CN106975507A - A kind of Ag/g C3N4Composite photo-catalyst and preparation method thereof - Google Patents
A kind of Ag/g C3N4Composite photo-catalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000002131 composite material Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 28
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 230000015556 catabolic process Effects 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000006731 degradation reaction Methods 0.000 claims abstract description 21
- 239000012265 solid product Substances 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002351 wastewater Substances 0.000 claims abstract description 7
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000004098 Tetracycline Substances 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims 1
- 235000007164 Oryza sativa Nutrition 0.000 claims 1
- 235000009566 rice Nutrition 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 34
- 230000003115 biocidal effect Effects 0.000 abstract description 7
- 238000013019 agitation Methods 0.000 abstract description 4
- 101710134784 Agnoprotein Proteins 0.000 abstract description 3
- 235000019364 tetracycline Nutrition 0.000 description 15
- 150000003522 tetracyclines Chemical class 0.000 description 15
- 229960002180 tetracycline Drugs 0.000 description 14
- 229930101283 tetracycline Natural products 0.000 description 14
- 238000006552 photochemical reaction Methods 0.000 description 13
- 238000002474 experimental method Methods 0.000 description 12
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 12
- 239000003643 water by type Substances 0.000 description 12
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000011258 core-shell material Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000002256 photodeposition Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 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
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005276 aerator Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229960003405 ciprofloxacin Drugs 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- DCOPUUMXTXDBNB-UHFFFAOYSA-N diclofenac Chemical compound OC(=O)CC1=CC=CC=C1NC1=C(Cl)C=CC=C1Cl DCOPUUMXTXDBNB-UHFFFAOYSA-N 0.000 description 1
- 229960001259 diclofenac Drugs 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
- 239000005447 environmental material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 244000000010 microbial pathogen Species 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000002060 nanoflake Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229910000510 noble metal Inorganic materials 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
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920000642 polymer Polymers 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
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000000725 suspension Substances 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
- 229940126680 traditional chinese medicines Drugs 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
Abstract
The invention provides a kind of Ag/g C3N4Composite photo-catalyst and preparation method thereof, step is as follows：Melamine is put into Muffle furnace and calcined according to calcination procedure, grinding is taken out after calcining terminates；Then powder is carried out to the calcining of identical program again, g C are obtained3N4；Then by g C3N4Mechanical agitation in the beaker equipped with deionized water and NaOH is put into, mixed liquor A is obtained；Mixed liquor A is transferred to progress constant temperature thermal response in reactor；After reaction terminates, room temperature to be dropped to washs solid product with deionized water, ethanol, dries, obtains g C3N4Nanometer sheet；By g C3N4Nanometer sheet and AgNO3It is placed in stirring in deionized water and obtains mixed liquid B；Mixed liquid B is placed on irradiation reduction AgNO under uviol lamp again3, after reaction terminates, room temperature to be dropped to washs solid product with deionized water, ethanol, dries, obtains Ag/g C3N4Composite photo-catalyst.The present invention is realized with Ag/g C3N4For the purpose of catalyst degradation antibiotic waste water.
Description
Technical field
The invention belongs to technical field of environmental material preparation, it is related to a kind of photodeposition method synthesis Ag/g-C3N4Complex light
Catalyst and preparation method.
Background technology
Antibiotic (Antibiotics) class medicine is primarily referred to as some by generations such as bacterium, mould or other microorganisms
Secondary metabolite either some artificial synthesized analogs.It is mainly used in treating various bacterium infections or pathogenic microorganisms sense
Class disease is contaminated, the healthy and life security to the mankind serves extremely important effect, be the mankind in medical science field
One of great achievement of upper acquirement.In recent years, the species of antibiotic, yield and consumption are continuously increased, to antibiotic medicine not
It is rationally serious using phenomenon, larger harm is brought to environment.By taking Ciprofloxacin as an example, many research reports show antibiotic
It has been widely present in soil, surface water, underground water, deposit, municipal sewage and animal excrements oxidation pond.Therefore, eliminate
Antibiotic lower tape comes in environment environmental pollution and be researcher the problems such as food chain product safety in the urgent need to solution
Significant problem certainly.
Polymer and graphite nitrogen carbide (g-C3N4) there is similar graphene layer structure, the overlay structure for having two dimension, in individual layer
G-C3N4Inside, C, N atom are with sp2Hydridization forms pi-conjugated system, because interlayer is combined with Van der Waals force, therefore is easier
Single layer structure is stripped into, is a kind of novel visible light responsive photocatalytic material.g-C3N4Synthetic method it is simple, prepare
Cost is low, and the raw material such as melamine, dicyanodiamine, urea only can be obtained by the preferable g- of catalytic performance by simply calcining
C3N4。g-C3N4Energy gap position is unique, and the light-catalyzed reaction higher to semiconductor requirement can be completed under bbbb visible rays, but
Due to g-C3N4Exciton binding energy is high, crystallinity is low so that photo-generate electron-hole is difficult to separate, and photo-generated carrier mobility is small, leads
Cause photocatalytic process quantum efficiency relatively low.So, take many measures to solve problem above researchers.For example：
(Zhang W,Zhou L,Deng H P,Ag modified g-C3N4composites with enhanced visible-
light photocatalytic activity for diclofenac degradation.Journal of Molecular
Catalysis A:Chemical 2016,423:270-276.), Ag/g-C is synthesized using photodeposition method3N4Complex light is urged
During agent, the activity of photochemical catalyst, g-C are improved by adjusting Ag amount3N4The electronics of generation is turned by Ag nano-particles
Move on in solution in pollutant reaction, effectively suppress the compound of electron-hole pair.(Wang J,Xia Y,Zhao H Y et
al.,Oxygen defects-mediated Z-scheme charge separation in g-C3N4/ZnO
photocatalysts for enhanced visible-light degradation of4-chlorophenol and
hydrogen evolution.Applied Ctalysis B:Environmental.2017,206:406-416.), by g-
C3N4Z-type hetero-junctions, g-C are prepared as with ZnO3N4Hole and ZnO electronics be combined with each other, remaining oxidation-reduction quality is stronger
Electron hole, effectively improve the efficiency of catalyst degradation pollutant.(Xing Z,Chen Y F,Liu C Y et al.,
Synthesis of core-shell ZnO/oxygen doped g-C3N4visible light driven
photocatalyst via hydrothermal method.Journal of Alloys and Compounds.2017,
708:853-861.), ZnO- oxygen dopings g-C is synthesized using hydro-thermal method3N4Core shell structure, core shell structure is conducive in hetero-junctions circle
Improve carrier separation efficiency in face；Oxygen doping g-C3N4Can effectively suppress electron-hole pair it is compound while, can also widen
Visible absorption scope, further improves catalyst degradation pollutant efficiency.The present invention is by g-C3N4It is prepared into two-dimensional nano thin
Piece, and in g-C3N4Nano flake surface deposits one layer of nano Ag particles, can have using noble metal local surfaces plasma effect
Help electric transmission and suppress Carrier recombination, improve photocatalytic activity.
The content of the invention
The purpose of the present invention is to prepare Ag/g-C using photodeposition method as technological means3N4Composite photo-catalyst.
The present invention is achieved through the following technical solutions：
A kind of Ag/g-C3N4Composite photo-catalyst, the photochemical catalyst that meets is by Ag particles and g-C3N4Nanometer sheet is combined
, the Ag uniform particles are scattered in g-C3N4Nanometer sheet surface；By 0.1g Ag/g-C3N4Composite photo-catalyst is used to drop
Solve concentration 20mg L-1Tetracycline simulated wastewater, degradation rate has reached 85.6% in 120min.
A kind of Ag/g-C3N4The preparation method of composite photo-catalyst, step is as follows：
Step 1, preparation g-C3N4；
Melamine is put into Muffle furnace and calcined according to calcination procedure, grinding is taken out after calcining terminates；Then
Powder is carried out to the calcining of identical program again, g-C is obtained3N4；Then by g-C3N4It is put into the beaker equipped with deionized water and NaOH
Middle mechanical agitation, obtains mixed liquor A；Mixed liquor A is transferred to progress constant temperature thermal response in reactor；After reaction terminates, wait to drop
To room temperature, solid product is washed with deionized water, ethanol, dries, obtains g-C3N4Nanometer sheet；
Step 2, preparation Ag/g-C3N4Composite photo-catalyst：
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
Irradiation reduction AgNO under lamp3, after reaction terminates, room temperature to be dropped to washs solid product with deionized water, ethanol, dries, obtains
Ag/g-C3N4Composite photo-catalyst.
In step 1, described calcination procedure is rises to 600 DEG C according to 4.5 DEG C/min heating rate, and the reaction time is
3h。
In step 1, when preparing mixed liquor A, used g-C3N4, NaOH and deionized water amount ratio be 1.0g：
0.30g：60mL.
In step 1, the temperature of described constant temperature thermal response is 110 DEG C, and the reaction time is 18h.
In step 2, when preparing mixed liquid B, used g-C3N4Nanometer sheet, AgNO3, deionized water amount ratio be
0.2g：0.005~0.1g：50mL.
In step 2, the time that reduction is irradiated under described uviol lamp is 30min~210min.
Prepared 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, 100mL tetracyclines simulated wastewater is added in reactor and its initial value is determined, composite photocatalyst is then added
Agent, magnetic agitation simultaneously opens aerator and is passed through air and maintain the catalyst in suspension or afloat, is spaced in During Illumination
Supernatant liquor is taken after 10min sampling analyses, centrifugation in spectrophotometer λmaxAbsorbance is determined at=358nm, and passes through public affairs
Formula：DR=[(A0-Ai)/A0] × 100% calculates degradation rate, wherein A0To reach the absorbance of tetracycline during adsorption equilibrium,
AiThe absorbance of the tetracycline determined for timing sampling.
Melamine used in the present invention, silver nitrate, the medicine such as sodium hydroxide is that analysis is pure, is purchased from traditional Chinese medicines chemistry examination
Agent Co., Ltd；Tetracycline antibiotic is mark product, is purchased from Shanghai along vigorous bioengineering Co., Ltd.
Beneficial effect：
The present invention is realized with Ag/g-C3N4For the purpose of catalyst degradation antibiotic waste water.Semi-conducting material is urged as light
Agent, it is seen that light is realized special catalysis or conversion effet by the interfacial interaction with contaminant molecule, made as exciting
The oxygen and hydrone of surrounding are excited into the free anion of great oxidizing force, so as to reach harmful organic substances in degraded environment
Purpose, this method do not result in the formation of the wasting of resources and additional pollution, and easy to operate, is a kind of the efficient of environmental protection
Treatment technology.
Brief description of the drawings
Fig. 1 is Ag/g-C3N4The SEM figures of composite photo-catalyst, wherein, figure a, b are Ag/g-C3N4；
Fig. 2 is Ag/g-C3N4The TEM figures of composite photo-catalyst, wherein, figure a is g-C3N4, figure b-d is Ag/g-C3N4；
Fig. 3 is Ag/g-C3N4The photoelectricity flow graph of composite photo-catalyst.
Embodiment
With reference to specific implementation example, the present invention will be further described.
Embodiment 1：
(1)g-C3N4The preparation of nanometer sheet：
3g melamines are calcined, calcining 3h in 600 DEG C of Muffle furnaces is moved to, heating rate is 4.5 DEG C/min.Wait to forge
Sinter and grinding is taken out after beam；Then powder is carried out to the calcining of identical program again, g-C is obtained3N4Nanometer sheet.Then by 1g g-
C3N4Nanometer sheet is put into equipped with 60cm3Mechanical agitation 30min in deionized water and 0.30g NaOH beaker；Then, solution is turned
Move to progress 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, obtains g-C3N4Nanometer sheet.
(2)Ag/g-C3N4Preparation：
By 0.20g g-C3N4Nanometer sheet and 0.05g AgNO3It is dissolved in 50ml deionized waters and stirs；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-C3N4Composite photo-catalyst.
(3) sample in (2) is taken to carry out photocatalytic degradation experiment in photochemical reaction instrument, the 0.1g photochemical catalysts are used to drop
Solve concentration 20mg L-1Tetracycline simulated wastewater, degradation rate has reached 85.6% in 120min.
Embodiment 2：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.005g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, dries, obtains Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 21.35% in 120min.
Embodiment 3：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.01g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, dries, obtains Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 27.42% in 120min.
Embodiment 4：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.03g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, dries, obtains Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 51.73% in 120min.
Embodiment 5：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.07g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, dries, obtains Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 40.15% in 120min.
Embodiment 6：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.08g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 3h reduction AgNO3, after reaction terminates, room temperature to be dropped to,
Solid product is washed with deionized water, ethanol, dries, obtains Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 35.48% in 120min.
Embodiment 7：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.05g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 30min reduction AgNO3, after reaction terminates, room to be dropped to
Temperature, solid product is washed with deionized water, ethanol, is dried, is obtained Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 53.06% in 120min.
Embodiment 8：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.05g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 60min reduction AgNO3, after reaction terminates, room to be dropped to
Temperature, solid product is washed with deionized water, ethanol, is dried, is obtained Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 55.64% in 120min.
Embodiment 9：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.05g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 90min reduction AgNO3, after reaction terminates, room to be dropped to
Temperature, solid product is washed with deionized water, ethanol, is dried, is obtained Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 55.97% in 120min.
Embodiment 10：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.05g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 120min reduction AgNO3, after reaction terminates, wait to drop to
Room temperature, solid product is washed with deionized water, ethanol, is dried, is obtained Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 64.94% in 120min.
Embodiment 11：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.05g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 150min reduction AgNO3, after reaction terminates, wait to drop to
Room temperature, solid product is washed with deionized water, ethanol, is dried, is obtained Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 72.48% in 120min.
Embodiment 12：
By the step in embodiment 1, unlike (2) by 0.20g g-C3N4Nanometer sheet and 0.05g AgNO3It is dissolved in
Stirred in 50ml deionized waters；Solution is placed under uviol lamp again and irradiates 210min reduction AgNO3, after reaction terminates, wait to drop to
Room temperature, solid product is washed with deionized water, ethanol, is dried, is obtained Ag/g-C3N4Composite photo-catalyst.
Take sample in (2) to carry out photocatalytic degradation experiment in photochemical reaction instrument, measure the 0.1g photochemical catalysts to dense
Spend for 20mg L-1The degradation rate of tetracycline reaches 80.51% in 120min.
On the sign of the present invention, Fig. 1 is Ag/g-C3N4Composite photo-catalyst SEM schemes；Ag/g-C is presented in figure3N4's
Pattern, Ag uniform particles are distributed in g-C3N4The surface of nanometer sheet.Fig. 2 is Ag/g-C3N4The TEM figures of composite photo-catalyst；From
G-C can be further observed that in figure3N4The laminate structure of nanometer sheet and the particle size of Ag particles.Fig. 3 is Ag/g-C3N4It is multiple
The photoelectricity flow graph of closing light catalyst, as can be seen from the figure Ag/g-C3N4Photo-current intensity apparently higher than g-C3N4, fully demonstrate,prove
Bright Ag is added to g-C3N4The photocatalytic activity of photochemical catalyst is effectively increased afterwards.
Claims (7)
1. a kind of Ag/g-C3N4Composite photo-catalyst, it is characterised in that the photochemical catalyst that meets is by Ag particles and g-C3N4Receive
Rice piece is composited, and the Ag uniform particles are scattered in g-C3N4Nanometer sheet surface；By 0.1g Ag/g-C3N4Composite photocatalyst
Agent is used to degrade concentration for 20mg L-1Tetracycline simulated wastewater, degradation rate has reached 85.6% in 120min.
2. a kind of Ag/g-C as claimed in claim 13N4The preparation method of composite photo-catalyst, it is characterised in that step is such as
Under：
Step 1, preparation g-C3N4；
Melamine is put into Muffle furnace and calcined according to calcination procedure, grinding is taken out after calcining terminates；Then by powder
End carries out the calcining of identical program again, obtains g-C3N4；Then by g-C3N4It is put into machine in the beaker equipped with deionized water and NaOH
Tool is stirred, and obtains mixed liquor A；Mixed liquor A is transferred to progress constant temperature thermal response in reactor；After reaction terminates, room to be dropped to
Temperature, washs solid product, dries, obtains g-C3N4Nanometer sheet；
Step 2, preparation Ag/g-C3N4Composite photo-catalyst：
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 reduction AgNO3, after reaction terminates, room temperature to be dropped to washs solid product, dries, obtains Ag/g-C3N4Composite photocatalyst
Agent.
3. a kind of Ag/g-C as claimed in claim 23N4The preparation method of composite photo-catalyst, it is characterised in that in step 1,
Described calcination procedure is rises to 600 DEG C according to 4.5 DEG C/min heating rate, and the reaction time is 3h.
4. a kind of Ag/g-C as claimed in claim 23N4The preparation method of composite photo-catalyst, it is characterised in that in step 1,
When preparing mixed liquor A, used g-C3N4, NaOH and deionized water amount ratio be 1.0g：0.30g：60mL.
5. a kind of Ag/g-C as claimed in claim 23N4The preparation method of composite photo-catalyst, it is characterised in that 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 Ag/g-C as claimed in claim 23N4The preparation method of composite photo-catalyst, it is characterised in that in step 2,
When preparing mixed liquid B, used g-C3N4Nanometer sheet, AgNO3, deionized water amount ratio be 0.2g：0.005~0.1g：
50mL。
7. a kind of Ag/g-C as claimed in claim 23N4The preparation method of composite photo-catalyst, it is characterised in that in step 2,
The time that reduction is irradiated under described uviol lamp is 30min~210min.
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