CN106881139A - A kind of CdS/Ag/g C3N4Heterojunction composite photocatalyst and preparation method - Google Patents
A kind of CdS/Ag/g C3N4Heterojunction composite photocatalyst and preparation method Download PDFInfo
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- CN106881139A CN106881139A CN201710168382.2A CN201710168382A CN106881139A CN 106881139 A CN106881139 A CN 106881139A CN 201710168382 A CN201710168382 A CN 201710168382A CN 106881139 A CN106881139 A CN 106881139A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 42
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 230000015556 catabolic process Effects 0.000 claims abstract description 16
- 238000006731 degradation reaction Methods 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 230000004044 response Effects 0.000 claims description 16
- 239000004098 Tetracycline Substances 0.000 claims description 14
- 230000001699 photocatalysis Effects 0.000 claims description 14
- 235000019364 tetracycline Nutrition 0.000 claims description 14
- 150000003522 tetracyclines Chemical class 0.000 claims description 14
- 229960002180 tetracycline Drugs 0.000 claims description 13
- 229930101283 tetracycline Natural products 0.000 claims description 13
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 239000012265 solid product Substances 0.000 claims description 9
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Inorganic materials Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000007146 photocatalysis Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000003115 biocidal effect Effects 0.000 abstract description 8
- 239000004065 semiconductor Substances 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 239000002351 wastewater Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 150000001450 anions Chemical class 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 10
- 238000006552 photochemical reaction Methods 0.000 description 10
- 239000003643 water by type Substances 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 8
- 239000013049 sediment Substances 0.000 description 6
- 238000001291 vacuum drying Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002256 photodeposition Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005276 aerator Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229960003405 ciprofloxacin Drugs 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- -1 dicyanodiamine Chemical compound 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000005447 environmental material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 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
- 238000005286 illumination Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- KQTXIZHBFFWWFW-UHFFFAOYSA-L silver(I) carbonate Inorganic materials [Ag]OC(=O)O[Ag] KQTXIZHBFFWWFW-UHFFFAOYSA-L 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
- 229940040944 tetracyclines Drugs 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000001052 transient effect Effects 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
- B01J27/24—Nitrogen compounds
-
- 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
- C02F2101/38—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 provides a kind of CdS/Ag/g C3N4Heterojunction composite photocatalyst and preparation method, step are as follows：Step 1, preparation g C3N4Nanometer sheet；Step 2, preparation Ag/g C3N4；Step 3, preparation CdS/Ag/g C3N4Composite photo-catalyst.The present invention is realized with CdS/Ag/g C3N4It is the purpose of catalyst degradation antibiotic waste water.Semi-conducting material is used as photochemical catalyst, visible ray is used as exciting, special catalysis or conversion effet is realized by the interfacial interaction with contaminant molecule, the oxygen of surrounding and hydrone is set to be excited into the free anion of great oxidizing force, so as to reach the purpose of harmful organic substances in degraded environment, the method does not result in the formation of the wasting of resources and additional pollution, and easy to operate, is a kind of efficient process technology of environmental protection.
Description
Technical field
The invention belongs to technical field of environmental material preparation, it is related to photodeposition method to synthesize CdS/Ag/g- with hydro-thermal method
C3N4The preparation method and its usage of composite photo-catalyst.
Background technology
Antibiotic (Antibiotics) class medicine is primarily referred to as some by generations such as bacterium, mould or other microorganisms
Secondary metabolite or some artificial synthesized analogs.It is mainly used in treating various bacterium infections or pathogenic microorganisms sense
Dye class disease, the healthy and life security to the mankind serves extremely important effect, is the mankind in medical science field
One of great achievement of upper acquirement.In recent years, residual condition of the antibiotic substance in water environment is on the rise.Wherein, with four
Ring element is especially pronounced for the antibioticses contaminated wastewater of representative, and serious threat is constituted to aquatic ecological and human health.Therefore,
It has been that researcher compels to be essential to eliminate the problems such as environmental pollution for bringing of antibiotic residue and food chain product safety in environment
The significant problem to be solved.
Photocatalysis technology is simple to operate with process environmental protection as a kind of senior oxidation technology, and catalytic efficiency is high to wait special
Point.It is well known that two kinds of couplings of semiconductor can improve carrier separation efficiency.Because hetero-junctions can lead using two and half
The energy level difference of body effectively facilitates the purpose of the separation, transfer and transmission in electronics and hole, such that it is able to suppress light induced electron and sky
Cave it is compound.In recent years, Z-type hetero-junctions is by researchers' extensive concern and is furtherd investigate, existing report (He J, Shao
D W,Zheng L C et al.Construction of Z-scheme Cu2O/Cu/AgBr/Ag photocatalyst
with enhanced photocatalytic activity and stability under visible
light.Appl.Catal.B-Environ.2016,203:917-926.), by oxidation-reduction process by decomposition while
Sedimentation synthesizes Cu2O/Cu/AgBr/Ag Z-types are heterogeneous, compound, the raising photocatalytic activity of effective control electron-hole pair；
(Song S Q,Meng A Y,Jiang S J et al.Construction of Z-scheme Ag2CO3/N-doped
graphene photocatalysts with enhanced visible-light photocatalytic activity
by tuning the nitrogen species.2016,396:1368-1374.), by Ag2CO3Formed with nitrogen-doped graphene
Z-type hetero-junctions can be effectively retained the strong electronics of redox ability and the process of degradation of contaminant is participated in hole, improve catalysis effect
Rate.
Polymer and graphite nitrogen carbide (g-C3N4) there is similar Graphene layer structure, it is a kind of novel visible-light response type
Catalysis material.g-C3N4Synthetic method is simple, preparation cost is low, the raw material such as melamine, dicyanodiamine, urea only passes through
Simple calcining can be obtained by the preferable g-C of catalytic performance3N4。g-C3N4Energy gap position is unique, can complete under visible light
The light-catalyzed reaction higher to semiconductor requirement, but due to g-C3N4Exciton binding energy is high, crystallinity is low so that light induced electron-sky
Cave is difficult to separate, and photo-generated carrier mobility is small, causes photocatalytic process quantum efficiency relatively low.So, by choosing other one
Plant semiconductor structure Z-type hetero-junctions and effectively suppress Carrier recombination, improve photocatalytic activity.
CdS can directly absorb ripple as a kind of most important its energy gap of semi-conducting material about 2.4eV of II-VI group
Visible ray less than 550nm long, is widely used in preparing many fields such as photoelectric tube, photo resistance and solar cell.Together
When, it has fabulous photocatalysis performance, in visible ray of the wavelength less than 500nm, it is possible to use CdS produce a large amount of electronics and
There is redox reaction in hole, Some Organic Pollutants can be oxidized into carbon dioxide, water and inorganic salts etc..By CdS and its
He forms the existing report of semiconductor (Huo P W, Tang Y F, Zhou M J et al.Fabrication of by material
ZnWO4-CdS heterostructure photocatalysts for visible light induced
degradation of ciprofloxacin antibiotics.J.Ind.Eng.Chem.,2016,37:340-346), lead to
Hydro-thermal method is crossed by CdS and ZnWO4Heterojunction structure is formed, being combined for effective control electron-hole pair improves photocatalysis and live
Property；(Zhou P P,Le Z G,Xie Y et al.Studies on facile synthesis and properties of
mesoporous CdS/TiO2composites for photocatalysis applications.J.Alloy.Compd.,
2017,692:170-177), CdS and TiO is synthesized by simple two steps sol-gal process2Hetero-junctions effectively inhibit electronics-
Hole pair it is compound while decreasing the photoetch of CdS.To further enhance electric transmission efficiency, Ag particles are introduced as biography
Defeated passage, can promote g-C3N4The electric transmission between CdS, improves photocatalytic activity.Therefore, CdS/Ag/g-C3N4Complex light
The waste water that catalyst comes in processing environment is a kind of more satisfactory material.
The content of the invention
The purpose of the present invention is with photodeposition method and hydro-thermal method as technological means prepares CdS/Ag/g-C3N4It is compound
Photochemical catalyst.
The present invention is achieved through the following technical solutions：
A kind of CdS/Ag/g-C3N4Heterojunction composite photocatalyst, the composite photo-catalyst is by CdS, Ag, g-C3N4
It is composited, Ag/g-C3N4Mass fraction be 20~90%, remaining is CdS；By the CdS/Ag/g-C3N4Hetero-junctions is answered
Closing light catalyst is used for the photocatalytic degradation to tetracycline, and degradation rate has reached 85.67% in 90min.
A kind of CdS/Ag/g-C3N4The preparation method of heterojunction composite photocatalyst, step is as follows：
Step 1, preparation g-C3N4Nanometer sheet：
Melamine is put into Muffle furnace and is calcined, grinding is taken out after calcining terminates；Then powder is carried out again
The calcining of identical program, then calcined product is put into mechanical agitation in the beaker for filling deionized water and NaOH, is mixed
Liquid A；Mixed liquor A is transferred in reactor carries out constant temperature thermal response；After reaction terminates, room temperature to be dropped to washs solid product,
Dry, obtain g-C3N4Nanometer sheet；
Step 2, preparation Ag/g-C3N4：
By g-C3N4Nanometer sheet and AgNO3It is placed in stirring in deionized water and obtains mixed liquid B；Mixed liquid B is placed on again ultraviolet
Reaction is irradiated under lamp, after reaction terminates, room temperature to be dropped to washs solid product with deionized water, ethanol, dried, obtain Ag/g-
C3N4, it is standby；
Step 3, preparation CdS/Ag/g-C3N4Composite photo-catalyst：
By CdCl22.5 and Cys dissolving in deionized water and stirring obtains mixed liquor C to being completely dissolved；
Adjust the pH of mixed liquor C with sodium hydroxide solution again, then to adding Ag/g-C in mixed liquor C3N4Stir, be subsequently adding
Na2S·9H2O is simultaneously uniformly mixing to obtain mixed liquor D, and then, solution is transferred in reactor carries out constant temperature thermal response；Reaction knot
Shu Hou, washing precipitate, drying obtains CdS/Ag/g-C3N4Composite photo-catalyst.
In step 1, the temperature of described calcining is gradually upgraded to 550 DEG C, reaction time according to the heating rate of 2.5 DEG C/min
It is 4h.
In step 1, when preparing mixed liquor A, the g-C for being used3N4, NaOH and H2The amount ratio of O is 1.0g：0.40g：
90mL。
In step 1, the temperature of described constant temperature thermal response is 110 DEG C, and the reaction time is 18h.
In step 2, the g-C3N4、AgNO3, deionized water amount ratio be 0.20g：0.01~0.07g：60ml.
In step 3, when preparing mixed liquor C, the CdCl for being used22.5th, Cys, deionized water, Ag/g-
C3N4、Na2S·9H2The amount ratio of O is 0.1833g：0.1756g：30mL：0.05~0.15g：0.045g.
In step 3, the concentration of the sodium hydroxide solution for being used is 0.1mol/L, and the pH for being adjusted is 5~8.
In step 3, the temperature of described constant temperature thermal response is 180 DEG C, and the reaction time is 2h.
Prepared CdS/Ag/g-C3N4Composite photo-catalyst, for the tetracycline in degrading waste water.
Photocatalytic activity evaluation：Carried out in DW-01 type photochemical reactions instrument (being purchased from Educational Instrument Factory of Yangzhou University), can
See light light irradiation, by 100mL tetracyclines simulated wastewater add reactor in and determine its initial value, be subsequently adding composite photocatalyst
Agent, magnetic agitation and open aerator be passed through air maintain the catalyst in suspension or afloat, in During Illumination be spaced
10min sampling analyses, take supernatant liquor in spectrophotometer λ after centrifugationmaxMensuration absorbance at=358nm, and by public affairs
Formula：DR=[(A0-Ai)/A0] × 100% calculates degradation rate, wherein A0To reach the absorbance of tetracycline during adsorption equilibrium,
AiIt is the absorbance of the tetracycline that timing sampling is determined.
Melamine used in the present invention, silver nitrate, NaOH, caddy, Cys salt is analyzes pure,
It is purchased from traditional Chinese medicines chemical reagent Co., Ltd；Tetracycline antibiotic is mark product, is purchased from Shanghai along vigorous bioengineering Co., Ltd.
Beneficial effect：
The present invention is realized with CdS/Ag/g-C3N4It is the purpose of catalyst degradation antibiotic waste water.Semi-conducting material conduct
Photochemical catalyst, it is seen that light realizes special catalysis or conversion effect as exciting by the interfacial interaction with contaminant molecule
Should, the oxygen of surrounding and hydrone is excited into the free anion of great oxidizing force, so as to reach degrade environment in have
The purpose of machine material, the method does not result in the formation of the wasting of resources and additional pollution, and easy to operate, is a kind of environmental protection
Efficient process technology.
Brief description of the drawings
Fig. 1 is CdS/Ag/g-C3N4Composite photo-catalyst fluorogram, wherein figure (a) is Solid fluorescene spectrum, figure (b) is
Transient state fluorescence spectrum；
Fig. 2 is CdS/Ag/g-C3N4The TEM figures of composite photo-catalyst；
Fig. 3 is CdS/Ag/g-C3N4The photoelectricity flow graph of composite photo-catalyst.
Specific embodiment
With reference to specific implementation example, the present invention will be further described.
Embodiment 1：
(1)g-C3N4The preparation of nanometer sheet：
5g melamines are calcined, calcining 4h in 550 DEG C of Muffle furnaces is moved to, heating rate is 2.5 DEG C/min.Wait to forge
Grinding is taken out after sintering beam；Then powder is carried out the calcining of identical program again, g-C is obtained3N4Nanometer sheet.Then by the g- of 1g
C3N4Nanometer sheet is put into equipped with 90cm3Mechanical agitation 30min in the beaker of deionized water and 0.40g NaOH；Then, solution is turned
Move to and carry out 18h constant temperature thermal responses in 110 DEG C of reactors；After reaction terminates, room temperature to be dropped to is washed with deionized water, ethanol
Solid product, dries, and obtains g-C3N4Nanometer sheet.
(2)Ag/g-C3N4Preparation：
By the g-C of 0.20g3N4Nanometer sheet and 0.05g AgNO3It is dissolved in stirring in 60ml deionized waters；Solution is put again
3h reduction AgNO is irradiated under uviol lamp3, after reaction terminates, room temperature to be dropped to washs solid product with deionized water, ethanol,
Dry, obtain Ag/g-C3N4, it is standby；
(3)CdS/Ag/g-C3N4The preparation of composite photo-catalyst：
By 0.1833g CdCl22.5 and 0.1756g Cys are dissolved in 30mL deionized waters and stir extremely
It is completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts the pH=7 of above-mentioned solution, then wherein adds 0.1g Ag/g-
C3N4Continue to stir, be subsequently adding 0.045g Na2S·9H2O simultaneously stirs, and then, solution is transferred into 180 DEG C instead
Answer and carry out 2h constant temperature thermal responses in kettle；After reaction terminates, sediment is separated with solution with magnet, uses ethanol washing precipitate,
Drying in vacuum drying chamber is put into, CdS/Ag/g-C is obtained3N4Composite photo-catalyst.
(4) sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (3), measures the photochemical catalyst to Fourth Ring
The degradation rate of plain antibiotic reaches 85.67% in 90min.
Embodiment 2：
By the step in embodiment 1, unlike (2) by the g-C of 0.20g3N4Nanometer sheet and 0.01g AgNO3It is dissolved in
Stirred in 60ml deionized waters；Solution is placed under uviol lamp again irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, is dried, obtain Ag/g-C3N4。
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (2), measures the photochemical catalyst to tetracycline
Degradation rate 30.56% is reached in 90min.
Embodiment 3：
By the step in embodiment 1, unlike (2) by the g-C of 0.20g3N4Nanometer sheet and 0.03g AgNO3It is dissolved in
Stirred in 60ml deionized waters；Solution is placed under uviol lamp again irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, is dried, obtain Ag/g-C3N4。
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (2), measures the photochemical catalyst to tetracycline
Degradation rate 50.41% is reached in 90min.
Embodiment 4：
By the step in embodiment 1, unlike (2) by the g-C of 0.20g3N4Nanometer sheet and 0.07g AgNO3It is dissolved in
Stirred in 60ml deionized waters；Solution is placed under uviol lamp again irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, is dried, obtain Ag/g-C3N4。
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (2), measures the photochemical catalyst to tetracycline
Degradation rate 40.83% is reached in 90min.
Embodiment 5：
By the step in embodiment 1, unlike (3) by 0.1833g CdCl22.5 and 0.1756g Cys
It is dissolved in 30mL deionized waters and stirs to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=5, then wherein add 0.1g Ag/g-C3N4Continue to stir, be subsequently adding 0.045g Na2S·9H2O simultaneously stirs equal
Even, then, solution is transferred to carries out 2h constant temperature thermal responses in 180 DEG C of reactors；Reaction terminate after, with magnet by sediment with
Solution is separated, and uses ethanol washing precipitate, is put into drying in vacuum drying chamber, obtains CdS/Ag/g-C3N4Composite photo-catalyst.
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (3), measures the photochemical catalyst to tetracycline
Degradation rate 52.72% is reached in 90min.
Embodiment 6：
By the step in embodiment 1, unlike (3) by 0.1833g CdCl22.5 and 0.1756g Cys
It is dissolved in 30mL deionized waters and stirs to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=6, then wherein add 0.1g Ag/g-C3N4Continue to stir, be subsequently adding 0.045g Na2S·9H2O simultaneously stirs equal
Even, then, solution is transferred to carries out 2h constant temperature thermal responses in 180 DEG C of reactors；Reaction terminate after, with magnet by sediment with
Solution is separated, and uses ethanol washing precipitate, is put into drying in vacuum drying chamber, obtains CdS/Ag/g-C3N4Composite photo-catalyst.
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (3), measures the photochemical catalyst to tetracycline
Degradation rate 56.37% is reached in 90min.
Embodiment 7：
By the step in embodiment 1, unlike (3) by 0.1833g CdCl22.5 and 0.1756g Cys
It is dissolved in 30mL deionized waters and stirs to being completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts above-mentioned solution
PH=8, then wherein add 0.1g Ag/g-C3N4Continue to stir, be subsequently adding 0.045g Na2S·9H2O simultaneously stirs equal
Even, then, solution is transferred to carries out 2h constant temperature thermal responses in 180 DEG C of reactors；Reaction terminate after, with magnet by sediment with
Solution is separated, and uses ethanol washing precipitate, is put into drying in vacuum drying chamber, obtains CdS/Ag/g-C3N4Composite photo-catalyst.
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (3), measures the photochemical catalyst to tetracycline
Degradation rate 55.61% is reached in 90min.
Embodiment 8：
By 0.1833g CdCl22.5 and 0.1756g Cys are dissolved in 30mL deionized waters and stir extremely
It is completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts the pH=7 of above-mentioned solution, then wherein adds 0.05g Ag/g-
C3N4Continue to stir, be subsequently adding 0.045g Na2S·9H2O simultaneously stirs, and then, solution is transferred into 180 DEG C instead
Answer and carry out 2h constant temperature thermal responses in kettle；After reaction terminates, sediment is separated with solution with magnet, uses ethanol washing precipitate,
Drying in vacuum drying chamber is put into, CdS/Ag/g-C is obtained3N4Composite photo-catalyst.
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (3), measures the photochemical catalyst to tetracycline
The degradation rate of antibiotic reaches 71.67% in 90min.
Embodiment 9：
By 0.1833g CdCl22.5 and 0.1756g Cys are dissolved in 30mL deionized waters and stir extremely
It is completely dissolved；0.1mol L are used again-1Sodium hydroxide solution adjusts the pH=7 of above-mentioned solution, then wherein adds 0.15g Ag/g-
C3N4Continue to stir, be subsequently adding 0.045g Na2S·9H2O simultaneously stirs, and then, solution is transferred into 180 DEG C instead
Answer and carry out 2h constant temperature thermal responses in kettle；After reaction terminates, sediment is separated with solution with magnet, uses ethanol washing precipitate,
Drying in vacuum drying chamber is put into, CdS/Ag/g-C is obtained3N4Composite photo-catalyst.
Sample carries out photocatalytic degradation experiment in photochemical reaction instrument in taking (3), measures the photochemical catalyst to tetracycline
The degradation rate of antibiotic reaches 81.76% in 90min.
On sign of the invention, Fig. 1 is CdS/Ag/g-C3N4Composite photo-catalyst photocatalysis fluorogram；It is very clear in figure
Chu presents CdS/Ag/g-C3N4With good catalysis activity.Fig. 2 is CdS/Ag/g-C3N4The TEM of composite photo-catalyst
Figure；As can be seen from the figure photochemical catalyst has good structure.Fig. 3 is CdS/Ag/g-C3N4The photoelectric current of composite photo-catalyst
Figure.As can be seen from the figure CdS/Ag/g-C3N4With excellent photocatalytic activity.
Claims (9)
1. a kind of CdS/Ag/g-C3N4A kind of heterojunction composite photocatalyst, it is characterised in that CdS/Ag/g-C3N4Hetero-junctions is answered
Closing light catalyst, the composite photo-catalyst is by CdS, Ag, g-C3N4It is composited, Ag/g-C3N4Mass fraction be 20
~90%, remaining is CdS；By the CdS/Ag/g-C3N4Heterojunction composite photocatalyst is used for the photocatalysis drop to tetracycline
Solution, degradation rate has reached 85.67% in 90min.
2. a kind of CdS/Ag/g-C as claimed in claim 13N4The preparation method of heterojunction composite photocatalyst, its feature exists
In a kind of CdS/Ag/g-C3N4The preparation method of heterojunction composite photocatalyst, step is as follows：
Step 1, preparation g-C3N4Nanometer sheet：
Melamine is put into Muffle furnace and is calcined, grinding is taken out after calcining terminates；Then powder is carried out again identical
The calcining of program, then calcined product is put into mechanical agitation in the beaker for filling deionized water and NaOH, obtains mixed liquor A；
Mixed liquor A is transferred in reactor carries out constant temperature thermal response；After reaction terminates, room temperature to be dropped to washs solid product, does
It is dry, obtain g-C3N4Nanometer sheet；
Step 2, preparation Ag/g-C3N4：
By g-C3N4Nanometer sheet and AgNO3It is placed in stirring in deionized water and obtains mixed liquid B；Mixed liquid B is placed under uviol lamp again
Irradiation reaction, after reaction terminates, room temperature to be dropped to washs solid product with deionized water, ethanol, dries, and obtains Ag/g-C3N4,
It is standby；
Step 3, preparation CdS/Ag/g-C3N4Composite photo-catalyst：
By CdCl22.5 and Cys dissolving in deionized water and stirring obtains mixed liquor C to being completely dissolved；Hydrogen is used again
The pH of sodium hydroxide solution regulation mixed liquor C, then to adding Ag/g-C in mixed liquor C3N4Stir, be subsequently adding Na2S·
9H2O is simultaneously uniformly mixing to obtain mixed liquor D, and then, solution is transferred in reactor carries out constant temperature thermal response；After reaction terminates,
Washing precipitate, drying, obtains CdS/Ag/g-C3N4Composite photo-catalyst.
3. a kind of CdS/Ag/g-C as claimed in claim 23N4The preparation method of heterojunction composite photocatalyst, its feature exists
In in step 1, the temperature of described calcining is gradually upgraded to 550 DEG C according to the heating rate of 2.5 DEG C/min, and the reaction time is 4h.
4. a kind of CdS/Ag/g-C as claimed in claim 23N4The preparation method of heterojunction composite photocatalyst, its feature exists
In, in step 1, when preparing mixed liquor A, the g-C for being used3N4, NaOH and H2The amount ratio of O is 1.0g：0.40g：90mL.
5. a kind of CdS/Ag/g-C as claimed in claim 23N4The preparation method of heterojunction composite photocatalyst, its feature exists
In in step 1, the temperature of described constant temperature thermal response is 110 DEG C, and the reaction time is 18h.
6. a kind of CdS/Ag/g-C as claimed in claim 23N4The preparation method of heterojunction composite photocatalyst, its feature exists
In, in step 2, the g-C3N4、AgNO3, deionized water amount ratio be 0.20g：0.01~0.07g：60ml.
7. a kind of CdS/Ag/g-C as claimed in claim 23N4The preparation method of heterojunction composite photocatalyst, its feature exists
In, in step 3, when preparing mixed liquor C, the CdCl for being used2.2.5, Cys, deionized water, Ag/g-C3N4、
Na2S·9H2The amount ratio of O is 0.1833g：0.1756g：30mL：0.05~0.15g：0.045g.
8. a kind of CdS/Ag/g-C as claimed in claim 23N4The preparation method of heterojunction composite photocatalyst, its feature exists
In in step 3, the concentration of the sodium hydroxide solution for being used is 0.1mol/L, and the pH for being adjusted is 5~8.
9. a kind of CdS/Ag/g-C as claimed in claim 23N4The preparation method of heterojunction composite photocatalyst, its feature exists
In in step 3, the temperature of described constant temperature thermal response is 180 DEG C, and the reaction time is 2h.
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| CN108404959B (en) * | 2018-03-09 | 2021-01-12 | 台州职业技术学院 | Rod-like g-C3N4@SnIn4S8Composite photocatalyst and preparation method thereof |
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| CN110075896A (en) * | 2019-04-09 | 2019-08-02 | 重庆大学 | FeS2/g-C3N4The preparation method and applications of heterojunction material |
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