CN109603810A - Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and its preparation method and application - Google Patents
Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and its preparation method and application Download PDFInfo
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- CN109603810A CN109603810A CN201811619833.0A CN201811619833A CN109603810A CN 109603810 A CN109603810 A CN 109603810A CN 201811619833 A CN201811619833 A CN 201811619833A CN 109603810 A CN109603810 A CN 109603810A
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- porous graphite
- molybdenum disulfide
- disulfide nano
- nano sheet
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 146
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 91
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 87
- 239000010439 graphite Substances 0.000 title claims abstract description 87
- 239000002135 nanosheet Substances 0.000 title claims abstract description 67
- 206010054949 Metaplasia Diseases 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 230000015689 metaplastic ossification Effects 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 title claims description 58
- 230000003115 biocidal effect Effects 0.000 claims abstract description 39
- 239000003610 charcoal Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 14
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 230000001699 photocatalysis Effects 0.000 claims abstract description 8
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims abstract description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 6
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000003763 carbonization Methods 0.000 claims description 13
- 238000000197 pyrolysis Methods 0.000 claims description 13
- 239000002154 agricultural waste Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- KIPLYOUQVMMOHB-MXWBXKMOSA-L [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O Chemical compound [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O KIPLYOUQVMMOHB-MXWBXKMOSA-L 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 229960001180 norfloxacin Drugs 0.000 claims description 5
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- 229960005404 sulfamethoxazole Drugs 0.000 claims description 5
- 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 description 5
- 229940063650 terramycin Drugs 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- GSDSWSVVBLHKDQ-UHFFFAOYSA-N 9-fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)COC3=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 229960001699 ofloxacin Drugs 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000004677 hydrates Chemical class 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 239000007789 gas Substances 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000002296 pyrolytic carbon Substances 0.000 claims 1
- 235000015393 sodium molybdate Nutrition 0.000 claims 1
- 239000011684 sodium molybdate Substances 0.000 claims 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims 1
- 239000010902 straw Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 8
- 230000006798 recombination Effects 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 150000001721 carbon Chemical class 0.000 abstract description 2
- 231100000614 poison Toxicity 0.000 abstract 1
- 230000007096 poisonous effect Effects 0.000 abstract 1
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 description 11
- 239000000243 solution Substances 0.000 description 9
- 239000003344 environmental pollutant Substances 0.000 description 4
- 238000005087 graphitization Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000446313 Lamella Species 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- UIOFUWFRIANQPC-JKIFEVAISA-N Floxacillin Chemical compound N([C@@H]1C(N2[C@H](C(C)(C)S[C@@H]21)C(O)=O)=O)C(=O)C1=C(C)ON=C1C1=C(F)C=CC=C1Cl UIOFUWFRIANQPC-JKIFEVAISA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000019771 cognition Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 229960004273 floxacillin Drugs 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- -1 molybdic acid hydrates Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000002023 wood Substances 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
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—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
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composites and its preparation method and application, and for the composite material using porous graphite charcoal as carrier, surface inserting has molybdenum disulfide nano sheet.Preparation method includes: to prepare porous graphite charcoal powder；In water by porous graphite charcoal powder ultrasonic disperse, two molybdic acid hydrate sodium are added and thioacetamide carries out hydro-thermal reaction, is centrifuged, washs, it is dry, obtain composite material of the present invention.Composite material of the present invention has many advantages, such as that large specific surface area, good conductivity, photo-generate electron-hole are low to recombination rate, photocatalytic activity is high, universality is high, preparation method has the advantages that simple process, easy to operate, low in cost, it is environmentally friendly, do not generate poisonous and harmful by-product, it is suitable for large scale preparation, meets the demand of actual production.Composite material of the present invention can fast and efficiently in processing environment antibiotic, there is good application value and application prospect.
Description
Technical field
The invention belongs to materials science fields, are related to a kind of molybdenum disulfide nano sheet/porous graphite charcoal composite wood
Material and its preparation method and application.
Background technique
In recent years, abuse of antibiotics has become universal phenomenon, and thus caused environment, ecological problem are also more and more.
With a large amount of uses of antibiotic, the antibiotic that part is not metabolized can be drained directly through animal hence into extraneous ring
Border is chronically exposed to the biology in environment in antibiotic, therefore may generate harm to microorganism in environment such as causes resistance
The generation of bacterium.The intracorporal drug tolerant bacteria of host can make drug accelerate degradation, weaken the bacteriostasis of drug, reduce drug effect.
Antibiotic is used as " novel environmental pollutant ", has in vivo with the characteristic that remains and accumulate in environment, it not only can
The healthy living for influencing the mankind, can also cause the destruction of unrepairable to environment.Therefore, deepen to pollute antibiotic in water body existing
The method of the cognition of shape, the science, safety of exploring processing antibiotic pollution is the hot spot of domestic and foreign scholars' Recent study.
Photocatalysis oxidation technique is increasingly becoming people from all walks of life due to its cheap, energy saving, nontoxic, efficient, easy-operating advantage
The emphasis of research.As typical transient metal sulfide, molybdenum disulfide has class graphene layer structure, good optical
Energy and electron transport property, are a kind of light absorption semiconductor materials to merit attention.It has the band gap of 1.8eV, can absorb
The photon excitation of visible frequency generates electron-hole pair, and the edge current potential of its valence band and conduction band is high, is conducive to carrier and joins
With the generation of oxidizing species (oxyradical).But there is photo-generate electron-holes pair for the agent of molybdenum disulfide homogenous catalyst
The problems such as recombination rate is high, electric conductivity is poor, and due to the effect of Van der Waals, molybdenum disulfide nano sheet is easy to reunite.Cause
This, overcomes deficiency present in above-mentioned molybdenum disulfide nano sheet, obtains a kind of large specific surface area, good conductivity, light induced electron-sky
The molybdenum disulfide nano sheet that cave is low to recombination rate, photocatalytic activity is high, universality is high/porous graphite metaplasia object carbon composite,
The pollutant (such as antibiotic) being effectively treated in environment is had a very important significance.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, a kind of large specific surface area, electric conductivity are provided
Good, photo-generate electron-hole is low to recombination rate, photocatalytic activity is high, universality is high molybdenum disulfide nano sheet/porous graphite metaplasia
Object carbon composite, also provide a kind of simple process, it is easy to operate, low in cost the advantages that, can be used for two sulphur of large scale preparation
Change molybdenum nanometer sheet/porous graphite metaplasia object carbon composite method and the molybdenum disulfide nano sheet/porous graphite metaplasia object
Application of the carbon composite in processing antibiotic.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite, the molybdenum disulfide nano sheet/porous stone
For black metaplasia object carbon composite using porous graphite charcoal as carrier, the porous graphite metaplasia object carbon surface is inlaid with two sulphur
Change molybdenum nanometer sheet.
The inventive concept total as one, the present invention also provides a kind of above-mentioned molybdenum disulfide nano sheet/porous graphites
The preparation method of metaplasia object carbon composite, comprising the following steps:
S1, agricultural wastes stalk is immersed in liquor potassic permanganate, it is dry, it obtains giving up immersed with the agricultural of potassium permanganate
Object stalk；
S2, the agricultural wastes stalk obtained in step S1 immersed with potassium permanganate is subjected to pyrolysis carbonization, washed, done
It is dry, it grinds, sieving obtains porous graphite charcoal powder；
S3, by porous graphite charcoal powder ultrasonic disperse obtained in step S2 in water, be added two molybdic acid hydrates
Sodium and thioacetamide carry out hydro-thermal reaction, are centrifuged, and wash, dry, obtain molybdenum disulfide nano sheet/porous graphite charcoal
Composite material.
Above-mentioned preparation method, further improved, the porous graphite charcoal powder and two molybdic acid hydrate sodium
Mass ratio is 0.05~0.15: 1；The molar ratio of the two molybdic acid hydrates sodium and thioacetamide is 1: 5.
Above-mentioned preparation method, further improved, in the step S1, the concentration of the liquor potassic permanganate is
0.5mol/L~1mol/L；The time of the immersion is 12h~for 24 hours；The drying carries out under vacuum conditions.
Above-mentioned preparation method, it is further improved, in the step S2, pyrolysis carbonization in a nitrogen atmosphere into
Row；Heating rate during the pyrolysis carbonization is 5 DEG C/min；The temperature of the pyrolysis carbonization is 700 DEG C~1000 DEG C；Institute
The time for stating pyrolysis carbonization is 1h~3h；The washing for successively using diluted acid and deionized water to the product after pyrolysis carbonization into
Row washing；The concentration of the diluted acid is 0.1mol/L~1mol/L；The diluted acid is dilute hydrochloric acid solution；The drying is in temperature
It is carried out at 60 DEG C；The sieving was 200 meshes.
Above-mentioned preparation method, it is further improved, in the step S3, time of the ultrasonic disperse be 30min~
60min；The temperature of the hydro-thermal reaction is 160 DEG C~200 DEG C；The time of the hydro-thermal reaction is 18h~for 24 hours；The washing
Successively to use dehydrated alcohol and deionized water to wash centrifugation product；The drying carries out at being 60 DEG C in temperature.
As a general technical idea, the present invention also provides a kind of above-mentioned molybdenum disulfide nano sheet/porous graphites
Molybdenum disulfide nano sheet made from metaplasia object carbon composite or above-mentioned preparation method/porous graphite metaplasia object carbon composite
Application in processing antibiotic.
Above-mentioned application, it is further improved, using molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite pair
Antibiotic in water body is handled, comprising the following steps: by molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite
After antibiotic water mixing progress dark reaction, adsorption equilibrium to be achieved, photocatalytic degradation reaction is carried out under illumination condition, it is complete
The processing of antibiotic in pairs of water body.
Above-mentioned application, it is further improved, the molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite with
The mass volume ratio of antibiotic water body is 0.1g~0.5g: 1L.
Above-mentioned application, further improved, antibiotic is quadracycline, terramycin, oxygen in the antibiotic water body
At least one of Flucloxacillin, Norfloxacin and sulfamethoxazole；The concentration of antibiotic is 10mg/L in the antibiotic water body
~50mg/L；The time of the dark reaction is 30min~60min；The time of photocatalytic degradation reaction be 60min~
120min。
Compared with the prior art, the advantages of the present invention are as follows:
(1) the present invention provides a kind of molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composites, with porous graphite
Change charcoal is carrier, and porous graphite metaplasia object carbon surface is inlaid with molybdenum disulfide nano sheet.In the present invention, porous graphite metaplasia
Object charcoal has very big specific surface area and good distribution of pores, has very strong adsorption capacity to pollutant.On this basis,
By the way that molybdenum disulfide nano sheet is embedded in porous graphite metaplasia object carbon surface, on the one hand using porous graphite charcoal as carrier
It can be realized molybdenum disulfide nano sheet to be relatively evenly distributed, molybdenum disulfide nano sheet farthest avoided to occur stacking reunion
Phenomenon；Another aspect porous graphite charcoal can be passed quickly because of the higher and with higher electric conductivity of its degree of graphitization
Electronics is passed, the separation of electron-hole pair is accelerated, improves the utilization rate of carrier, thus molybdenum disulfide nano sheet is uniformly embedded in
Porous graphite metaplasia object carbon surface, electronics can be passed by contact surface in semiconductor material molybdenum disulfide and porous graphite charcoal
Movement is led, to reduce the compound of Pair production, improves photocatalysis efficiency.Molybdenum disulfide nano sheet/porous graphite of the present invention
Metaplasia object carbon composite have large specific surface area, good conductivity, photo-generate electron-hole is low to recombination rate, photocatalytic activity is high,
The advantages that universality is high, pollutant (such as antibiotic) that can fast and efficiently in processing environment have good application value
And application prospect.Molybdenum disulfide nano sheet of the present invention/porous graphite metaplasia object carbon composite is that a kind of pattern is complete, it is good to have
The catalysis material of good photoelectrochemical behaviour has excellent treatment effeciency and stable cyclicity in terms of water pollution processing
Energy.
(2) the present invention also provides a kind of molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite preparation sides
Method prepares porous graphite charcoal using agricultural wastes stalk as carbon matrix precursor, using this porous graphite charcoal as carrier
Molybdenum disulfide nano sheet is uniformly embedded in porous graphite metaplasia object carbon surface by hydrothermal synthesis method, so that pattern be prepared
Completely, the molybdenum disulfide with good photoelectrochemical behaviour/porous graphite metaplasia object carbon composite.In the present invention, institute's selection
Material, reagent are cheap and from a wealth of sources, and wherein stalk contains a large amount of lignin, cellulose as agricultural wastes, more as preparing
Biomass forerunner's physical efficiency of hole graphite charcoal effectively reduces cost, and improves the recycling of farming organic matter；Using potassium ferrate this
One is novel, efficient, the porous and graphitization of carbon material can be achieved at the same time in multifunctional green inorganic agent, can not only simplify material
Preparation step and operation, while can also avoid using high toxicity compound during catalyzed graphitization.Preparation of the invention
Method has the advantages that simple process, easy to operate, low in cost, while the preparation method is environmentally friendly, does not generate and toxic has
Evil by-product, is suitable for large scale preparation, meets the demand of actual production.
(3) molybdenum disulfide nano sheet of the present invention/porous graphite metaplasia object carbon composite can be used for handling antibiotic, pass through
By molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and antibiotic water mixing, pass through dark reaction and photocatalysis
The efficient removal to antibiotic in water body can be realized in degradation reaction.By taking quadracycline as an example, molybdenum disulfide nano of the present invention
Piece/porous graphite metaplasia object carbon composite is up to 91.82% to the removal rate of the quadracycline in water body, can be realized pair
Antibiotic effectively removes, so as to which polluter ecological risk caused by the ecosystem in water body is effectively reduced.
Detailed description of the invention
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, the technical scheme in the embodiment of the invention is clearly and completely described.
Fig. 1 is that molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite obtained is swept in the embodiment of the present invention 1
Retouch electron microscope.
Fig. 2 is saturating for molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite obtained in the embodiment of the present invention 1
Penetrate electron microscope.
Fig. 3 is molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite photocatalytic degradation in the embodiment of the present invention 2
The efficiency chart of quadracycline.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
It limits the scope of the invention.
In following present invention embodiment, unless otherwise noted, used material and instrument are commercially available, used technique
For common process, used equipment is conventional equipment, and the data obtained is the average value for repeating experiment more than three times.
Embodiment 1
A kind of molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite, using porous graphite charcoal as carrier,
Porous graphite metaplasia object carbon surface is inlaid with molybdenum disulfide nano sheet.
A kind of preparation method of the molybdenum disulfide nano sheet of above-mentioned the present embodiment/porous graphite metaplasia object carbon composite,
The following steps are included:
(1) porous graphite charcoal (PGBC) is prepared:
(1.1) using the agricultural wastes stalk being ground up, sieved after natural air drying as carbon matrix precursor, being placed in concentration is 1mol/L high
It in ferrous acid potassium solution, impregnates 24 hours under agitation, is subsequently placed in drying in vacuum oven, obtains immersed with permanganic acid
The agricultural wastes stalk of potassium.
(1.2) powder (i.e. immersed with the agricultural wastes stalk of potassium permanganate) obtained after will be dry in step (1.1) turns
It moves in tube furnace, is warming up to 900 DEG C with heating rate under a nitrogen atmosphere for 5 DEG C/min and carries out pyrolysis carbonization 1h, reaction knot
Natural cooling after beam, carbide is successively used concentration for the dilute hydrochloric acid solution of 1mol/L and deionized water to pyrolysis carbonization after
Product is washed, dry under the conditions of 60 DEG C, grinding, is crossed 200 sieves, is obtained porous graphite charcoal (PGBC) powder.
(2) molybdenum disulfide nano sheet is loaded:
Porous graphite charcoal powder obtained in 16mg, 24mg, 32mg step (1) is taken to be respectively placed in deionized water
In, ultrasonic disperse 30 minutes, bis- molybdic acid hydrate of 240mg was sequentially added into gained porous graphite charcoal powder dispersion liquid
Sodium and 375mg thioacetamide (molar ratio 1: 5), are uniformly mixed under magnetic stirring, obtain presoma mixed liquor；Respectively will
Above-mentioned resulting precursor mixed solution moves into the stainless steel cauldron with polytetrafluoroethylliner liner, reacts at 180 DEG C
24 hours；Reaction terminates natural cooling, centrifugation, successively using dehydrated alcohol and deionized water to the resulting black precipitate of centrifugation
It is washed, it is dry under the conditions of 60 DEG C, molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite is obtained, wherein more
When the quality of hole graphitization charcoal powder is 16mg, 24mg, 32mg, corresponding molybdenum disulfide nano sheet/porous graphite metaplasia
It is MoS that object carbon composite is numbered respectively2/PGBC16、MoS2/PGBC24、MoS2/PGBC32。
It is corresponding when the mass ratio of porous graphite charcoal powder and two molybdic acid hydrate sodium is 0.1: 1 in the present embodiment
The matter of porous graphite charcoal and molybdenum disulfide nano sheet in molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite
Amount is than being 0.15: 1.
Fig. 1 is molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite obtained in the embodiment of the present invention 1
(MoS2/PGBC24) scanning electron microscope (SEM) photograph.As shown in Figure 1, molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite table
Face becomes more coarse, inlayed the gauffer lamella of a large amount of curved edges thereon, it was demonstrated that molybdenum disulfide nano sheet is in porous stone
Being successfully generated on inkization charcoal, and the marginal portion of lamella can be exposed farthest to improve catalytic activity.
Fig. 2 is molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite obtained in the embodiment of the present invention 1
(MoS2/PGBC24) transmission electron microscope picture.Can be observed simultaneously in Fig. 2 molybdenum disulfide (~0.66nm) and graphitized carbon (~
Specific lattice spacing 0.35nm), sufficiently demonstrates the interaction of two kinds of materials, i.e. molybdenum disulfide nano sheet/porous graphite
Change the successful synthesis of charcoal composite catalyst.
Embodiment 2
A kind of application of molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite in processing antibiotic, specifically
For using molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite (MoS obtained in embodiment 12/PGBC16、MoS2/
PGBC24、MoS2/PGBC32) quadracycline in water body is handled, comprising the following steps:
Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite (MoS obtained in Example 12/PGBC16、
MoS2/PGBC24、MoS2/PGBC32), molybdenum disulfide nano sheet (MoS2), each 20mg is respectively placed in 50mL, concentration 20mg/L
Quadracycline solution in, be uniformly mixed, dark reaction 30min carried out under dark condition, after adsorption equilibrium to be achieved, in xenon
The lower photocatalytic degradation that carries out of lamp (300W, λ > 420nm) irradiation reacts 60min, processing of the completion to quadracycline in water body.
The removal rate of quadracycline in analytical solution is measured by sampling in different time intervals, as a result such as 1 institute of Fig. 3 and table
Show.
Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite and molybdenum disulfide are received in 1 embodiment of the present invention 2 of table
Influence of the rice piece to quadracycline removal effect in solution
| MoS2/PGBC16 | MoS2/PGBC24 | MoS2/PGBC32 | MoS2 | |
| Removal rate (%) | 82.58 | 91.82 | 73.34 | 43.85 |
Fig. 3 is molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite photocatalytic degradation in the embodiment of the present invention 2
The efficiency chart of quadracycline.By table 1 and Fig. 3 it is found that compared with blank test and simple molybdenum disulfide check experiment, the present invention
Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite it is non-to the removal rate of antibiotic in water body (quadracycline)
Chang Gao, wherein can reach highest antibiotic when the dosage of porous graphite charcoal is 24mg when synthetic composite material and go
Except rate, so as to which polluter ecological risk caused by the ecosystem in water body is effectively reduced.
Utilize molybdenum disulfide nano sheet obtained in the embodiment of the present invention 1/porous graphite metaplasia object carbon composite
(MoS2/PGBC24) (dense to different antibiotic (terramycin, Ofloxacin, Norfloxacin and sulfamethoxazole) solution
Degree is 20mg/L) it degrades, processing method is same as Example 2, and the results are shown in Table 2 for removal.
Molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite (MoS obtained in 2 embodiment of the present invention 1 of table2/
PGBC24)
Influence to different antibiotic removal effects
| Terramycin | Ofloxacin | Norfloxacin | Sulfamethoxazole | |
| Removal rate (%) | 88.35 | 90.07 | 85.79 | 78.83 |
As shown in Table 2, molybdenum disulfide nano sheet of the present invention/porous graphite metaplasia object carbon composite (MoS2/PGBC24) right
Terramycin, Ofloxacin, Norfloxacin and sulfamethoxazole removal rate be followed successively by 88.35%, 90.07%, 85.79% and
78.83%.As it can be seen that molybdenum disulfide nano sheet of the present invention/porous graphite metaplasia object carbon composite can effectively degrade in water body
Antibiotic, the antibiotic effectively removed in water body is had a very important significance.
Above embodiments are only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned reality
Apply example.All technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It is noted that being led for this technology
For the those of ordinary skill in domain, improvements and modifications without departing from the principle of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of molybdenum disulfide nano sheet/porous graphite metaplasia object carbon composite, which is characterized in that the molybdenum disulfide nano
Piece/porous graphite metaplasia object carbon composite is using porous graphite charcoal as carrier, the porous graphite metaplasia object carbon surface
It is inlaid with molybdenum disulfide nano sheet.
2. a kind of molybdenum disulfide nano sheet as described in claim 1/porous graphite metaplasia object carbon composite preparation method,
Characterized by comprising the following steps:
S1, agricultural wastes stalk is immersed in liquor potassic permanganate, it is dry, obtain the agricultural wastes straw immersed with potassium permanganate
Stalk；
S2, the agricultural wastes stalk obtained in step S1 immersed with potassium permanganate is subjected to pyrolysis carbonization, washed, it is dry, it grinds
Mill, sieving, obtains porous graphite charcoal powder；
S3, by porous graphite charcoal powder ultrasonic disperse obtained in step S2 in water, be added two molybdic acid hydrate sodium and
Thioacetamide carries out hydro-thermal reaction, is centrifuged, and washs, dry, and it is compound to obtain molybdenum disulfide nano sheet/porous graphite charcoal
Material.
3. preparation method according to claim 2, which is characterized in that the porous graphite charcoal powder and two hydrations
The mass ratio of sodium molybdate is 0.05~0.15: 1；The molar ratio of the two molybdic acid hydrates sodium and thioacetamide is 1: 5.
4. preparation method according to claim 2 or 3, which is characterized in that in the step S1, the liquor potassic permanganate
Concentration be 0.5mol/L~1mol/L；The time of the immersion is 12h~for 24 hours；The drying carries out under vacuum conditions.
5. preparation method according to claim 2 or 3, which is characterized in that in the step S2, the pyrolysis carbonization is in nitrogen
It is carried out under gas atmosphere；Heating rate during the pyrolysis carbonization is 5 DEG C/min；The temperature of the pyrolysis carbonization is 700 DEG C
~1000 DEG C；The time of the pyrolysis carbonization is 1h~3h；The washing is successively using diluted acid and deionized water to pyrolytic carbon
Product after change is washed；The concentration of the diluted acid is 0.1mol/L~1mol/L；The diluted acid is dilute hydrochloric acid solution；It is described
Drying carries out at being 60 DEG C in temperature；The sieving was 200 meshes.
6. preparation method according to claim 2 or 3, which is characterized in that in the step S3, the ultrasonic disperse when
Between be 30min~60min；The temperature of the hydro-thermal reaction is 160 DEG C~200 DEG C；The time of the hydro-thermal reaction be 18h~
24h；The washing is successively to be washed using dehydrated alcohol and deionized water to centrifugation product；The drying is 60 in temperature
It is carried out at DEG C.
7. a kind of molybdenum disulfide nano sheet as described in claim 1/porous graphite metaplasia object carbon composite or as right is wanted
Molybdenum disulfide nano sheet made from preparation method described in asking any one of 2~5/porous graphite metaplasia object carbon composite is being located
Manage the application in antibiotic.
8. application according to claim 7, which is characterized in that use molybdenum disulfide nano sheet/porous graphite charcoal
Composite material handles the antibiotic in water body, comprising the following steps: by molybdenum disulfide nano sheet/porous graphite metaplasia object
Carbon composite carries out photocatalysis after antibiotic water mixing progress dark reaction, adsorption equilibrium to be achieved under illumination condition
Degradation reaction completes the processing to antibiotic in water body.
9. application according to claim 8, which is characterized in that the molybdenum disulfide nano sheet/porous graphite charcoal
The mass volume ratio of composite material and antibiotic water body is 0.1g~0.5g: 1L.
10. application according to claim 8 or claim 9, which is characterized in that antibiotic is hydrochloric acid Fourth Ring in the antibiotic water body
At least one of element, terramycin, Ofloxacin, Norfloxacin and sulfamethoxazole；Antibiotic in the antibiotic water body
Concentration is 10mg/L~50mg/L；The time of the dark reaction is 30min~60min；The time of the photocatalytic degradation reaction
For 60min~120min.
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