CN102836709A - Ag@Ag2O microcrystals of photocatalytic material with specific patterns and high surface activity and preparation method thereof - Google Patents
Ag@Ag2O microcrystals of photocatalytic material with specific patterns and high surface activity and preparation method thereof Download PDFInfo
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Abstract
The invention relates to Ag@Ag2O microcrystals of a photocatalytic material with specific patterns and high surface activity and a preparation method thereof. The Ag@Ag2O microcrystals of the photocatalytic material are made of a compound photocatalytic material with the corresponding patterns formed by depositing silver nano particles at the surfaces of silver oxide particles with different patterns. The Ag@Ag2O microcrystals of the photocatalytic material with the specific patterns and high surface activity and the preparation method thereof are characterized in that silver oxide is in a cubic crystal system, the particle size is 0.5 to 2.0mum, and the particle size of the silver nano particles deposited at the surfaces is 20 to 30nm; and the silver oxide particles have one of the 5 following patterns: a cubic block, a rhombohedral dodecahedron, an octahedron, a 18-faced body or a 26-faced body. The invention also provides a preparation method of Ag@Ag2O. By exposing the crystal face of Ag2O, which has different surface energy, and loading silver deposited at the surface of the Ag2O, the Ag@Ag2O photocatalytic material disclosed by the invention has high surface activity, the preparation method is simple, the reaction condition is mild, the operation is convenient, and the energy consumption is little.
Description
Technical field
The present invention relates to a kind of specific morphology high surface catalysis material AgAg that has
2O crystallite and preparation method thereof belongs to the synthetic field of visible light-responded micro-nano photocatalysis powder material.
Background technology
In recent years, becoming increasingly conspicuous of the energy and environmental problem seriously influenced expanding economy.Environmental pollution has brought huge harm for Human's production and life, and especially the pollution of water resource has jeopardized the healthy of the mankind, and the method for being badly in need of feasibility is disposed of sewage.Traditional method administer water pollute exist that power consumption is big, complex equipments, expense are high, be prone to bring shortcoming such as secondary pollution.Therefore, develop the focus that a kind of novel, efficient, practical environmental protection treatment technology becomes people's research.Along with going deep into of research; It is found that the heterogeneous photocatalysis technology of semiconductor comes degradable organic pollutant through environmentally friendly redox reaction; Photocatalysis technology has well combined this two big worlds Sexual Themes of energy and environment; Have that energy consumption is low, easy and simple to handle, reaction condition is gentle, usage range is wide, can reduce advantages such as secondary pollution, utilize green energy resource of solar energy problem of curbing environmental pollution, thereby aspect waste water control, more and more receive people's attention.
Silver oxide be with in typical narrow bandgap semiconductor material, all have a wide range of applications in a lot of fields, as as polishing agent, colouring agent, silver oxide electrode, catalyst or the like.Silver oxide can well absorb the visible region in the sunshine, therefore can be used as photocatalyst material.But, the not only light-catalysed inefficiency of the silver oxide photochemical catalyst that traditional method obtains, the photo-generated carrier recombination rate is high, and the pattern of not controlling it is regulated and control its photo-catalysis capability.
Summary of the invention
To the deficiency of prior art, the present invention provides a kind of high-efficiency photocatalysis material AgAg of multiform looks
2O and preparation method thereof.
Term explanation: AgAg
2O is meant that silver is coated on the composite of silver oxide outer surface, the conventional expression in this area.
Technical scheme of the present invention is following:
A kind of catalysis material AgAg
2The O crystallite is that wherein, said silver oxide is a cubic system at the composite photocatalyst material of the corresponding pattern of formation of the silver oxide particle surface deposition silver nano-grain of different-shape, and particle diameter is 0.5-2.0 μ m, and the silver nano-grain particle diameter of surface deposition is 20-30nm.The silver oxide particle of said different-shape has one of following 5 kinds of patterns: cubic block, water chestnut side's dodecahedron, octahedron, 18 bodies or 26 bodies.
Catalysis material AgAg of the present invention
2The preparation method of O crystallite comprises the steps:
(1) prepares the liquor argenti nitratis ophthalmicus of 0.01-0.5M respectively; 0.01-0.5M enveloping agent solution, complexing agent is selected from ammonium nitrate, ammonium acetate, diammonium hydrogen phosphate or ammoniacal liquor;
(2) the 0.01-0.5M enveloping agent solution is joined in the 0.01-0.5M liquor argenti nitratis ophthalmicus by 2.5 ~ 5:2.5 volume ratio, stirred 10 minutes; Get silver-colored ammonium salt solution;
(3) sodium hydroxide solution of adding 2M in above-mentioned silver-colored ammonium salt solution; Sodium hydroxide solution and silver-colored ammonium salt solution volume ratio (0.25-0.75): (5 ~ 7.5); Stirred 10 ~ 15 minutes centrifugal 15 ~ 25 minutes, precipitate with deionized water that obtains and washing with alcohol, 60 ℃ were descended dry 6-12 hour;
(4) get the dry product of step (3) gained, press mass volume ratio 2 ~ 3g:1000ml, joining concentration is the 20mg/L methyl orange solution; With radiation of visible light 10-30 minute of λ>420nm; Suction filtration, gained solids be with deionized water and washing with alcohol 3 times, 60 ℃ dry 6-12 hour down.
Resulting AgAg2O and step (3) silver oxide consistent appearance has one of following five kinds of patterns: cube, water chestnut side's dodecahedron, octahedron, 18 bodies or 26 bodies.
Preferred according to the present invention, liquor argenti nitratis ophthalmicus is identical with the concentration of enveloping agent solution in the step (1), gets 0.01M, 0.02M, 0.03M, 0.04M, 0.05M or 0.5M respectively.
Preferred according to the present invention, Ag in the silver-colored ammonium salt solution of step (2)
+: NH
4 +=1:2 mol ratio.
Preferred according to the present invention, when the used complexing agent of step (2) was diammonium hydrogen phosphate, the consumption of the 2M sodium hydroxide solution in the step (3) was 0.75:5.
Preferred according to the present invention, when the used complexing agent of step (2) was ammonium nitrate, ammonium acetate or ammoniacal liquor, the consumption of the 2M sodium hydroxide solution in the step (3) was 0.25:5.
Preferred according to the present invention, the time dry in the step (3) is 12 hours.
Preferred according to the present invention, the light application time in the step (4) is 10 minutes, and be 12 hours drying time.
Further preferred according to the present invention, a kind of catalysis material AgAg with specific morphology high surface
2The preparation method of O, step is following:
2.5ml the liquor argenti nitratis ophthalmicus of 0.01-0.05M in add the enveloping agent solution of 0.01-0.05M, stirs after 10 minutes, add the sodium hydroxide solution of the 2M of 0.25-0.75ml, continue stirring 10 minutes; Centrifugal 20 minutes of changeing of gained sample 5000, gained precipitate with deionized water and washing with alcohol 3 times, 60 ℃ of dryings 12 hours down; Resulting dry product is got 0.2g, is added in the methyl orange solution of 20mg/L of 100ml, and visible light irradiation 10 minutes down, the sample that obtains, suction filtration, with deionized water and washing with alcohol 3 times, 60 times dryings 12 hours.
On above-described preferred scheme basis, further preferred scheme such as one of following:
I. the silver nitrate with 0.01M mixes with the ammonium nitrate solution of 0.01M, adds the sodium hydroxide solution 0.25ml of 2M at last, obtains the cube silver oxide; Or,
Ii. the silver nitrate with 0.03M mixes with the ammonium acetate solution of 0.0M, adds the sodium hydroxide solution 0.25ml of 2M at last, obtains the dodecahedral silver oxide in water chestnut side; Or,
Iii. the silver nitrate with 0.5M mixes with the ammonia spirit of 0.5M, adds the sodium hydroxide solution 0.25ml of 2M at last, obtains octahedra silver oxide; Or,
Iv. the silver nitrate with 0.02M mixes with the ammonium nitrate solution of 0.02M, adds the sodium hydroxide solution 0.75ml of 2M at last, obtains 18 body silver oxide silver oxides; Or,
V. the silver nitrate with 0.03M mixes with the ammonium nitrate solution of 0.03M, adds the sodium hydroxide solution 0.25ml of 2M at last, obtains 26 body silver oxides.
The AgAg of five kinds of patterns of the present invention
2The O catalysis material has different photocatalysis performances, can be used for degradation of organic substances.
Visible light responsible photocatalytic material AgAg of the present invention
2The application of O is applied to the removal of organic pollution in air, waste water, surface water or the drinking water, or is used for the photocatalysis removal of heavy metal ion.
Excellent results of the present invention is following:
1. catalysis material AgAg of the present invention
2O has 5 kinds of different-shape characteristics: cubic block, water chestnut side's dodecahedron, octahedron, 18 bodies or 26 bodies.And Ag at different-shape
2The O area load the Ag nano particle.This catalysis material is visible light-responded, finds that through experiment test the material of this structure of different-shape is having different photocatalysis performances.
The present invention through the method for photo-reduction silver ion at Ag
2The O surface is with Ag
+In-situ reducing becomes Ag
0, reaction forms AgAg
2The O composite construction.
3. the catalysis material of resulting five kinds of patterns; Because the different surface of each crystal face can; Resulting sample shows different photocatalysis performances, and wherein the photochemical catalyst of cube pattern demonstrates best photocatalytic activity, 90% the methyl orange dye of in 10 minutes, degrading.
4. catalysis material AgAg of the present invention
2The O preparation method is simple, with low cost, the synthetic method mild condition has higher commercial application prospect.
Find the AgAg of different-shape through experimental study
2O demonstrates different photocatalysis performances, the degraded AgAg of cube pattern
2Can in 10 minutes, degrade 90% methyl orange dye of O, Comparatively speaking, water chestnut side's dodecahedron and octahedral AgAg
2O can only degrade 40% and 20% in 10 minutes.{ 100} face (constituting cubical crystal face) has the highest surface ability owing to silver oxide for this.
Description of drawings
Fig. 1 is the SEM figure of the cube silver oxide of embodiment 1 preparation.
Fig. 2 is the SEM figure of water chestnut side's dodecahedron silver oxide of embodiment 2 preparations.
Fig. 3 is the SEM figure of the octahedra silver oxide of embodiment 3 preparations.
Fig. 4 is the SEM figure of ten octahedra silver oxides of embodiment 4 preparations.
Fig. 5 is the SEM figure of 20 hexahedron silver oxides of embodiment 5 preparations.
Fig. 6 is the photocatalysis comparison diagram of embodiment 1,2,3,4,5 products.Abscissa is that the time, (unit: min), ordinate was the initial concentration (C of concentration (C)/rhodamine B of the methyl orange solution of degraded certain hour
0).Figure a-e is respectively octahedra AgAg
2O, cube AgAg
2O, water chestnut side dodecahedron AgAg
2O, 18 body AgAg
2O, 26 body AgAg
2The photocatalytic degradation efficiency chart of O.
Fig. 7 is the X-ray diffractogram of embodiment 1,2, and a is a cubic oxide silver, and b is a cube AgAg
2O, c water chestnut side dodecahedron AgAg
2O.Abscissa be 2 θ (°), ordinate is intensity (a.u).
The specific embodiment
, but be not limited thereto further specifying among the present invention below in conjunction with accompanying drawing.
It is following among the embodiment prepared material to be carried out the method for photocatalytic activity test:
Photocatalysis test (cross section 30cm in glass beaker
2, high 5cm) carry out under the normal temperature and pressure.Light source is selected the 300W xenon lamp that optical filter is housed for use, makes optical source wavelength greater than 420nm.Come the photocatalytic activity of assess sample with methyl orange.Take by weighing 0.1g sample dispersion (20mg/L) in the 100mL methyl orange solution.Before the light-catalyzed reaction test, lucifuge magnetic agitation 30min makes methyl orange reach adsorption equilibrium at catalyst surface, and every at a distance from 2min sampling 5ml behind the logical light, centrifugation is got supernatant and used the measurement of ultraviolet-visible spectrophotometer absorbance.
As a comparison, the AgAg of other patterns
2O carries out the photocatalytic activity test under equal experiment condition.
Embodiment 1
2.5ml the liquor argenti nitratis ophthalmicus of 0.01M in add the ammonium nitrate solution of 5ml 0.01M, stirs after 10 minutes, add the sodium hydroxide solution of the 2M of 0.25ml, continue stirring 10 minutes.The centrifuge that resulting sample 5000 changes is centrifugal, gained pitchy precipitate with deionized water and washing with alcohol 3 times.60 times dryings 12 hours; Obtain cubical Ag
2O, cube length of side size is at 0.5 μ m.Fig. 1 is the Electronic Speculum picture of the sample that obtains.Get resulting sample 0.2g, be added in the methyl orange solution of 20mg/L of 100ml, visible light irradiation 10 minutes down obtains the black sample, suction filtration, and with deionized water and washing with alcohol 3 times, 60 ℃ of following dryings 12 hours.This has just obtained cubical AgAg
2O structured light catalysis material, the size of institute's depositing silver is between 20-30nm.Get cube AgAg
2O sample 0.1g is added in the methyl orange solution of 20mg/L of 100ml, and visible light is irradiation down, surveys its degradation efficiency with ultraviolet-uisible spectrophotometer.Curve b in the corresponding diagram 6.
2.5ml the liquor argenti nitratis ophthalmicus of 0.03M in add the ammonium acetate solution of 5ml 0.03M, stirs after 10 minutes, add the sodium hydroxide solution of the 2M of 0.25ml, continue stirring 10 minutes.The centrifuge that resulting sample 5000 changes is centrifugal and with deionized water and washing with alcohol 3 times.Drying is 12 hours under 60 ℃.The dodecahedral Ag in the water chestnut side that obtains
2O.Water chestnut side's dodecahedron size is at 0.7 μ m.Fig. 2 is the Electronic Speculum picture of the sample that obtains.Resulting sample is got 0.2g, is added in the methyl orange solution of 20mg/L of 100ml, and visible light irradiation 10 minutes down obtains test sample, suction filtration, and with deionized water and washing with alcohol 3 times, 60 ℃ of following dryings 12 hours.This has just obtained the dodecahedral AgAg in water chestnut side
2O structured light catalysis material, the size of institute's depositing silver is between 20-30nm.Get water chestnut side dodecahedron AgAg
2O sample 0.1g is added in the methyl orange solution of 20mg/L of 100ml, and visible light is irradiation down, surveys its degradation efficiency with ultraviolet-uisible spectrophotometer.Curve c in the corresponding diagram 6.
Embodiment 3
2.5ml the liquor argenti nitratis ophthalmicus of 0.5M in add the ammonia spirit of 5ml 0.5M, stirs after 10 minutes, add the sodium hydroxide solution of the 2M of 0.25ml, continue stirring 10 minutes.The centrifuge that resulting sample 5000 changes is centrifugal and with deionized water and washing with alcohol 3 times.Drying is 12 hours under 60 ℃.The octahedral Ag that obtains
2O.Octahedra size is at 2 μ m.Fig. 3 is the Electronic Speculum figure of the sample that obtains.Resulting sample is got 0.2g, is added in the methyl orange solution of 20mg/L of 100ml, and visible light irradiation 10 minutes down obtains test sample, suction filtration, and with deionized water and washing with alcohol 3 times, 60 ℃ of following dryings 12 hours.This has just obtained octahedral AgAg
2O structured light catalysis material, the size of institute's depositing silver is between 20-30nm.Get octahedra AgAg
2O sample 0.1g is added in the methyl orange solution of 20mg/L of 100ml, and visible light is irradiation down, surveys its degradation efficiency with ultraviolet-uisible spectrophotometer.Curve a in the corresponding diagram 6.
2.5ml the liquor argenti nitratis ophthalmicus of 0.01M in add the ammonium dibasic phosphate solution of 2.5ml 0.01M, stirs after 10 minutes, add the sodium hydroxide solution of the 2M of 0.75ml, continue stirring 10 minutes.The centrifuge that resulting sample 5000 changes is centrifugal and with deionized water and washing with alcohol 3 times.Drying is 12 hours under 60 ℃.The Ag of 18 bodies that obtain
2O.Ten octahedra sizes are at 0.7 μ m.Resulting sample is got 0.2g, is added in the methyl orange solution of 20mg/L of 100ml, and visible light irradiation 10 minutes down obtains test sample, suction filtration, and with deionized water and washing with alcohol 3 times, 60 ℃ of following dryings 12 hours.This has just obtained the AgAg of 18 bodies
2O structured light catalysis material, the size of institute's depositing silver is between 20-30nm.Get 18 body AgAg
2O sample 0.1g is added in the methyl orange solution of 20mg/L of 100ml, and visible light is irradiation down, surveys its degradation efficiency with ultraviolet-uisible spectrophotometer.Curve d in the corresponding diagram 6.
Embodiment 5
2.5ml the liquor argenti nitratis ophthalmicus of 0.03M in add the ammonium nitrate solution of 5ml 0.03M, stirs after 10 minutes, add the sodium hydroxide solution of the 2M of 0.25ml, continue stirring 10 minutes.The centrifuge that resulting sample 5000 changes is centrifugal and with deionized water and washing with alcohol 3 times.Drying is 12 hours under 60 ℃.The Ag of 18 bodies that obtain
2O.26 body sizes are at 0.9 μ m.Fig. 5 is the Electronic Speculum picture of the sample that obtains.Resulting sample is got 0.2g, is added in the methyl orange solution of 20mg/L of 100ml, and visible light irradiation 10 minutes down, the sample that obtains, suction filtration, with deionized water and washing with alcohol 3 times, 60 ℃ of following dryings 12 hours.This has just obtained the AgAg of 26 bodies
2O structured light catalysis material, the size of institute's depositing silver is between 20-30nm.Get 26 body AgAg
2O sample 0.1g is added in the methyl orange solution of 20mg/L of 100ml, and visible light is irradiation down, surveys its degradation efficiency with ultraviolet-uisible spectrophotometer.Curve e in the corresponding diagram 6.
Claims (10)
1. catalysis material AgAg
2The O crystallite; It is composite photocatalyst material at the corresponding pattern of formation of the silver oxide particle surface deposition silver nano-grain of different-shape; It is characterized in that said silver oxide is a cubic system, particle diameter is 0.5-2.0 μ m, and the silver nano-grain particle diameter of surface deposition is 20-30nm; The silver oxide particle of said different-shape has one of following 5 kinds of patterns: cubic block, water chestnut side's dodecahedron, octahedron, 18 bodies or 26 bodies.
2. the described catalysis material AgAg of claim 1
2The preparation method of O crystallite comprises the steps:
(1) prepares the liquor argenti nitratis ophthalmicus of 0.01-0.5M respectively; 0.01-0.5M enveloping agent solution, complexing agent is selected from ammonium nitrate, ammonium acetate, diammonium hydrogen phosphate or ammoniacal liquor;
(2) the 0.01-0.5M enveloping agent solution is joined in the 0.01-0.5M liquor argenti nitratis ophthalmicus by 2.5 ~ 5:2.5 volume ratio, stirred 10 minutes; Get silver-colored ammonium salt solution;
(3) sodium hydroxide solution of adding 2M in above-mentioned silver-colored ammonium salt solution; Sodium hydroxide solution and silver-colored ammonium salt solution volume ratio (0.25-0.75): (5 ~ 7.5); Stirred 10 ~ 15 minutes centrifugal 15 ~ 25 minutes, precipitate with deionized water that obtains and washing with alcohol 3 times, 60 ℃ were descended dry 6-12 hour;
(4) dry product of getting step (3) gained is pressed mass volume ratio 2 ~ 3g:1000ml; Joining concentration is the 20mg/L methyl orange solution, with radiation of visible light 10-30 minute of λ>420nm, and suction filtration; The gained solids is with deionized water and washing with alcohol 3 times, 60 ℃ dry 6-12 hour down.
3. catalysis material AgAg as claimed in claim 2
2The preparation method of O crystallite is characterized in that liquor argenti nitratis ophthalmicus is identical with the concentration of enveloping agent solution in the step (1), gets 0.01M, 0.02M, 0.03M, 0.04M, 0.05M or 0.5M respectively.
4. catalysis material AgAg as claimed in claim 2
2The preparation method of O crystallite is characterized in that Ag in the silver-colored ammonium salt solution of step (2)
+: NH
4 +=1:2 mol ratio.
5. catalysis material AgAg as claimed in claim 2
2The preparation method of O crystallite, when it is characterized in that the used complexing agent of step (2) is diammonium hydrogen phosphate, the consumption of the 2M sodium hydroxide solution in the step (3) is 0.75:5.
6. catalysis material AgAg as claimed in claim 2
2The preparation method of O crystallite, when it is characterized in that the used complexing agent of step (2) is ammonium nitrate, ammonium acetate or ammoniacal liquor, the consumption of the 2M sodium hydroxide solution in the step (3) is 0.25:5.
7. catalysis material AgAg as claimed in claim 2
2The preparation method of O crystallite is characterized in that the time dry in the step (3) is 12 hours.
8. catalysis material AgAg as claimed in claim 2
2The preparation method of O crystallite is characterized in that the light application time in the step (4) is 10 minutes, and be 12 hours drying time.
9. catalysis material AgAg as claimed in claim 2
2The preparation method of O crystallite is characterized in that step is following:
2.5ml the liquor argenti nitratis ophthalmicus of 0.01-0.05M in add the enveloping agent solution of 0.01-0.05M, stirs after 10 minutes, add the sodium hydroxide solution of the 2M of 0.25-0.75ml, continue stirring 10 minutes; Centrifugal 20 minutes of changeing of resulting sample 5000, gained precipitate with deionized water and washing with alcohol 3 times; Drying is 12 hours under 60 ℃; The gained dry product is got 0.2g, is added in the methyl orange solution of 20mg/L of 100ml, and visible light irradiation 10 minutes down, the sample that obtains, suction filtration, with deionized water and washing with alcohol 3 times, 60 times dryings 12 hours.
10. catalysis material AgAg as claimed in claim 9
2The preparation method of O crystallite is characterized in that as one of following:
I. the silver nitrate with 0.01M mixes with the ammonium nitrate solution of 0.01M, adds the sodium hydroxide solution 0.25ml of 2M, obtains the cube silver oxide; Or,
Ii. the silver nitrate with 0.03M mixes with the ammonium acetate solution of 0.0M, adds the sodium hydroxide solution 0.25ml of 2M, obtains the dodecahedral silver oxide in water chestnut side; Or,
Iii. the silver nitrate with 0.5M mixes with the ammonia spirit of 0.5M, adds the sodium hydroxide solution 0.25ml of 2M, obtains octahedra silver oxide; Or,
Iv. the silver nitrate with 0.02M mixes with the ammonium nitrate solution of 0.02M, adds the sodium hydroxide solution 0.75ml of 2M, obtains 18 body silver oxide silver oxides; Or,
V. the silver nitrate with 0.03M mixes with the ammonium nitrate solution of 0.03M, adds the sodium hydroxide solution 0.25ml of 2M, obtains 26 body silver oxides.
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