CN110102324A - A kind of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst and its preparation method and application - Google Patents
A kind of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst and its preparation method and application Download PDFInfo
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- CN110102324A CN110102324A CN201910233235.8A CN201910233235A CN110102324A CN 110102324 A CN110102324 A CN 110102324A CN 201910233235 A CN201910233235 A CN 201910233235A CN 110102324 A CN110102324 A CN 110102324A
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- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 title claims abstract description 43
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 title claims abstract description 39
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910001958 silver carbonate Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 29
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 28
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 25
- 238000013019 agitation Methods 0.000 claims abstract description 20
- KQTXIZHBFFWWFW-UHFFFAOYSA-L silver(I) carbonate Inorganic materials [Ag]OC(=O)O[Ag] KQTXIZHBFFWWFW-UHFFFAOYSA-L 0.000 claims abstract description 16
- WIKQEUJFZPCFNJ-UHFFFAOYSA-N carbonic acid;silver Chemical compound [Ag].[Ag].OC(O)=O WIKQEUJFZPCFNJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000474 mercury oxide Inorganic materials 0.000 claims abstract description 11
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 claims abstract description 11
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims description 44
- 229910021641 deionized water Inorganic materials 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000002604 ultrasonography Methods 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 10
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 8
- 239000001099 ammonium carbonate Substances 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 15
- 238000006555 catalytic reaction Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000002351 wastewater Substances 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 238000000926 separation method Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000004108 freeze drying Methods 0.000 description 3
- 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 3
- 229940043267 rhodamine b Drugs 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000011218 binary composite Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 2
- 235000019799 monosodium phosphate Nutrition 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 2
- 229910000161 silver phosphate Inorganic materials 0.000 description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 2
- 241000931705 Cicada Species 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 polyethylene pyrrole Pyrrolidone Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229940019931 silver phosphate Drugs 0.000 description 1
- UGWRVHSFESMVND-UHFFFAOYSA-N silver;ethane-1,2-diol;nitrate Chemical compound [Ag+].OCCO.[O-][N+]([O-])=O UGWRVHSFESMVND-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
-
- 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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
Abstract
The invention belongs to catalysis material technical field, a kind of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst and its preparation method and application is disclosed.The Three-element composite photocatalyst Ag2CO3/ AgBr/GO is that graphene oxide solution is added drop-wise in silver nitrate solution, then ultrasonic in darkroom to obtain solution B；Then carbonate is added in CTAB solution, magnetic agitation makes it dissolve to obtain solution C；Solution C is added dropwise in solution B in darkroom again, obtains yellow mercury oxide, after washed and centrifugal treating, is freeze-dried and is made in the case where vacuum degree is 35~45MPa.The method of the present invention simple process, gained tri compound catalysis material photocatalytic activity with higher and stability, degradable organic pollutant it is high-efficient, have good application prospect in treatment of Organic Wastewater.
Description
Technical field
The invention belongs to catalysis material technical fields, more particularly, to a kind of new and effective silver carbonate (Ag2CO3)/
Silver bromide (AgBr)/GO Three-element composite photocatalyst and its preparation method and application.
Background technique
With the rapid development of industry, environmental pollution has become one of the serious problems that we must solve in recent years.It is special
It is not that some organic dyestuff are widely used in our daily chemical industry.Waste water containing these organic dyestuff will lead to sternly
The environmental pollution of weight.Photocatalysis has proved to be a kind of side that can efficiently use the organic pollutant in solar energy degrading waste water
Method.However, traditional semiconductor light-catalyst such as TiO2It can only be by ultraviolet excitation with ZnO etc..It is well known that ultraviolet light only accounts for
4% or so of sunlight, well below the ratio (45%) of visible light.Therefore, there is an urgent need to develop with high activity and well
The visible light-responded photochemical catalyst of stability.
In recent years, a series of Ag based photocatalyst such as Ag3PO4And Ag2CO3Deng organic contamination of degrading under visible light illumination
Excellent photocatalytic activity is shown when object.However, these Ag based photocatalysts are easy to happen light during light-catalyzed reaction
Corrosion, reduces photocatalytic activity and photostability.For example, application No. is the Chinese invention patents of CN201010561326.3
" preparation method and applications of visible-light photocatalyst silver and silver orthophosphate ", preparation method take sodium dihydrogen phosphate, polyethylene pyrrole
Pyrrolidone is dissolved in ethylene glycol, is put in water-bath, and magnetic agitation takes silver nitrate to be dissolved in ethylene glycol.By silver nitrate
Ethylene glycol solution is added drop-wise in the ethylene glycol solution of sodium dihydrogen phosphate and polyvinylpyrrolidone, 60 DEG C of constant temperature stirrings.By phosphoric acid
Silver-colored solution moves into magnetic agitation in 160 DEG C of oil baths, washs after reaction silver-colored and silver phosphate catalyst.Though above-mentioned preparation method
Photocatalytic activity is so improved to a certain extent, and still, preparation process is complex, has used more organic solvent.
For another example application No. is the Chinese invention patent of CN201410517383.X " preparation method of visible light catalyst silver carbonate ", systems
Preparation Method is to take soluble silver salt and carbonate that carbon is prepared using ion exchange coprecipitation or hydro-thermal method for reactant
Sour silver precipitating, using filter, washing, it is dry after silver carbonate photochemical catalyst can be obtained.Although the silver carbonate tool of this method preparation
There is preferable visible light photocatalysis active, but single silver carbonate catalysis material is easy to happen photoetch, stability is not high.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art and disadvantage, a kind of new and effective Ag is provided2CO3/ AgBr/GO tri-
First composite photo-catalyst.Composite photo-catalyst photocatalytic activity with higher and stability.
Another object of the present invention is to provide above-mentioned new and effective Ag2CO3The preparation of/AgBr/GO Three-element composite photocatalyst
Method.
Still a further object of the present invention is to provide above-mentioned new and effective Ag2CO3/ AgBr/GO Three-element composite photocatalyst is answered
With.
The purpose of the present invention is realized by following technical proposals:
A kind of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst, the Three-element composite photocatalyst
Ag2CO3/ AgBr/GO is that graphene oxide solution is added drop-wise in silver nitrate solution, then ultrasonic in darkroom to obtain solution B；So
Carbonate is added in CTAB solution afterwards, magnetic agitation makes it dissolve to obtain solution C；Solution C is added dropwise in darkroom again
Into solution B, yellow mercury oxide is obtained, after washed and centrifugal treating, be freeze-dried and be made in the case where vacuum degree is 35~45MPa.
Preferably, the volume ratio of the quality and deionized water of graphene oxide is (1~2) in the graphene oxide solution
G:(0.5~1) × 105mL。
Preferably, in the silver nitrate solution silver nitrate mole and deionized water volume be (3~6) mmol:(40~
60)ml；The graphene oxide solution and the volume ratio of silver nitrate solution are (5~10): (40~60)；The time of the ultrasound
For 20~30min.
Preferably, in the CTAB solution cetyl trimethylammonium bromide mole and the volume ratio of deionized water be
(0.05~2) mmoL:(40~60) ml；The carbonate mole and CTAB solution volume ratio be (2~4) mmoL:(40~
60)ml。
Preferably, the carbonate is one or more of ammonium hydrogen carbonate, ammonium carbonate or sodium carbonate.
Preferably, the washing is ethyl alcohol and deionized water with agent；The rate of the centrifugation is 8000~10000rpm/
min；The temperature of the freeze-drying is -40~-46 DEG C.
The preparation method of the new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst, including it is following specific
Step:
S1. in the deionized water A for taking graphene oxide to be added to, evenly dispersed solution A is made in abundant ultrasound, takes solution A
It is added to ultrasound in deionized water B, graphene oxide solution is made；
S2. graphene oxide solution is added drop-wise in silver nitrate solution, it is then ultrasonic in darkroom, obtain solution B；
S3. carbonate, the uniform solution C that magnetic agitation makes it dissolve are added in CTAB solution；
S4. solution C is added dropwise in solution B in darkroom, obtains yellow mercury oxide；Simultaneously with ethyl alcohol and deionization washing
Centrifugation is freeze-dried in the case where vacuum degree is 35~45MPa, Ag is made2CO3/AgBr/GO。
Preferably, the quality of graphene oxide described in step S1 and the volume ratio of deionized water A are (0.01~0.02)
G:(50~100) mL；The solution A and the volume ratio of deionized water B are (1~3): (10~20).
Preferably, the time ultrasonic described in step S1 is 2~4h.
New and effective silver carbonate/silver bromide/the application of the GO Three-element composite photocatalyst in photocatalysis field.
Compared with prior art, the invention has the following advantages:
1. new and effective Ag prepared by the present invention2CO3/ AgBr/GO Three-element composite photocatalyst has given full play to graphite oxide
The synergistic effect of alkene and silver carbonate not only promotes the separation of photo-generate electron-hole pair and effectively improves light-catalysed performance,
And less organic solvent is only used, method and process is simple, high-efficient, the suitable large-scale production of degradable organic pollutant.
2. new and effective Ag of the invention2CO3It is living that/AgBr/GO tri compound catalysis material shows higher photocatalysis
Property and stability, there is good application prospect in treatment of Organic Wastewater.
Detailed description of the invention
Fig. 1 is new and effective Ag made from embodiment 12CO3The scanning electron microscope of/AgBr/GO tri compound catalysis material
Figure.
Fig. 2 is new and effective Ag made from embodiment 12CO3/ AgBr/GO tri compound catalysis material and comparative example 1-3
Binary composite photocatalyst material obtained rhodamine B degradation figure light degradation rate curve under visible light.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. 0.01g graphene oxide is taken to be added in the deionized water of 50mL, sufficiently ultrasound is made evenly dispersed molten for 4 hours
Liquid takes the above-mentioned solution of 1mL to be added to ultrasound 4 hours in 19mL deionized water, evenly dispersed solution is made.
2. 6mmoL silver nitrate is taken to be added in the deionized water of 40mL, magnetic agitation keeps silver nitrate completely molten in darkroom
Solution.
3. taking the graphene oxide solution in 7.5mL step 1, it is added dropwise in silver nitrate solution, then in darkroom
Ultrasonic 30min.
4. 1mmoL cetyl trimethylammonium bromide (CTAB) is taken to be added in the deionized water of 40mL, heated at 40 DEG C
Stirring, dissolves it sufficiently.
5. the ammonium hydrogen carbonate of 3mmoL, the uniform solution that magnetic agitation makes it dissolve are added in CTAB solution.
6. the solution of step 5 is added dropwise in darkroom in the solution of step 3, yellow mercury oxide sample is obtained.
7. then precipitation and centrifugal separation (rate 8000rpm/min) prepared by step 6 is successively used ethyl alcohol and deionized water
It washes three times and is centrifuged, at -40 DEG C of condensation temperature, vacuum degree is that 35MPa is freeze-dried, and obtains Ag2CO3/AgBr/GO。
Fig. 1 is new and effective Ag made from the present embodiment2CO3The scanning electron microscope of/AgBr/GO tri compound catalysis material
Figure.As can be known from Fig. 1, the graphene oxide of cicada's wings shape is supported on very well on rodlike silver carbonate and silver bromide；Illustrate Ag2CO3/
AgBr/GO tri compound catalysis material successfully prepares.Fig. 2 is new and effective Ag made from the present embodiment2CO3/
Binary composite photocatalyst material made from AgBr/GO tri compound catalysis material and comparative example 1-3 is degraded sieve under visible light
Red bright B figure light degradation rate curve.From comparing in Fig. 2 it is found that in the rhodamine B degradation solution of same concentrations and volume
Ag2CO3/ AgBr/GO tri compound catalysis material rhodamine B degradation the used time is most short, and rate is most fast.Illustrate Ag2CO3/AgBr/
GO tri compound catalysis material is compared to Ag in the comparative example 1-3 prepared under the same terms2CO3/AgBr、Ag2CO3/ GO and
AgBr/GO binary catalysis material has higher photocatalytic activity and stability.
Embodiment 2
1. 0.01g graphene oxide is taken to be added in the deionized water of 50mL, sufficiently ultrasound is made evenly dispersed molten for 4 hours
Liquid takes the above-mentioned solution of 1mL to be added to ultrasound 4 hours in 19mL deionized water, evenly dispersed solution is made.
2. 1.0192g silver nitrate is taken to be added in the deionized water of 40mL, magnetic agitation keeps silver nitrate complete in darkroom
Dissolution.
3. taking the graphene oxide solution in 7.5mL step 1, it is added dropwise in silver nitrate solution, then in darkroom
Ultrasonic 30min.
4. 0.3644g cetyl trimethylammonium bromide (CTAB) is taken to be added in the deionized water of 40mL, add at 40 DEG C
Thermal agitation dissolves it sufficiently.
5. the ammonium carbonate of 0.2882g, the uniform solution that magnetic agitation makes it dissolve are added in CTAB solution.
6. step 5 solution is added dropwise in 3 solution in darkroom, yellow mercury oxide sample is obtained.
7. then precipitation and centrifugal separation (rate 8000rpm/min) prepared by step 6 is successively used ethyl alcohol and deionized water
It washes three times and is centrifuged, at -40 DEG C of condensation temperature, vacuum degree is that 35MPa is freeze-dried, and obtains Ag2CO3/AgBr/GO。
Embodiment 3
1. 0.01g graphene oxide is taken to be added in the deionized water of 50mL, sufficiently ultrasound is made evenly dispersed molten for 4 hours
Liquid takes the above-mentioned solution of 1mL to be added to ultrasound 4 hours in 19mL deionized water, evenly dispersed solution is made.
2. 1.0192g silver nitrate is taken to be added in the deionized water of 40mL, magnetic agitation keeps silver nitrate complete in darkroom
Dissolution.
3. taking the graphene oxide solution in 7.5mL step 1, it is added dropwise in silver nitrate solution, then in darkroom
Ultrasonic 30min.
4. 0.3644g cetyl trimethylammonium bromide (CTAB) is taken to be added in the deionized water of 40mL, add at 40 DEG C
Thermal agitation dissolves it sufficiently.
5. the sodium carbonate of 0.3180g, the uniform solution that magnetic agitation makes it dissolve are added in CTAB solution.
6. step 5 solution is added dropwise in 3 solution in darkroom, yellow mercury oxide sample is obtained.
7. then precipitation and centrifugal separation (rate 8000rpm/min) prepared by step 6 is successively used ethyl alcohol and deionized water
It washes three times and is centrifuged, at -40 DEG C of condensation temperature, vacuum degree is the freeze-drying of 35MPa row, obtains Ag2CO3/AgBr/GO。
Comparative example 1
1. 6mmoL silver nitrate is taken to be added in the deionized water of 40mL, magnetic agitation keeps silver nitrate completely molten in darkroom
Solution.
2. 1mmoL cetyl trimethylammonium bromide (CTAB) is taken to be added in the deionized water of 40mL, heated at 40 DEG C
Stirring, dissolves it sufficiently.
3. the ammonium hydrogen carbonate of 3mmoL, the uniform solution that magnetic agitation makes it dissolve are added in CTAB solution.
4. step 3 solution is added dropwise in darkroom in the solution of step 1, yellow mercury oxide sample is obtained.
5. then precipitation and centrifugal separation (rate 8000rpm/min) prepared by step 4 is successively used ethyl alcohol and deionized water
It washes three times and is centrifuged, at -40 DEG C of condensation temperature, vacuum degree is that 35MPa is freeze-dried, and obtains Ag2CO3/AgBr。
Comparative example 2
1. 0.01g graphene oxide is taken to be added in the deionized water of 50mL, sufficiently ultrasound is made evenly dispersed molten for 4 hours
Liquid takes the above-mentioned solution of 1mL to be added to ultrasound 4 hours in 19mL deionized water, evenly dispersed solution is made.
2. 6mmoL silver nitrate is taken to be added in the deionized water of 40mL, magnetic agitation keeps silver nitrate completely molten in darkroom
Solution.
3. taking the graphene oxide solution in 7.5mL step 1, it is added dropwise in silver nitrate solution, then in darkroom
Ultrasonic 30min.
4. the ammonium hydrogen carbonate of 3mmoL is taken to be added in the deionized water of 40mL, in 40 DEG C of heating stirrings, keep it sufficiently molten
Solution.
5. solution in step 4 is added dropwise in step 3 solution in darkroom, yellow mercury oxide sample is obtained.
7. then precipitation and centrifugal separation (rate 8000rpm/min) prepared by step 6 is successively used ethyl alcohol and deionized water
It washes three times and is centrifuged, at -40 DEG C of condensation temperature, vacuum degree is that 35MPa is freeze-dried, and obtains Ag2CO3/GO。
Comparative example 3
1. 0.01g graphene oxide is taken to be added in the deionized water of 50mL, sufficiently ultrasound is made evenly dispersed molten for 4 hours
Liquid takes the above-mentioned solution of 1mL to be added to ultrasound 4 hours in 19mL deionized water, evenly dispersed solution is made.
2. 1.0192g silver nitrate is taken to be added in the deionized water of 40mL, magnetic agitation keeps silver nitrate complete in darkroom
Dissolution.
3. taking the graphene oxide solution in 7.5mL step 1, it is added dropwise in silver nitrate solution, then in darkroom
Ultrasonic 30min.
4. 0.3644g cetyl trimethylammonium bromide (CTAB) is taken to be added in the deionized water of 40mL, add at 40 DEG C
Thermal agitation dissolves it sufficiently.
5. step 4 solution is added dropwise in darkroom in the solution of step 3, yellow mercury oxide sample is obtained.
6. then precipitation and centrifugal separation (rate 8000rpm/min) prepared by step 5 is successively used ethyl alcohol and deionized water
It washes three times and is centrifuged, at -40 DEG C of condensation temperature, vacuum degree is the freeze-drying of 35MPa row, obtains AgBr/GO.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst, which is characterized in that the tri compound light
Catalyst Ag2CO3/ AgBr/GO is that graphene oxide solution is added drop-wise in silver nitrate solution, then moltenly ultrasonic in darkroom
Liquid B；Then carbonate is added in CTAB solution, magnetic agitation makes it dissolve to obtain solution C；Again by solution C in darkroom by
It is added dropwise in solution B, obtains yellow mercury oxide, after washed and centrifugal treating, be freeze-dried in the case where vacuum degree is 35~45MPa
It is made.
2. new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 1, which is characterized in that
The volume ratio of the quality and deionized water of graphene oxide is (1~2) g:(0.5~1 in the graphene oxide solution) ×
105mL。
3. new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 1, which is characterized in that
In the silver nitrate solution silver nitrate mole and deionized water volume be (3~6) mmol:(40~60) ml；The oxidation
The volume ratio of graphene solution and silver nitrate solution is (5~10): (40~60)；The time of the ultrasound is 20~30min.
4. new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 1, which is characterized in that
In the CTAB solution cetyl trimethylammonium bromide mole and deionized water volume ratio be (0.05~2) mmoL:(40
~60) ml；The carbonate mole and CTAB solution volume ratio be (2~4) mmoL:(40~60) ml.
5. new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 1, which is characterized in that
The carbonate is one or more of ammonium hydrogen carbonate, ammonium carbonate or sodium carbonate.
6. new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 1, which is characterized in that
The washing is ethyl alcohol and deionized water with agent；The rate of the centrifugation is 8000~10000rpm/min；The freezing is dry
Dry temperature is -40~-46 DEG C.
7. the system of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 1-6
Preparation Method, which is characterized in that comprise the following specific steps that:
S1. in the deionized water A for taking graphene oxide to be added to, evenly dispersed solution A is made in abundant ultrasound, and solution A is taken to be added
It is ultrasonic into deionized water B, graphene oxide solution is made；
S2. graphene oxide solution is added drop-wise in silver nitrate solution, it is then ultrasonic in darkroom, obtain solution B；
S3. carbonate, the uniform solution C that magnetic agitation makes it dissolve are added in CTAB solution；
S4. solution C is added dropwise in solution B in darkroom, obtains yellow mercury oxide；With ethyl alcohol and deionization washing and from
The heart is freeze-dried in the case where vacuum degree is 35~45MPa, Ag is made2CO3/AgBr/GO。
8. the preparation method of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 7,
It is characterized in that, the quality of graphene oxide described in step S1 and the volume ratio of deionized water A are (0.01~0.02) g:(50
~100) mL；The solution A and the volume ratio of deionized water B are (1~3): (10~20).
9. the preparation method of new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst according to claim 7,
It is characterized in that, the time ultrasonic described in step S1 is 2~4h.
10. new and effective silver carbonate/silver bromide/GO Three-element composite photocatalyst described in any one of claims 1-6 is urged in light
Application in change field.
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