CN104096578A - Preparation method for an Ag/AgBr/GO nano-composite photocatalyst - Google Patents
Preparation method for an Ag/AgBr/GO nano-composite photocatalyst Download PDFInfo
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Abstract
The invention discloses a preparation method for an Ag/AgBr/GO nano-composite photocatalyst containing graphene oxide (GO), and belongs to the field of photocatalysts. Active components of the Ag/AgBr/GO nano-composite photocatalyst are Ag/AgBr/GO; the structure is that Ag/AgBr colloidal spheres are uniformly distributed on the layer-shaped GO. The preparation method is simple, and is fulfilled according to an one-step method; PVP and CTAB are adopted as surfactants; the CTAB is source of the BR<-> at the same time; first, the PVP and the CTAB are dissolved in glycol at a certain temperature; the GO and AgNO3 are added; reaction is conducted at 155 DEG C for 15 min to obtain the Ag/AgBr/GO nano-composite material. The prepared Ag/AgBr/GO nano-composite material is adopted as a photocatalyst, is used for light degradation of rhodamine, and acquires excellent catalyzed effect; meanwhile, the catalyst shows favorable stability.
Description
Technical field
The invention belongs to photochemical catalyst field, be specifically related to the technology of preparing of the photochemical catalyst Ag/AgBr/GO nano composite material that one contains graphene oxide (GO), particularly the technology of preparing of the controlled Ag/AgBr/GO nano composite material of a kind of pattern and composition.It is photochemical catalyst that the present invention closes prepared Ag/AgBr/GO nano composite material, obtains good catalytic effect for light degradation rhodamine.
Background technology
The controlled many components hybrid material of pattern and composition all has great potential using value (P.Li in fields such as catalysis, solar energy conversion and photoelectric technologies, et al.Au-ZnO Hybrid Nanopyramids and Their Photocatalytic Properties, J.Am.Chem.Soc.2011,133,5660-5663; T.Yu, et al.AqueousPhase Synthesis of Pt/CeO
2hybrid Nanostructures and Their Catalytic Properties, Adv.Mater.2010,22,5188-5192.).Graphene is one of important material with carbon element, has much good character, and for example specific area is large, and heat endurance is high, and conductive capability is strong etc., is widely used in the various fields including photocatalysis.GO prepares the important presoma of Graphene, has identical two dimensional surface monoatomic layer structure with Graphene, and difference is to have a lot of oxy radicals (OH ,-COOH ,-O-, C=O) on GO surface.These oxy radicals give Graphene some new features, for example good water-soluble, this is conducive to further grapheme modified (X.An, et al., Graphene-based photocatalytic composit es, RSC Adv., 1 (2011) 1426-1434.D.R.Dreyer, et al., The chemistry of graphene oxide, Chem.Soc.Rev., 39 (2010) 228-240.).Conductor photocatalysis material has advantages of outstanding aspect environmental protection, aspect depollution of environment processing, there is very strong potential using value (M.N.Chong, et al.Recent developments in photocatalytic water treatment technology:a review, Water Res.44 (2010) 2997-3027.P.Gao, et al.Sulfonated graphene oxide-ZnO-Ag photocatalyst for fast photodegradation and disinfection under visible light, J Hazard Mater.262 (2013) 826-835.C.Chen, et al.Nanoporous Nitrogen-Doped Titanium Dioxide with Excellent Photocatalytic Activity under Visible Light Irradiation Produced by Molecular Layer Deposition, Angew.Chem.Int.Ed., 52 (2013) 9196-9200.).And Ag/AgX hybrid material wherein especially comes into one's own, although AgX is light-sensitive material, Ag/AgX hybrid systems has certain stability, the light wavelength wide ranges that Ag/AgX absorbs, can improve the utilization rate of sunshine, Ag/AgX has very high photocatalytic activity.(R.Dong, et al.Ecofriendly Synthesis and Photocatalytic Activity of Uniform Cubic Ag@AgCl Plasmonic Photocatalyst J.Phys.Chem.C, 117 (2013) 213-220.J.Song, et al.Fabrication of Ag-coated AgBr nanoparticles and their plasmonic photocatalytic applications, RSC Adv., 4 (2014) 4558-4563.M.Zhu, et al.Graphene Oxide Enwrapped Ag/AgX (X=Br, Cl) Nanocomposite as a Highly Efficient Visible-Light Plasmonic Photocatalyst.ACS Nano, silver/the silver halides such as 5 (2011) 4529-4536. Zhu Ming mountains: a class novel plasma photochemical catalyst, chemical progress, 25 (2013), 209-220.).In Ag/AgX composite, introduce GO, can further improve its photocatalysis performance.Ag/AgX produces electronics and hole under illumination condition, due to the electric conductivity of GO, can promote electric charge to separate with hole; In addition, adding of GO can make its composite increase the absorption to organic dyestuff, thereby improves catalytic effect silver/silver halides such as (: a class novel plasma photochemical catalyst, chemical progress, 25 (2013), 209-220.) Zhu Mingshan.
Although it is varied to prepare the method for Ag/AgX/GO nano composite material, how to prepare easily pattern and form controlled Ag/AgBr/GO nano composite material remaining a technological difficulties.For many years, people are devoted to study preparation method and the principle of such material always.The bibliographical information approaching with this patent has: the people such as Zhu (M.Zhu, et al.Ag/AgBr/Graphene Oxide Nanocomposite Synthesized via Oil/Water and Water/Oil Microemulsions:A Comparison of Sunlight Energized Plasmonic Photocatalytic Activity.Langmuir, 28 (2012) 3385-3390.) prepare Ag/AgBr/GO nano composite material with microemulsion method.The people such as people and Zhang such as Wang (J.Wang, et al., Graphene oxide coupled AgBr nanosheets:an efficient dual-functional visible-light-responsive nanophotocatalyst with enhanced performance, J.Mater.Chem.A, 2013, 1, 2827-2832.H.Zhang, et al., Graphene Sheets Grafted Ag@AgCl Hybrid with Enhanced Plasmonic Photocatalytic Activity under Visible Light, Environ.Sci.Technol., 45 (2011) 5731-5736.) prepare Ag@AgCl/GO hybrid material with solvent-thermal method.It is more loaded down with trivial details comparatively speaking that microemulsion method is prepared Ag/AgBr/GO nano composite material, the people such as Wang are the Ag/AgBr/GO nano composite materials of the sheet of preparation, Ag@AgCl/GO nano composite material and the people such as Zhang prepare by solwution method, using hydrochloric acid as chlorine source, do not use surfactant yet.And Dual Surfactants legal system of the present invention has no report for Ag/AgBr/GO nano composite material.
Summary of the invention
The object of the invention is to provide a kind of pattern and forms the preparation method of controlled Ag/AgBr/GO nano composite material, obtains good effect to the Ag/AgBr/GO nano composite material of preparing with the present invention as photocatalyst for degrading rhodamine.
In order to realize above-mentioned technical purpose, the present invention is achieved by the following technical programs.
The invention provides a kind of Ag/AgBr/GO nano composite material, its active component is Ag/AgBr/GO, and its structure is that Ag/AgBr colloidal spheres is evenly distributed in stratiform GO above, and the particle diameter of Ag/AgBr is 100～900nm, and its concrete preparation process is as follows:
0.5g graphite powder and 1.5g KMnO
4join in the round-bottomed flask that the 12mL concentrated sulfuric acid is housed, ice-water bath condition lower magnetic force stirs 4h, is heated to 35 DEG C, constant temperature stirs 30min, dropwise adds 23mL distilled water, is warming up to 98 DEG C, stir 15min, this mixture is transferred in ice-water bath, add 70mL distilled water diluting, add again the hydrogen peroxide of 10mL 30%, stir 30min, solution becomes yellow, centrifugation, fully wash to till supernatant liquor pH=7, lower sediment thing is drying to obtain to GO.
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60～120 DEG C, constant temperature stirs 30min, add 54～150mg polyvinylpyrrolidone (PVP) and 100～160mg softex kw (CTAB), continue to stir until the two dissolves completely, then the GO that adds 3～10mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 80～150mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is risen to 155 DEG C, keep 15min, reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
By adjusting initial reaction temperature, AgNO
3, GO, PVP and CTAB the preparation condition such as consumption can control pattern and the composition of Ag/AgBr/GO nano composite material.When initial reaction temperature is 60 DEG C, AgNO
3, GO, PVP and CTAB consumption while being respectively 100mg, 5mg, 95mg and 120mg, it is upper that Ag/AgBr colloidal spheres is dispersed in stratiform GO uniformly, Ag/AgBr colloidal spheres diameter is wherein between 300～400nm.
Ag/AgBr/GO nano composite material prepared by the present invention can be used as photochemical catalyst when degrading rhodamine, has shown good catalytic effect.When the prepared Ag/AgBr/GO nano-composite catalyst of the present invention is used for light degradation rhodamine, reaction condition is: concentration is 10mg mL
-1rhodamine aqueous solution 20mL, catalyst amount is 30mg, sunshine is as light source, when irradiation time is 40min, the degradation rate of rhodamine is 93%, in the time that light application time is 60min, degradation rate reaches 97%, and when light application time is 120min, degradation rate reaches 98%.In addition, this catalyst also has good stability, the above-mentioned rhodamine aqueous solution of catalytic degradation, and continuous circulation 6 times, degradation rate still can reach 83%.
Compared with prior art, the present invention has following technical advantage:
(1) the adding of GO in catalyst preparation process, can promote the formation of the Ag/AgBr colloidal spheres of good dispersion, particle size homogeneous;
In preparation Ag/AgBr/GO nano composite material process, find, GO also has the effect of surfactant.Add GO compared with not adding GO, dispersiveness and the homogeneity of Ag/AgBr colloidal spheres significantly improve.
(2) preparation process of catalyst is simple;
Ag/AgBr/GO Nano-composite materials process is simple, adopts one-step method to complete.Taking PVP and CTAB as surfactant, meanwhile, CTAB is also Br
-source, make first at a certain temperature the two be dissolved in ethylene glycol, add GO and it fully disperseed, then add AgNO
3, 155 DEG C of reaction 15min, just obtain Ag/AgBr/GO nano composite material.
(3) catalytic efficiency of catalyst is high;
Relatively typical photochemical catalyst TiO
2, light absorbing wave-length coverage increases, and has improved the utilization rate of sunshine.For the reaction of degraded rhodamine, in the time that catalyst amount is 30mg, sunshine is as light source, and when irradiation time is 40min, the degradation rate of rhodamine reaches 93%.
(4) catalytic stability of catalyst is good;
The catalytic degradation rhodamine aqueous solution, continuous circulation 6 times, degradation rate still can reach 83%.
Brief description of the drawings
Fig. 1 is the stereoscan photograph of the prepared Ag/AgBr/GO nano composite material of the embodiment of the present invention 2;
As can be seen from Figure 1, it is upper that Ag/AgBr colloidal spheres is evenly distributed in stratiform GO, and the diameter of colloidal spheres is 300～400nm.
Fig. 2 is the FTIR curve map of the prepared Ag/AgBr/GO nano composite material of the embodiment of the present invention 2 and pure GO;
Can find out from the FTIR curve of GO: 3400cm
-1the broad peak at place is the stretching vibration peak of O – H, 1376cm
-1and 1222cm
-1the peak at place is respectively the stretching vibration peak of C – OH and C – O – C, 1056cm
-1the peak at place is C-O vibrations peaks, shows to exist at the epoxide group that has between layers of GO 1615cm
-1the peak at place is the hydrone of absorption and the vibration peak (T.Yang of unoxidized graphite powder, et al., Cyanobacterium metallothionein decorated graphene oxide nanosheets for highly selective adsorption of ultra-trace cadmium, J.Mater.Chem.22 (2012) 21909-21916.M.Hilder, et al., Graphene/zinc nano-composites by electrochemical co-deposition.Phys.Chem.Chem.Phys.14 (2012) 14034-14040.).Relatively the FTIR curve of Ag/AgBr/GO nano composite material can be found, the carbonyl absorption peak on GO is by original 1716cm
-1place is displaced to 1735cm
-1place, this shows that interaction (J.Petroski has occurred for Ag/AgBr and GO sheet, et al., FTIR Study of the Adsorption of the Capping Material to Different Platinum Nanoparticle Shapes.J.Phys.Chem.A, 107 (2003) 8371-8375.P.Yang, et al., Hydrogenation of Nitrobenzenes Catalyzed by Platinum Nanoparticle Core-Polyaryl Ether Trisacetic Acid Ammonium Chloride Dendrimer Shell Nanocomposite.J.Mol.Catal.A, 260 (2006) 4-10.).
Detailed description of the invention
Below by example, feature of the present invention is described further, but the present invention is not limited to following embodiment.
One, the preparation of Ag/AgBr/GO nano composite material
Embodiment 1
The concrete preparation process of 1#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
0.5g graphite powder and 1.5g KMnO
4join in the round-bottomed flask that the 12mL concentrated sulfuric acid is housed, ice-water bath condition lower magnetic force stirs 4h, is heated to 35 DEG C, constant temperature stirs 30min, dropwise adds 23mL distilled water, is warming up to 98 DEG C, stir 15min, this mixture is transferred in ice-water bath, add 70mL distilled water diluting, add again the hydrogen peroxide of 10mL 30%, stir 30min, solution becomes yellow, centrifugation, fully wash to till supernatant liquor pH=7, lower sediment thing is drying to obtain to GO.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 54mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 2
The concrete preparation process of 2#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried, and its stereoscan photograph is as shown in Figure 1.
Embodiment 3
The concrete preparation process of 3#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 150mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 4
The concrete preparation process of 4#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 90 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 5
The concrete preparation process of 5#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 120 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, and stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 6
The concrete preparation process of 6#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 100mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 7
The concrete preparation process of 7#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 160mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 8
The concrete preparation process of 8#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 3mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 9
The concrete preparation process of 9#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 10mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 100mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 10
The concrete preparation process of 10#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 80mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 11
The concrete preparation process of 11#Ag/AgBr colloidal spheres catalyst is as follows:
The concrete preparation process of Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 115mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Embodiment 12
The concrete preparation process of 12#Ag/AgBr/GO nano composite material is as follows:
(1) preparation of GO
With the preparation method of GO in embodiment 1.
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60 DEG C, constant temperature stirs 30min, add 95mgPVP and 120mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 5mg to prepare with said method, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A.Take at normal temperatures in addition 150mg AgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B.Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is appreciated 155 DEG C, stir 15min reaction end.Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite material after being dried.
Two, Ag/AgBr/GO nano composite material is as the activity rating of catalyst
Table 1:Ag/AgBr/GO nano composite material photocatalytic degradation rhodamine experimental result
(a)reaction condition: degraded concentration is 10mg L
-1rhodamine aqueous solution 20mL
Measure 20mL 10mg L
-1the rhodamine aqueous solution is put into conical flask, add 30mg Ag/AgBr/GO nano-composite catalyst, at dark place, ultrasonic dispersion 30min makes it reach adsorption equilibrium, then under the condition stirring, under sunshine, irradiate 2h, the concentration every 20min with rhodamine in the 722S spectrophotometer measurement aqueous solution.
Table 1 is the prepared Ag/AgBr/GO nano-composite catalyst of the present invention, the degradation rate of different light time when degraded rhodamine.As can be seen from Table 1, under the irradiation of sunshine, Ag/AgBr/GO nano-composite catalyst has shown good catalytic activity to degraded rhodamine.In the time irradiating 40min, the degradation rate of rhodamine is 93%, and in the time that light application time is 60min, degradation rate reaches 97%, and when light application time is 120min, degradation rate reaches 98%.
The stability experiment result of table 2:Ag/AgBr/GO nano composite photo-catalyst
Table 2 is stability tests of catalyst A g/AgBr/GO.Degraded 20mL concentration is 10mg L
-1the rhodamine aqueous solution, while degraded for the first time, catalyst amount is 30mg, light application time 2h, after completion of the reaction, centrifugation, reclaim catalyst, then to add 20mL concentration is 10mg L
-1the rhodamine aqueous solution, carries out exposure experiments to light, and catalyst so recycles 6 times, and as can be seen from Table 2, the degradation rate of rhodamine still can reach 83%, and this shows: the having good stability of Ag/AgBr/GO nano-composite catalyst.
Claims (2)
1. a preparation method for Ag/AgBr/GO nano composite photo-catalyst, is characterized in that comprising the following steps:
(1) preparation of GO
0.5g graphite powder and 1.5g KMnO
4join in the round-bottomed flask that the 12mL concentrated sulfuric acid is housed, ice-water bath condition lower magnetic force stirs 4h, is heated to 35 DEG C, constant temperature stirs 30min, dropwise adds 23mL distilled water, is warming up to 98 DEG C, stir 15min, this mixture is transferred in ice-water bath, add 70mL distilled water diluting, add again the hydrogen peroxide of 10mL30%, stir 30min, solution becomes yellow, centrifugation, fully wash to till supernatant liquor pH=7, lower sediment thing is drying to obtain to GO;
(2) preparation of Ag/AgBr/GO nano composite material
Measure 12mL ethylene glycol and put into round-bottomed flask, at 60～120 DEG C of initial reaction temperature, constant temperature stirs 30min, add 54～150mg PVP and 100～160mg CTAB, continue to stir until the two dissolves completely, then the GO that adds 3～10mg step (1) to prepare, continue to stir 2h, so that GO is evenly distributed in above-mentioned solution, suspension is now called A; Take at normal temperatures in addition 80～150mgAgNO
3, it is dissolved in 1.5mL ethylene glycol, be called solution B; Under the state stirring, solution B is splashed in suspending liquid A with plastic dropper, stir 30min, temperature is risen to 155 DEG C, keep 15min, reaction end; Reactant is cooled to room temperature, centrifugation, washing, obtains Ag/AgBr/GO nano composite photo-catalyst after being dried.
2. the preparation method of Ag/AgBr/GO nano composite photo-catalyst as claimed in claim 1, is characterized in that, in step (2), described initial reaction temperature is 60 DEG C, described AgNO
3, GO, PVP and CTAB consumption be respectively 100mg, 5mg, 95mg and 120mg.
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| CN105833865A (en) * | 2016-04-11 | 2016-08-10 | 河南科技学院 | A preparing method of a graphene-loaded Ag photocatalyst having a cubic morphology |
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| CN105709782A (en) * | 2016-03-09 | 2016-06-29 | 安徽工业大学 | Preparing method and application of Ag/AgBr/BiOCl-(001) nanometer composite material |
| CN105833865A (en) * | 2016-04-11 | 2016-08-10 | 河南科技学院 | A preparing method of a graphene-loaded Ag photocatalyst having a cubic morphology |
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| CN106268803A (en) * | 2016-07-20 | 2017-01-04 | 武夷学院 | A kind of preparation method of the graphene-supported Ag Bi photocatalyst with 40 shape of octahedron |
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| CN111604070B (en) * | 2020-06-28 | 2023-05-23 | 廊坊师范学院 | Composite membrane photocatalyst and preparation method and application thereof |
| CN114950498A (en) * | 2022-05-16 | 2022-08-30 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
| CN114950498B (en) * | 2022-05-16 | 2023-12-22 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
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