CN106391059A - Preparation method of ZnO/MoS2 nanosheet compound photocatalyst - Google Patents
Preparation method of ZnO/MoS2 nanosheet compound photocatalyst Download PDFInfo
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 44
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 19
- 150000001875 compounds Chemical class 0.000 title abstract description 12
- 239000002135 nanosheet Substances 0.000 title abstract description 11
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title abstract description 8
- 229910001868 water Inorganic materials 0.000 claims abstract description 18
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 235000013877 carbamide Nutrition 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims description 2
- 229950000845 politef Drugs 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract description 110
- 239000011787 zinc oxide Substances 0.000 abstract description 52
- 230000001699 photocatalysis Effects 0.000 abstract description 21
- 239000000126 substance Substances 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000005286 illumination Methods 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 230000002045 lasting effect Effects 0.000 abstract 1
- 235000015393 sodium molybdate Nutrition 0.000 abstract 1
- 239000011684 sodium molybdate Substances 0.000 abstract 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 abstract 1
- 238000007146 photocatalysis Methods 0.000 description 18
- 239000000463 material Substances 0.000 description 12
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 8
- 229910052750 molybdenum Inorganic materials 0.000 description 8
- 239000011733 molybdenum Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000003344 environmental pollutant Substances 0.000 description 6
- 231100000719 pollutant Toxicity 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [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 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- -1 Stable in properties Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002077 nanosphere Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 208000011580 syndromic disease Diseases 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000238 buergerite Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010336 energy treatment Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003960 organic solvent 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
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003643 water by type 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
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- C02F2101/38—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- 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 relates to a preparation method of a ZnO/MoS2 nanosheet compound photocatalyst. The photocatalyst with low price and high efficiency is obtained by doping a small amount of zinc oxide into molybdenum disulfide; specifically the photocatalyst is prepared by reacting the zinc oxide, sodium molybdate dehydrate and thioacetamide through a hydrothermal method. The ZnO /MoS2 nanosheet compound in the invention can quickly degrade organic pollutants, particularly dye organic pollutes, in waste water into non-pollution substances such as H2O and CO2 under normal temperature, normal pressure and illumination, and the ZnO/MoS2 nanosheet compound has lasting photocatalytic activity.
Description
Technical field
The present invention relates to a kind of ZnO/MoS2The preparation method of nanometer sheet complex photocatalyst, particularly belongs to photocatalyst
Technical field.
Background technology
In the environment, water pollution is one of main pollution of current environment, the especially Organic Pollution in water body.Organic
The toxicity of pollutant is larger, Environment release rate is higher, impact face is also relatively wide, due to its various in style and considerable volume of production with make
Consumption, brings to human health and environment and significantly endangers.Organic pollution makes soil quality decline, water quality
Pollution, food contaminant residual are exceeded, bring very big destruction to environment.The topmost source of China's water pollution is Industry Waste
Water agricultural effluent and city domestic sewage, in these waste water, major pollutants are solubility organic pollutions.They pass through various
Approach enters environment, most of entrance water body, causes the pollution of various water bodys.Therefore, set up organic dirt in effective degradation water
The method of dye thing plays an important role for water conservation.
Photocatalysis technology can be by degradable to various organic with waste gas for waste water and inorganic matters pollutant for CO2And H2O, and
And have the advantages that energy consumption is low, secondary pollution is few, reaction condition is fitted catalyst neutralisation and had repeatable utilization, so photocatalysis skill
Art becomes the focus of current environment technical research.Wherein, ZnO is the very wide material of common semiconductor middle width strip gap, and broadband is to be
Eg=3.37eV, is used as photocatalyst.Laminar nano MoS2Broadband degree be 1.80eV, there is light under visible light
Catalysis activity, MoS simultaneously2There is larger specific surface area in nanostructured, thus enhancing MoS2Photocatalytic activity.So,
MoS2It is widely used in hydrodesulfurization, photolysis water hydrogen and the catalytic reactions such as photocatalytic degradation Organic substance.With using solar energy and
Wastewater treatment is background, and as target, we are prepared for ZnO/MoS to the photocatalytic activity improving ZnO in visible ray2Nanometer sheet is multiple
Compound.It is model reaction using rhodamine B degradation under visible light, observe the impact to photocatalytic activity for this composite, and
And by ZnO/MoS2Nanometer sheet complex is applied to the degraded to organic pollution.
Molybdenum bisuphide(MoS2)It is the main component of molybdenite, be a kind of dark gray solid powder with metallic luster,
Stable in properties, water insoluble, diluted acid and concentrated sulphuric acid, typically insoluble in other acid, alkali, organic solvent.Molybdenum bisuphide and graphite
Similar, belong to hexagonal crystal system, MoS2Crystal have three kinds of crystal structures:1T shape, 2H shape, 3R shape.Wherein 1T- MoS2With 3R-
MoS2Belong to inferior stable state, 2H- MoS2Exist under normal conditions, natural 2H- MoS2Typical layer structure material in being.
Due to MoS2There are special structure and physicochemical characteristicss, so it is before every field all has relatively broad application
Scape, but nanometer MoS2There is larger specific surface area and very high surface activity, there is stronger absorbability simultaneously and urge
The advantages of change performance.It is widely used in the field applications such as hydrodenitrogeneration, lubricant, electric hydrogen storage, hydrodesulfurization and catalyst.
It is mainly applied and still falls within hydrogenation and field of lubricant, also fewer in the application of other field.Particularly it is for visible
The degraded difficulty of the hard-degraded substance under light is higher.The photo-generate electron-hole that main reasons is that its surface, to less, is tied with water
Conjunction is hardly formed hydroxyl radical free radical, thus the organic pollution being difficult in a large amount of degradation water.
Zinc oxide is belonging to the compound of II-VI race, and it has three kinds of different crystal structures, cubic salt mine, six side's fibre zinc
Ore deposit and three kinds of structures of cubic zinc blende.Under field conditions (factors), cube buergerite and cubic rock ore deposit structure are at meta shape
State, so zinc oxide(ZnO)It is to be existed with the symmetrical wurtzite structure of six sides.Due to zinc oxide(ZnO)There is wider forbidden band
Width(3.37eV), so zinc oxide(ZnO)It is a kind of important semi-conducting material.Zinc oxide(ZnO)It is kind of a quasiconductor
The electronic structure of catalyst, under having illumination condition, when the photon with certain energy or have and exceed quasiconductor bandgap energy
Photon enter quasiconductor be that electrons transit to conduction band from valence band, thus forming a hole.It is in the conduction band electricity of excited state
Son and valence band hole can tie and offset the energy of input again, and the hole of valence band can be the hydroxyl of surrounding(OH-)Electronics is robbed
Dispossess, so that hydroxyl(OH-)Become free radical, because it has strong oxidizing property, Organic substance can be degraded, by pathogenic bacteria
Kill with virus.But because it has some intrinsic defects, limit its utilization in reality.Zinc oxide is a kind of wide taboo
Band quasiconductor, can only absorb ultraviolet light, and UV energy only accounts for the 4% of solar energy, zinc oxide is for the utilization of sunlight
Rate is very low;Meanwhile, the ultraviolet excitation semiconductor product third contact of a total solar or lunar eclipse gives birth to electron-hole pair, light induced electron and hole be attached to zinc oxide
On organic pollution have an effect, be degraded to water and carbon dioxide, but the recombination rate in light induced electron and hole be remote
More than the speed having an effect with Organic substance, so greatly reduce zinc oxide photocatalysis performance.
Conventional method has Zhu Yun, the ZnO-MoS of meter Wen Jun, Ma Jinlou, Wang Qiang etc.2Photoelectric characteristic one literary composition of hetero-junctions, this article
Successively deposited the MoS of Ag doping using chemical vapour deposition technique on a si substrate2Thin film and the ZnO film of Ag doping, form
ZnO-MoS2Hetero-junctions, is mainly used in photoelectric field, does not apply in terms of photocatalysis, and the product preparation difficulty of production is relatively
Height, principally falls into the preparation of epitaxial, and prepares ZnO-MoS herein2Nanometer sheet complex is different.ZnO-MoS produced herein2Receive
Rice piece complex is ZnO and MoS2 is all nanometer sheet, is belonging to be compound to together by two kinds of nanometer sheet materials, in current document
In still belong to the first time.
In addition meaning quintessence is in MoS2Micro-nano-sphere and MoS2In the preparation of@ZnO nano-heterogeneous structure and performance study one literary composition
To MoS2Preparation method and MoS2The preparation method of@ZnO complex gives narration.ZnO and MoS in common preparation method2
Both compositely proportionals are mainly ZnO and account for vast scale, MoS2Belong to small scale, so mainly use the photocatalysis performance of ZnO
And MoS2High conduction performance and high-specific surface area mutually promoting.MoS in complex photocatalyst of the present invention2Account for vast scale,
ZnO accounts for small scale, is found that the ZnO/MnS that mass ratio is 10% first2Also have good photocatalysis performance, and mass ratio
10% ZnO/MnS2, in the test doing photocatalysis rhodamine B, under the same terms, photo-catalysis capability is than similar for nanometer sheet complex
Research Ability significantly improves.
And similar research is not involved with how preparing ZnO and MoS2The mutually compound method of two kinds of nanometer sheet materials,
From the point of view of the degradation effect to material rhodamine B of the same race, under the same terms, the complex photocatalysis performance of present invention preparation is excellent
Different.
A kind of Zinc oxide nano sheet-molybdenum disulfide nano sheet the complex of present invention preparation has a lot of advantages.Molybdenum bisuphide
It has high-specific surface area high conduction performance and preferable photocatalysis performance.It is before photocatalysis field has preferable application
Scape.But because its photo-generate electron-hole is to less, its photocatalysis performance is decayed quickly.Zinc oxide is a kind of very ripe light
Catalyst, its photocatalysis performance is very high, and there is substantial amounts of photo-generate electron-hole pair on surface, can provide substantial amounts of for molybdenum bisuphide
Individually electronics and hole, but its photo-generate electron-hole is far longer than electron transfer speed to recombination velocity, result in photocatalysis
The reduction of performance.The present invention will be mutually compound for both materials, can be complementary to one another its performance.On the one hand due to molybdenum bisuphide
High conduction performance, so that complex photo-generate electron-hole substantially reduces to recombination velocity, provides more multipotency to light-catalyzed reaction
Amount.The high-specific surface area of another aspect molybdenum bisuphide provides a lot of reaction site for light-catalyzed reaction, has greatly accelerated light
The carrying out of catalytic reaction.
Content of the invention
The purpose of the present invention is the defect existing for prior art, provides a kind of ZnO/MoS2Nanometer sheet is combined object light and urges
The preparation method of agent, described photocatalyst passes through hydro-thermal by Zinc oxide nano sheet, two molybdic acid hydrate sodium and thioacetamide
Reaction is obtained, and preparation process is as follows:
(1)Synthesis ZnO nano piece
Add 2-4mmol zinc nitrate hexahydrate, 0.2-0.4mmol sodium lauryl sulphate in 6-10mL dehydrated alcohol, through magnetic
Power stirs, and obtains solution A;Add 1-3mmol carbamide in 7-12mL deionized water, through magnetic agitation uniformly, obtain molten
In liquid B;Under conditions of being stirred continuously, solution B is dropwise instilled in solution A, after completion of dropping, the mixed solution obtaining is turned
Enter in the rustless steel autoclave that politef is inner bag;Rustless steel autoclave is put into electric drying oven with forced convection
In, maintain 100 DEG C, after reacting 6 hours, after naturally cooling to room temperature, product is centrifuged, gained filter cake is respectively
After dehydrated alcohol and distilled water wash, then in vacuum drying oven, maintain 60 DEG C of vacuum drying 12-14h;Vacuum drying is produced
Thing is put in chamber type electric resistance furnace, maintains 400 DEG C of calcining 2-3h, obtains ZnO nano piece.
(2)Synthesis ZnO/MoS2Nanometer sheet
By step(1)The ZnO nano piece of synthesis, 100-200mg bis- molybdic acid hydrate sodium, 300-400mg thioacetamide are added to
In 50-100mL deionized water, through magnetic agitation uniform after pour in reactor;Reactor is put in electric drying oven with forced convection,
Maintain 220 DEG C of reaction 20-30h, then after naturally cooling to room temperature, product be centrifuged processing, gained filter cake spend from
Sub- water is centrifuged 2-3 time, again filter cake is carried out freeze-drying process thereafter, obtains ZnO-MoS2Nanometer sheet complex photocatalyst,
Wherein ZnO and MoS2Mass ratio be 10%.
The principle of the present invention be molybdenum bisuphide due to its high-specific surface area, relatively low carrying and high conductivity, can be too
Electron transition phenomenon is produced under the irradiation of sunlight.Material surface produce photo-generate electron-hole pair, photo-generate electron-hole pair with
Water reaction produces OH, and OH and Organic substance react its exhaustive oxidation Cheng Shui and carbon dioxide etc..Zinc oxide is that a kind of light is urged
Change the very strong catalyst of performance, a small amount of doping can provide substantial amounts of photo-generate electron-hole pair for molybdenum bisuphide.Two kinds of material phases
Mutually promote to make its complex photocatalysis performance be enhanced.
Beneficial effects of the present invention:
1 present invention firstly discovers that mass ratio 10%ZnO/MoS2Nanometer sheet complex has significant photocatalysis performance, sunlight
Utilization rate high, can be complete by organic pollutant degradation in the time under sunlight, shorter.
2nd, ZnO/MoS of the present invention2Nanometer sheet complex is a kind of new complex, and room of the present invention is by ZnO nano sheet material
It is doped to MoS2In nanometer sheet material, it is belonging to the mutually compound of two kinds of nanometer sheet materials.And the ZnO/MoS of existing report2Compound
It is compound with nano-particle that thing is the compound of two kinds of nano-particle or nanosphere, is not the mutually multiple of two kinds of nanometer sheet materials
Close.ZnO/MoS of the present invention2Nobody's preparation before nanometer sheet complex photocatalyst, and preparation method is simple.
3 ZnO/MoS of the present invention2Nanometer sheet complex occupation mode is simple, as long as catalyst is put in sewage, then
Irradiate just permissible under natural light, at normal temperatures and pressures can be to use.
4 ZnO/MoS of the present invention2Nanometer sheet complex photocatalyst integrated cost is cheap, reuses efficiency high, is one
Plant the very high product of cost performance.
Brief description
Fig. 1 is Zinc oxide nano sheet of the present invention-molybdenum disulfide nano sheet complex photocatalysis performance figure;
Fig. 2 is Zinc oxide nano sheet of the present invention-molybdenum disulfide nano sheet complex electron microscopic picture.
Specific embodiment
Embodiment 1
Formerly measure 6mL dehydrated alcohol in beaker A and beaker B respectively and 7mL deionized water is mixed to form agent, then weigh
2mmol zinc nitrate hexahydrate(Zn(NO3)2•6H2O)Add in beaker A with 0.2mmol sodium lauryl sulphate, be placed on magnetic force to stir
Mix and stir on device;Then weigh 2mmol carbamide(NH2CONH2)Add in beaker B, be equally placed on stirring on magnetic stirring apparatuss
Uniformly;Again solution in beaker B is drop by drop added in beaker A and is stirred continuously, then solution in beaker A is poured into 50mL with poly-
Tetrafluoroethene is that in the rustless steel autoclave of inner bag, reactor is put into 6 hours in 100 DEG C of electric drying oven with forced convections, here
Afterwards, autoclave is naturally cooled to room temperature.Then dehydrated alcohol and distilled water centrifuge washing is used to remove impurity.Finally,
Precipitated products after centrifugation are placed in 60 DEG C of vacuum drying oven and are dried 12 hours;Afterwards, put into 400 DEG C of chamber type electric resistance furnace
Middle calcining 2 hours, then cool down, products therefrom is ZnO.;The present invention preparation photocatalyst photocatalysis test in, using 50mg
It is in 10 milligrams per liter of rhodamine B solution that this photocatalyst adds it to 50 milliliters of concentration, in dark reaction 30min by dirt
Dye thing absorption completely, is then reacted under xenon lamp irradiation, often crosses 10min and samples once, until will be complete for pollutant light degradation.
Photocatalyst of the present invention is easy to use, at normal temperatures and pressures, is directly thrown in pollutant water body just permissible
Complete the Degradation to pollutant, and reclaim conveniently, be suitable for heavy industrialization and utilize.
Embodiment 2
Weigh 100mg bis- molybdic acid hydrate sodium to add in 100mL beaker A with 200mg thioacetamide;The oxygen of preparation in treating excess syndrome example 1
Change zinc nanometer sheet 6mg, ZnO/MoS2Doping takes ZnO to add formation B in A than 10%;50 deionized waters are added to be placed on magnetic force toward in B
Stir on agitator formation C;The solution C stirring is poured in reactor;Reactor is put into electric heating forced air drying
Heat up in case, setting temperature is 220 DEG C, heat time heating time is 24 hours;After question response terminates, wait reactor natural to room temperature, then
Deionized water is centrifuged 2-3 time;Precipitate after step 6 is centrifuged is put into refrigerator and is carried out freezing and so that deionized water is freezed;Will be cold
The solid having frozen is put into and is carried out lyophilization in freezer dryer thus obtaining 10% ZnO/MoS2Nanometer sheet complex.
Embodiment 3
Weigh 100mg bis- molybdic acid hydrate sodium to add in 100mL beaker A with 200mg thioacetamide;The oxygen of preparation in treating excess syndrome example 1
Change zinc nanometer sheet 3mg, first ZnO is ground, then ZnO and MoS2Weigh ZnO by 5% and add formation B in A;50ml is added to go toward in B
Ionized water is placed on magnetic stirring apparatuss the formation C that stirs;The solution C stirring is poured in reactor;Reactor is put
Enter in electric drying oven with forced convection and heat up, setting temperature is 220 DEG C, heat time heating time is 24 hours;After question response terminates, wait reactor
Nature is to room temperature, then deionized water is centrifuged 2-3 time;By centrifugation after precipitate put into refrigerator carry out freezing make deionized water tie
Freeze;The solid freezing is put into and carries out lyophilization in freezer dryer thus obtaining 5% ZnO/MoS2Nanometer sheet.
Claims (1)
1. a kind of ZnO/MoS2The preparation method of nanometer sheet complex photocatalyst it is characterised in that:Described photocatalyst is by oxygen
Change zinc nanometer sheet, two molybdic acid hydrate sodium and thioacetamide to be obtained by hydro-thermal method, preparation process is as follows:
(1)Synthesis ZnO nano piece
Add 2-4mmol zinc nitrate hexahydrate, 0.2-0.4mmol sodium lauryl sulphate in 6-10mL dehydrated alcohol, through magnetic
Power stirs, and obtains solution A;Add 1-3mmol carbamide in 7-12mL deionized water, through magnetic agitation uniformly, obtain molten
In liquid B;Under conditions of being stirred continuously, solution B is dropwise instilled in solution A, after completion of dropping, the mixed solution obtaining is turned
Enter in the rustless steel autoclave that politef is inner bag;Rustless steel autoclave is put into electric drying oven with forced convection
In, maintain 100 DEG C, after reacting 6 hours, after naturally cooling to room temperature, product is centrifuged, gained filter cake is respectively
After dehydrated alcohol and distilled water wash, then in vacuum drying oven, maintain 60 DEG C of vacuum drying 12-14h;Vacuum drying is produced
Thing is put in chamber type electric resistance furnace, maintains 400 DEG C of calcining 2-3h, obtains ZnO nano piece;
(2)Synthesis ZnO/MoS2Nanometer sheet
ZnO nano piece that step (1) is synthesized, 100-200mg bis- molybdic acid hydrate sodium, 300-400mg thioacetamide are added to
In 50-100mL deionized water, through magnetic agitation uniform after pour in reactor;Reactor is put in electric drying oven with forced convection,
Maintain 220 DEG C of reaction 20-30h, then after naturally cooling to room temperature, product be centrifuged processing, gained filter cake spend from
Sub- water is centrifuged 2-3 time, again filter cake is carried out freeze-drying process thereafter, obtains ZnO-MoS2Nanometer sheet complex photocatalyst,
Wherein ZnO and MoS2Mass ratio be 10%.
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