CN109985651A - A kind of graphite phase carbon nitride/silver oxide composite photo-catalyst and preparation method thereof - Google Patents
A kind of graphite phase carbon nitride/silver oxide composite photo-catalyst and preparation method thereof Download PDFInfo
- Publication number
- CN109985651A CN109985651A CN201910267025.0A CN201910267025A CN109985651A CN 109985651 A CN109985651 A CN 109985651A CN 201910267025 A CN201910267025 A CN 201910267025A CN 109985651 A CN109985651 A CN 109985651A
- Authority
- CN
- China
- Prior art keywords
- carbon nitride
- silver oxide
- phase carbon
- oxide composite
- graphite phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910001923 silver oxide Inorganic materials 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 19
- 239000010439 graphite Substances 0.000 title claims abstract description 19
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 claims abstract description 30
- 239000006185 dispersion Substances 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 26
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 description 21
- 238000007146 photocatalysis Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 239000012265 solid product Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 238000013019 agitation Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- VFWRGKJLLYDFBY-UHFFFAOYSA-N silver;hydrate Chemical compound O.[Ag].[Ag] VFWRGKJLLYDFBY-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000005303 weighing Methods 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
A kind of graphite phase carbon nitride/silver oxide composite photo-catalyst and preparation method thereof, graphite phase carbon nitride/silver oxide composite photo-catalyst preparation method include the following steps: 1) to calcine dicyanodiamine at 450-650 DEG C and obtain g-C3N4;2) g-C is prepared3N4Dispersion liquid, to g-C3N4Sodium hydroxide is added in dispersion liquid and silver nitrate is reacted, obtains crude product, crude product is washed, is dried to obtain Ag2O/g‑C3N4Composite photo-catalyst.The Ag being prepared according to the method for the present invention2O/g‑C3N4Composite photo-catalyst has good photocatalytic activity and stability.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of graphite phase carbon nitride/silver oxide composite photo-catalyst
And preparation method thereof.
Background technique
Solar energy is a kind of renewable and clean energy resource, in the case where fossil fuel is increasingly exhausted, solar energy gradually at
The important component of the energy is used for the mankind.Under the trend of sustainable development, photocatalysis technology be proved to be it is a kind of efficiently,
Green and potential emerging technology.Photocatalysis technology is a kind of a kind of skill that the band structure special based on semiconductor is established
Art, core are semiconductor light-catalysts.However the photochemical catalyst that researcher's discovery is studied at present is TiO2, TiO2Forbidden band
Wider (3.2eV) is only capable of absorbing the ultraviolet light for being less than 387nm, and solar energy utilization ratio is low, and the recombination rate of its carrier is high, light
Catalytic efficiency is low.Solar spectrum by 5% ultraviolet light, near-infrared (NIR) light group of visible light of 42-45% and 50% or more
At, however the photochemical catalyst studied at present, ultraviolet light is only absorbed mostly, or absorb a part of visible light, to the benefit of sunlight
It is low with rate, to limit its large-scale practical application.In order to make full use of solar energy, develop novel with excellent close red
The photochemical catalyst of outer photoresponse has important practical significance.
Summary of the invention
Present invention solves the technical problem that are as follows: semiconductor material has been prepared using common chemical synthesis in the present invention
Graphite phase carbon nitride (g-C3N4) and metallic compound photochemical catalyst silver oxide (Ag2O) composite photo-catalyst Ag2O/g-C3N4,
There is good photocatalytic activity under near infrared light, improve the utilization efficiency of sunlight.
Specific solution provided by the invention includes the following steps:
1) dicyanodiamine is calcined at 450-650 DEG C and obtains g-C3N4;
2) g-C is prepared3N4Dispersion liquid, Xiang Suoshu g-C3N4Sodium hydroxide is added in dispersion liquid and silver salt is reacted, obtains
Crude product washs the crude product, is dried to obtain Ag2O/g-C3N4Composite photo-catalyst.
The utility model has the advantages that
Silver oxide Ag2O is a kind of nontoxic, the brown powder with simple cubic structure, it is hot in silver oxide
The most stable of one kind of mechanical property.As p-type semiconductor, silver oxide is found to be a kind of with a narrow 1.2ev energy
The visible light catalyst of band gap, valence band are about 1.4ev, and conduction band is about 0.2ev, and silver oxide has excellent visible light-close red
Outer photoresponse ability, however since its forbidden bandwidth is relatively narrow, electrons and holes recombination rate is higher, so pure Ag2O is in light
It is very restricted in catalytic applications.g-C3N4It is a kind of inorganic semiconductor material, there is typical semiconductor energy band structure,
Its valence band is about 1.4eV, and conduction band is about -1.30eV, and forbidden bandwidth is about 2.7eV, is a kind of to urge with visible light-responded light
Change material.
Due to Ag2O and g-C3N4Between fermi level and position of energy band difference, Ag2O/g-C3N4Middle Ag2O and g-
C3N4P-n heterojunction structure is formed, and forms an internal electric field at p-n heterojunction interface.It is only aerobic under near infrared light
Change silver Ag2O, which can be excited, generates electrons and holes, Ag2Electronics (e in the valence band (VB) of O-) conduction band CB can be excited to
On, same amount of hole (h is left in its valence band+) simultaneously, Ag2Light induced electron on O conduction band CB under the action of internal electric field,
Transfer to the g-C of corrigendum3N4Conduction band CB on, facilitate Ag2The light induced electron of O and the separation in hole, greatly reduce Ag2O
Internal electron and hole it is compound, effectively increase Ag2The photocatalytic activity of O.
Based on the above technical solution, the present invention can also be improved as follows:
Further, the calcination time of step 1) is 2-6h.
Dicyanodiamine can sufficiently be reacted under this condition, obtain g-C3N4Yield is high, purity is high.
Specifically, in air atmosphere, Muffle furnace being warming up to 450-650 DEG C and calcines 2-6h, is then naturally cooled to
Room temperature, grinding obtain faint yellow solid product.
Further, heating rate is 0.5-3 DEG C/min in step 1).
Specifically, in air atmosphere, will be warming up in step 1) in Muffle furnace with the heating rate of 0.5-3 DEG C/min
450-650℃。
Preferably, heating rate is 1-2 DEG C/min. in step 1)
G-C is obtained under this condition3N4Yield is high, and crystallinity is high.
Further, g-C in the step 2)3N4The dispersion solvent of dispersion liquid is pure water, g-C in the dispersion liquid3N4It is dense
Degree is 0.18-1.2g/L.
Thus, it is only necessary to a small amount of g-C be added3N4, so that it may obtain the Ag of photocatalytic activity with higher2O/g-C3N4It is compound
Photochemical catalyst.
Further, by g-C in step 2)3N4It is added to ultrasound 20-40min in pure water, obtains g-C3N4Dispersion liquid.
G-C under this condition3N4G-C in dispersion liquid3N4 is uniformly dispersed.
Further, g-C in step 2)3N4Mass ratio with the silver salt is 1:(6-40).
Further, the g-C after sodium hydroxide and silver nitrate is added in step 2)3N4The concentration of sodium hydroxide is in dispersion liquid
0.1-0.5mol/L。
Preferably, the g-C after sodium hydroxide and silver nitrate is added in step 2)3N4The concentration of sodium hydroxide is in dispersion liquid
0.1-0.5mol/L。
With this condition, high yield, the Ag of high activity can be obtained2O/g-C3N4Composite photo-catalyst.
Further, to the g-C after addition sodium hydroxide and silver nitrate in step 2)3N4Dispersion liquid continues to stir 20-
40min obtains the crude product.
Under this condition, sufficient reaction can be obtained in raw material, obtains composite photocatalyst with good photocatalytic activity.
Further, step 2) carries out in darkroom.
Thus, it is possible to which silver nitrate solution is avoided to decompose under light illumination, Ag is generated, the higher g- of purity can be obtained as a result,
C3N4/Ag2O。
The Ag being prepared according to the method for the present invention2O/g-C3N4Composite photo-catalyst has good under near infrared light
Photocatalytic activity, improve the utilization efficiency of sunlight;Ag2O/g-C3N4Composite catalyst improves Ag2O light induced electron and sky
The rate of departure in cave, photocatalytic activity are substantially better than pure Ag2O photochemical catalyst.
The present invention also provides a kind of graphite phase carbon nitride/silver oxide composite photo-catalysts, according to graphite described above
Phase carbon nitride/silver oxide composite photocatalyst preparation method is prepared.
Thus g-C is obtained3N4/Ag2O composite photocatalyst has good photocatalytic activity and stability.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 is g-C3N4/Ag2O composite photo-catalyst is near infrared region to the photocatalytic degradation figure of RhB.
Fig. 2 is g-C3N4/Ag2Spectrum change figure of O (1:16) composite photo-catalyst in near-infrared region degradation RhB.
Fig. 3 is g-C3N4/Ag2Circulation of O (1:16) composite photo-catalyst in near-infrared region, which is degraded, to be schemed.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
Below with reference to Fig. 1-3 and with reference to the specific embodiment description present invention.
Embodiment 1
(1)g-C3N4Preparation
2g dicyanodiamine solid is taken to be put into the crucible of capping, under air atmosphere, with 0.5 DEG C/min in Muffle furnace
Heating rate be warming up to 450 DEG C and calcine 2h, then cooled to room temperature, grinding obtains faint yellow g-C3N4Solid powder.
(2)Ag2O/g-C3N4The preparation of composite photo-catalyst
By 0.0368 gram of g-C3N4Powder, which is added in 30ml deionized water and is ultrasonically treated 30min, obtains g-C3N4Dispersion
0.17gNaOH is added to g-C by liquid3N4In dispersion liquid and 30min is stirred, under agitation, 13mL0.1mol/ is added dropwise
The AgNO of L3Solution is reacted, and under dark condition, is continued stirring 20 minutes, is centrifugally separating to obtain thick production using centrifuge
Object, then be washed with deionized and be centrifuged, in triplicate, solid product is in 60 DEG C of dry 12h.
Embodiment 2
(1)g-C3N4Preparation
12g dicyanodiamine solid is taken to be put into the crucible of capping, under air atmosphere, with 3 DEG C/min's in Muffle furnace
Heating rate is warming up to 650 DEG C and calcines 6h, then cooled to room temperature, and grinding obtains faint yellow g-C3N4Solid powder.
(2)Ag2O/g-C3N4The preparation of composite photo-catalyst
By 0.0055 gram of g-C3N4 powder, which is added in 30ml deionized water and is ultrasonically treated 30min, obtains g-C3N4Dispersion
0.86gNaOH is added to g-C by liquid3N4In dispersion liquid and 30min is stirred, under agitation, 13mL0.1mol/ is added dropwise
The AgNO of L3Solution is reacted, and is continued stirring 40 minutes under dark condition, is centrifugally separating to obtain crude product using centrifuge,
It is washed with deionized and is centrifuged again, in triplicate, solid product is in 60 DEG C of dry 12h.
Embodiment 3
(1)g-C3N4Preparation
5g dicyanodiamine solid is taken to be put into the crucible of capping, under air atmosphere, with 1.5 DEG C/min in Muffle furnace
Heating rate be warming up to 550 DEG C and calcine 4h, then cooled to room temperature, grinding obtains faint yellow g-C3N4Solid powder.
(2)Ag2O/g-C3N4The preparation of composite photo-catalyst
By 0.0188 gram of g-C3N4Powder, which is added in 30ml deionized water and is ultrasonically treated 30min, obtains g-C3N4Dispersion
0.6gNaOH is added to g-C by liquid3N4In dispersion liquid and 30min is stirred, under agitation, 13mL0.1mol/L is added dropwise
AgNO3Solution is reacted, and to continuous stirring 30 minutes is continued under dark condition, is centrifugally separating to obtain thick production using centrifuge
Object, then be washed with deionized and be centrifuged, in triplicate, solid product is in 60 DEG C of dry 12h.
Embodiment 4-6
It is similar to Example 1, the difference is that, g-C in embodiment 4, embodiment 5 and embodiment 63N4The amount of taking point
It Wei not 0.0368g, 0.0094g and 0.0047g.
Comparative example 1
5g dicyanodiamine solid is taken to be put into the crucible of capping, under air atmosphere, with 1.5 DEG C/min in Muffle furnace
Heating rate be warming up to 550 DEG C and calcine 4h, then cooled to room temperature, grinding obtains faint yellow g-C3N4Solid powder.
Comparative example 2
0.6gNaOH is added in pure water and is stirred 30min, under agitation, 13mL0.1mol/L is added dropwise
AgNO3Solution obtains mixed reaction solution, continuously stirs 30 minutes under dark condition to the mixed reaction solution, using centrifugation
Machine is centrifugally separating to obtain crude product, then is washed with deionized and is centrifuged, and in triplicate, solid product is obtained in 60 DEG C of dry 12h
To Ag2O。
The photocatalytic activity of catalyst is analyzed
Active testing is carried out to the final product in embodiment 3-6 and comparative example 1-2 respectively, and makees two groups to according to the facts
It tests.Rhodamine B (RhB) solution of 100mL10mg/L is taken, photochemical catalyst dosage is 0.1g, after being uniformly dispersed, takes RhB stoste
6mL is labeled as No.1 sample.Under non-illuminated conditions, 30min is stirred, so that catalyst is reached absorption-desorption in RhB solution flat
Weighing apparatus draws reaction solution 6mL and is labeled as No. two samples, opens light source (optical source wavelength λ >=800nm) and starts timing, mixed
Reaction solution carries out degradation 120min under visible light, takes a sample every 30min, samples taken is centrifugated in centrifuge
10min takes supernatant 5mL to measure absorbance value on full scan ultraviolet-visible spectrophotometer, and it is molten to record target contaminant
Light absorption value of the liquid in maximum absorption wave strong point (i.e. at 554nm).
It is imitated by detecting the light absorption value of solution under different light application times come photocatalytic degradation of the analysis of catalyst material to RhB
Fruit sees formula (1):
Wherein, C0、A0Respectively represent the initial concentration and absorbance value of solution, Ct、AtIt respectively represents molten after light application time th
Liquid concentration and absorbance.
As a result as shown in Figure 1, RhB is hardly degraded in the case where no light has photochemical catalyst (control 1);Do not having
There is catalyst, only under near infrared light light conditions (control 2), RhB is also hardly degraded.It can illustrate, g-C3N4/Ag2O
Composite photo-catalyst is to complete under the collective effect of light and photochemical catalyst to RhB photocatalytic degradation in near-infrared region;It is pure
g-C3N4Photocatalytic Degradation, pure Ag are not almost generated to RhB in near-infrared region2O has light to RhB in near-infrared region
Catalytic degradation effect, but relative to pure g-C3N4And Ag2O, g-C3N4/Ag2Photocatalysis of the O composite photo-catalyst in near-infrared region
Performance is remarkably reinforced;In the synthesis process of photochemical catalyst, work as g-C3N4Additional amount be respectively 0.0368g, 0.188g,
0.0094g and 0.0047g, i.e. g-C3N4/Ag2The mass ratio of O is respectively 1:8 (embodiment 4), 1:16 (embodiment 3), 1:32
(embodiment 5), 1:64 (embodiment 6), obtained g-C3N4/Ag2O composite photo-catalyst activity is apparently higher than pure Ag2O photocatalysis
Agent, after illumination 5 hours, the removal rate to RhB is respectively 57%, 61%, 56% and 40%.In g-C3N4/Ag2The quality of O
During changing to 1:64 from 1:8, the activity of obtained composite photocatalyst first increases to be declined afterwards.In g-C3N4/Ag2O mass
When than for 1:16, the photocatalytic activity highest of obtained composite catalyst.As shown in Fig. 2, g-C3N4/Ag2O (1:16) complex light
Catalyst near-infrared region degradation RhB spectrum change figure, with the increase in reaction time, the maximum absorption band 554nm of RhB
Place's absorbance value is gradually decreasing, and close to 0 after 5h, shows that RhB molecule is effectively decomposed.When composite photo-catalyst mass ratio is
When 1:64, with pure Ag2The catalytic performance of O is close, this may be due to g-C3N4Specific gravity only accounts for 1.5%, g- of composite photo-catalyst
C3N4Content is very few, thus with pure Ag2The active difference of O is little.
The thiocyanic acid g-C prepared with embodiment 13N4/Ag2O (1:16) be catalyst carry out photocatalysis (optical source wavelength λ >=
800nm) the circulation experiment of degradation RhB, as shown in figure 3, after circulation 4 times, g-C3N4/Ag2O still has good photocatalysis living
Property, illustrate the g-C of this method preparation3N4/Ag2O catalyst has good photocatalysis stability.
Although the embodiment of the present invention is described in detail above, it will be understood by those skilled in the art that:
A variety of change, modification, replacement and modification can be carried out to these embodiments in the case where not departing from the principle of the present invention and objective,
The scope of the present invention is defined by the claims and their equivalents.
Claims (10)
1. a kind of graphite phase carbon nitride/silver oxide composite photo-catalyst preparation method, which comprises the steps of:
1) dicyanodiamine is calcined at 450-650 DEG C and obtains g-C3N4;
2) g-C is prepared3N4Dispersion liquid, Xiang Suoshu g-C3N4Sodium hydroxide is added in dispersion liquid and silver nitrate is reacted, obtains thick
Product washs the crude product, is dried to obtain Ag2O/g-C3N4Composite photo-catalyst.
2. graphite phase carbon nitride according to claim 1/silver oxide composite photocatalyst preparation method, which is characterized in that step
It is rapid 1) in calcination time be 2-6h.
3. graphite phase carbon nitride according to claim 1/silver oxide composite photocatalyst preparation method, which is characterized in that step
It is rapid 1) in heating rate be 0.5-3 DEG C/min.
4. graphite phase carbon nitride according to claim 1/silver oxide composite photocatalyst preparation method, which is characterized in that step
It is rapid 2) in g-C3N4The dispersion solvent of dispersion liquid is pure water, g-C in the dispersion liquid3N4Concentration be 0.18-1.2g/L.
5. graphite phase carbon nitride according to claim 4/silver oxide composite photocatalyst preparation method, which is characterized in that step
It is rapid 2) in by g-C3N4It is added to ultrasound 20-40min in pure water, obtains g-C3N4Dispersion liquid.
6. graphite phase carbon nitride according to claim 1/silver oxide composite photocatalyst preparation method, which is characterized in that step
It is rapid 2) in g-C3N4Mass ratio with the silver nitrate is 1:(6-40).
7. graphite phase carbon nitride according to claim 1/silver oxide composite photocatalyst preparation method, which is characterized in that step
Rapid 2) the middle g-C being added after sodium hydroxide and silver nitrate3N4The concentration of sodium hydroxide is 0.1-0.5mol/L in dispersion liquid.
8. graphite phase carbon nitride according to claim 1/silver oxide composite photocatalyst preparation method, which is characterized in that step
It is rapid 2) in it is described addition sodium hydroxide and silver nitrate after g-C3N4Dispersion liquid continues to stir 20-40min, obtains the thick production
Object.
9. -8 any graphite phase carbon nitride/silver oxide composite photocatalyst preparation method, feature exist according to claim 1
In step 2) carries out in darkroom.
10. a kind of graphite phase carbon nitride/silver oxide composite photo-catalyst, which is characterized in that any described by claim 1-9
Graphite phase carbon nitride/silver oxide composite photocatalyst preparation method is prepared.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910267025.0A CN109985651A (en) | 2019-04-03 | 2019-04-03 | A kind of graphite phase carbon nitride/silver oxide composite photo-catalyst and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910267025.0A CN109985651A (en) | 2019-04-03 | 2019-04-03 | A kind of graphite phase carbon nitride/silver oxide composite photo-catalyst and preparation method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN109985651A true CN109985651A (en) | 2019-07-09 |
Family
ID=67132219
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910267025.0A Pending CN109985651A (en) | 2019-04-03 | 2019-04-03 | A kind of graphite phase carbon nitride/silver oxide composite photo-catalyst and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109985651A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115041212A (en) * | 2022-06-17 | 2022-09-13 | 河北农业大学 | Silver chloride-carbon nitride composite photocatalyst and preparation method and application thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH07284664A (en) * | 1994-04-20 | 1995-10-31 | Riken Corp | Waste gas purification material and method for purifying waste gas |
EP2064765A2 (en) * | 2006-04-18 | 2009-06-03 | Universita Degli Studi Di Padova | Electrocatalysts based on mono/plurimetallic carbon nitrides for polymer electrolyte membrane fuel cells fuelled with hydrogen (pefc) and methanol (dmfc) and for h2 electrogenerators |
CN102702807A (en) * | 2012-06-14 | 2012-10-03 | 金华氟特催化科技有限公司 | Photo-catalytic composite coating and preparation method thereof |
CN105964248A (en) * | 2016-05-09 | 2016-09-28 | 深圳市文浩科技有限公司 | Preparation method of coal ash microsphere loaded modified nanometer titanium dioxide composite photocatalyst |
CN108855059A (en) * | 2018-07-09 | 2018-11-23 | 武汉科技大学 | A kind of fly ash float load silver oxide composite photo-catalyst and preparation method thereof |
CN109304476A (en) * | 2017-07-28 | 2019-02-05 | 中国石油化工股份有限公司 | Carbon coating transition metal nanocomposite and its preparation method and application |
-
2019
- 2019-04-03 CN CN201910267025.0A patent/CN109985651A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH07284664A (en) * | 1994-04-20 | 1995-10-31 | Riken Corp | Waste gas purification material and method for purifying waste gas |
EP2064765A2 (en) * | 2006-04-18 | 2009-06-03 | Universita Degli Studi Di Padova | Electrocatalysts based on mono/plurimetallic carbon nitrides for polymer electrolyte membrane fuel cells fuelled with hydrogen (pefc) and methanol (dmfc) and for h2 electrogenerators |
CN102702807A (en) * | 2012-06-14 | 2012-10-03 | 金华氟特催化科技有限公司 | Photo-catalytic composite coating and preparation method thereof |
CN105964248A (en) * | 2016-05-09 | 2016-09-28 | 深圳市文浩科技有限公司 | Preparation method of coal ash microsphere loaded modified nanometer titanium dioxide composite photocatalyst |
CN109304476A (en) * | 2017-07-28 | 2019-02-05 | 中国石油化工股份有限公司 | Carbon coating transition metal nanocomposite and its preparation method and application |
CN108855059A (en) * | 2018-07-09 | 2018-11-23 | 武汉科技大学 | A kind of fly ash float load silver oxide composite photo-catalyst and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
HAI-TAO REN 等: "Improved Photochemical Reactivities of Ag2O/g‑C3N4 in Phenol Degradation under UV and Visible Light", 《INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115041212A (en) * | 2022-06-17 | 2022-09-13 | 河北农业大学 | Silver chloride-carbon nitride composite photocatalyst and preparation method and application thereof |
CN115041212B (en) * | 2022-06-17 | 2023-07-28 | 河北农业大学 | Silver chloride-carbon nitride composite photocatalyst and preparation method and application thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105709793B (en) | Niobium pentoxide nano stick/nitrogen-doped graphene composite photo-catalyst, preparation method and application of cadmium sulfide nano-particles modification | |
CN107233909A (en) | A kind of preparation method and its usage of SrNb2 O6/nitridation carbon composite nano-material | |
CN108355669B (en) | Magnetic nano onion carbon loaded Bi2WO6Photocatalyst and preparation method and application thereof | |
CN108479816A (en) | A kind of preparation method of high-effect iodine vacancy bismuth oxygen iodine catalysis material and the application in poisoning treatment of Organic Wastewater | |
CN108671955B (en) | Composite catalyst for photolysis of aquatic hydrogen and preparation method thereof | |
CN106622293B (en) | A kind of H-TiO2/CdS/Cu2-xThe preparation method of S nanobelt | |
CN109126854A (en) | A kind of CdS/g-C3N4The preparation method of double nano piece composite photo-catalyst | |
CN110639620A (en) | Composite photocatalyst for degrading tetracycline and preparation method and application thereof | |
CN103861618A (en) | Preparation method for SnO2-based composite visible light photocatalyst | |
CN106391062A (en) | BiVO4/BiOCl heterojunction photocatalyst and preparation method thereof | |
CN108421551A (en) | A kind of CdIn2S4Nano dot hydridization TiO2Hollow ball composite photo-catalyst and its preparation method and application | |
CN111330602A (en) | Carbon cloth loaded BiOCl/BiVO4Recyclable flexible composite photocatalytic material, preparation method and application | |
CN108772091A (en) | One kind being used for CO2It is catalyzed heterojunction photocatalyst and its preparation of reduction | |
CN109847780A (en) | A kind of AgBr/BiOI/g-C3N4The preparation method and applications of tri compound catalysis material | |
CN107126945A (en) | A kind of TiO2Mixed crystal nano-rod assembly photochemical catalyst and preparation method thereof | |
CN107098429A (en) | A kind of BiVO4/BiPO4Composite and its preparation method and application | |
CN105817244B (en) | A kind of AgI/ β Bi2O3‑Bi2O2CO3Photochemical catalyst and its preparation method and application | |
CN105771953A (en) | Preparation method of zinc titanate and titanium dioxide composite nano material | |
CN109985651A (en) | A kind of graphite phase carbon nitride/silver oxide composite photo-catalyst and preparation method thereof | |
CN108607580B (en) | Indium sulfide/indium vanadate composite photocatalyst and preparation method and application thereof | |
CN106732587B (en) | A kind of preparation method of the ZnO polycrystal nanobelt package assembly of high H2-producing capacity atomic state Ag modification | |
CN107349951A (en) | A kind of CuO/g C3N4The preparation method of blood capillary tubulose nano-complex | |
CN114849789B (en) | Preparation method and application of MIL-125 supported 1T-phase molybdenum sulfide composite photocatalyst | |
CN109569569A (en) | A kind of photochemical catalyst and its preparation method and application with ternary heterojunction structure | |
CN108855192A (en) | Load the preparation method of bismuth molybdate nitrogen defect nitridation carbon composite photocatalyst |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190709 |