for 0.5-2h at 700-800 ℃ in a hydrogen atmosphere.
6. A SnO applied to sewage treatment according to claim 1 2 -MoS 2 Modified graphene aerogel, its characterized in that: the hydrothermal reaction condition in the step (5) is that the hydrothermal reaction is carried out for 8-15h at 160-200 ℃.
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