CN103071496B - Visible-light-driven photocatalyst and preparation method and application thereof - Google Patents
Visible-light-driven photocatalyst and preparation method and application thereof Download PDFInfo
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- CN103071496B CN103071496B CN201310043936.8A CN201310043936A CN103071496B CN 103071496 B CN103071496 B CN 103071496B CN 201310043936 A CN201310043936 A CN 201310043936A CN 103071496 B CN103071496 B CN 103071496B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011941 photocatalyst Substances 0.000 title claims abstract 4
- 239000003054 catalyst Substances 0.000 claims abstract description 36
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 23
- 101710134784 Agnoprotein Proteins 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 5
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract 5
- 125000000223 arsonoyl group Chemical group [H][As](*)(*)=O 0.000 claims abstract 5
- 230000000593 degrading effect Effects 0.000 claims abstract 2
- 239000002244 precipitate Substances 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 238000004448 titration Methods 0.000 claims description 9
- IHZDYHDJAVUIBH-UHFFFAOYSA-L disodium hydrogenarsenate Chemical compound [Na+].[Na+].O[As]([O-])([O-])=O IHZDYHDJAVUIBH-UHFFFAOYSA-L 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 11
- 238000013019 agitation Methods 0.000 description 8
- 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 7
- 229940043267 rhodamine b Drugs 0.000 description 7
- 239000013049 sediment Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- -1 12mg/L Chemical compound 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
本发明公开了一种可见光催化剂及其制备方法与应用。本发明主要包括：分别称取AgNO3、Na2HAsO4置于不同烧杯中，用去离子水溶解后，并分别装入两个分液漏斗中；用浓氨水配置成一定浓度的氨水；在室温磁力搅拌的条件下，将AgNO3溶液和Na2HAsO4溶液采用并流沉淀法反应；其滴速为2~3d/s，滴定过程中同时用氨水控制混合物的pH为5~8，滴定完毕后在室温下继续磁力搅拌2h；将制得的桔黄色沉淀物洗涤数次，然后于60℃温度下烘干，得到红褐色粉末状产物，即Ag3AsO4光催化剂。本发明制备方法简单，条件温和易控，有利于大规模推广应用，本发明制备Ag3AsO4光催化剂活性高，适用于在可见光下降解有机污染物。The invention discloses a visible light catalyst as well as its preparation method and application. The invention mainly includes: weighing AgNO 3 and Na 2 HAsO 4 respectively, placing them in different beakers, dissolving them with deionized water, and putting them into two separating funnels respectively; using concentrated ammonia water to prepare ammonia water of a certain concentration; Under the condition of magnetic stirring at room temperature, the AgNO 3 solution and the Na 2 HAsO 4 solution were reacted by the co-current precipitation method; After completion, magnetic stirring was continued at room temperature for 2 h; the obtained orange precipitate was washed several times, and then dried at 60° C. to obtain a reddish-brown powder product, namely Ag 3 AsO 4 photocatalyst. The preparation method of the invention is simple, the conditions are mild and easy to control, and is beneficial to large-scale popularization and application. The Ag 3 AsO 4 photocatalyst prepared by the invention has high activity and is suitable for degrading organic pollutants under visible light.
Description
Technical field
The invention belongs to chemical and environment-friendly engineering technical field, be specifically related to a kind of visible light catalyst and preparation method thereof and application.
Background technology
Photocatalitic Technique of Semiconductor can at room temperature directly utilize sunshine by organic pollution oxidative degradation.Therefore, by photocatalysis method, making full use of sunshine and carry out degradable organic pollutant, is an effective way that solves current problem of environmental pollution.The appropriate design of photochemical catalyst is the central factor that determines photocatalysis performance, generally need to consider the problem of the following aspects: (1) light absorption interval.Ultraviolet light only accounts for 4% left and right of sunshine gross energy, and visible ray accounts for 46% left and right of sunshine gross energy.Therefore, utilize the key of solar energy to be to utilize the visible ray in sunshine.(2) oxidation or reducing power.The oxidation that photochemical catalyst is strong or reducing power are its highly active prerequisites.But the photochemical catalyst that can absorb visible ray all has narrower band gap, a little less than this means that its redox ability, this generally causes its photocatalytic activity low.Therefore, preparation has the photochemical catalyst of suitable band structure, when making it have wide visible light-responded scope, also has strong oxidation or reducing power, thereby show high visible light catalysis activity, be one and have very much challenge and a research theme highly significant.
Document reported first in 2010, Ag
3pO
4semiconductor is as a kind of novel visible light catalyst with high-quantum efficiency, and the activity of its degradable organic pollutant is far above BiVO
4, AgBr, AgI and N doped Ti O
2etc. common visible light catalyst (seeing document Nature Materials, 2010,9,559-564).
Summary of the invention
One of object of the present invention is to provide a kind of novel visible light catalyst, and this visible light catalyst molecular formula is Ag
3asO
4, for Powdered, apparent is bronzing, microstructure is spherical shape.
More particularly, the microstructure of this visible light catalyst is the spherical shape of 0.25 μ m.
Two of object of the present invention is to provide a kind of preparation method of above-mentioned visible light catalyst, and it comprises the step of following order:
(1) take respectively AgNO
3, Na
2hAsO
4be placed in different beakers, be mixed with the AgNO that concentration is 0.1 ~ 0.4mol/L with deionized water dissolving
3solution and concentration are the Na of 0.025 ~ 0.1mol/L
2hAsO
4after solution, and be respectively charged in two separatory funnels; Be mixed with the ammoniacal liquor that concentration is 0.05 ~ 0.2mol/L with concentrated ammonia liquor;
(2) under the condition of room temperature magnetic agitation, the AgNO that step (1) is prepared
3solution and Na
2hAsO
4solution adopts the reaction of parallel-flow precipitation method; Its speed is 2 ~ 3d/s, and in titration process, use the pH of the ammoniacal liquor control mixture that step (1) prepares is 5 ~ 8 simultaneously, at room temperature continues magnetic agitation 2h after titration;
(3) orange colour sediment washing step (2) being made for several times, is then dried at 60 DEG C of temperature, obtains bronzing powdery product, i.e. Ag
3asO
4photochemical catalyst.
In above-mentioned steps (2), the mass ratio of controlling the concentration material of liquor argenti nitratis ophthalmicus, disodium hydrogen arsenate solution, ammoniacal liquor in mixture course of reaction is 4:1:2.
Three of object of the present invention is to provide the application of above-mentioned visible light catalyst, and this visible light catalyst is applicable to degradable organic pollutant under visible ray.
The present invention, by a kind of easy method, prepares a kind of novel visible light catalyst Ag
3asO
4.By experiment, characterize Ag
3asO
4absorption band edge in about 730nm, therefore very high to the utilization ratio of visible ray.And, in the degraded of rhodamine B, the specific activity Ag of photochemical catalyst of the present invention
3pO
4also high.Therefore, Ag of the present invention
3asO
4it is a kind of novel, efficient visible light catalyst.Document, patent finding show, the present invention is Ag
3asO
4the first report of photochemical catalyst, this photochemical catalyst has potential application prospect in Organic Waste Water Treatment field.
Beneficial effect of the present invention is:
(1) the present invention adopts disodium hydrogen arsenate to prepare Ag
3asO
4, adopt ammoniacal liquor control reaction system Acidity of Aikalinity, guarantee Ag
3asO
4high photocatalysis characteristic.
(2) the present invention is by Ag
3asO
4material is applied to photocatalysis field, Ag under visible ray
3asO
4have good rhodamine B photocatalytic activity, its activity is under equal conditions higher than Ag
3pO
4and AgI.
(3) preparation method of the present invention is extremely simple, and mild condition is easily controlled (under normal temperature and pressure, the room temperature of <35 DEG C), is conducive to large-scale promotion application.
Brief description of the drawings
Fig. 1 is the Ag of the embodiment of the present invention
3asO
4x-ray diffraction (XRD) figure of photochemical catalyst.
Fig. 2 is the Ag of the embodiment of the present invention
3asO
4eSEM (SEM) figure of photochemical catalyst.
Fig. 3 is the Ag of the embodiment of the present invention
3asO
4uV-Vis reflective spectrum (UV-Vis DRS) figure of photochemical catalyst.
Fig. 4 is the Ag of the embodiment of the present invention
3asO
4photochemical catalyst and Ag
3pO
4, AgI photochemical catalyst active result figure; Wherein, C
0for photochemical catalyst adds the initial concentration of front rhodamine B, i.e. 12mg/L, C inscribes the concentration of rhodamine B while being arbitrary in photocatalytic process.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
Take respectively AgNO
3, Na
2hAsO
4be placed in different beakers, be mixed with the AgNO that concentration is 0.2mol/L with deionized water dissolving
3solution and concentration are the Na of 0.05mol/L
2hAsO
4after solution, pack in two separatory funnels; Be mixed with the ammoniacal liquor that concentration is 0.1mol/L with concentrated ammonia liquor; Under the condition of room temperature magnetic agitation, adopt parallel-flow precipitation legal system by AgNO
3solution and Na
2hAsO
4solution reaction is produced the orange colour sediment Ag with photocatalytic activity
3asO
4; Its speed is 2 ~ 3d/s, and in titration process, use the pH of prepared ammoniacal liquor control mixture is 5 ~ 8 simultaneously, at room temperature continues magnetic agitation 2h after titration.The mass ratio of controlling the concentration material of liquor argenti nitratis ophthalmicus, disodium hydrogen arsenate solution, ammoniacal liquor in mixture course of reaction is 4:1:2.By deionized water washing 3 times for orange colour sediment, then just obtain Ag in 60 DEG C of oven dry
3asO
4photochemical catalyst is bronzing powder.
Embodiment 2:
Take respectively AgNO
3, Na
2hAsO
4be placed in different beakers, be mixed with the AgNO that concentration is 0.1mol/L with deionized water dissolving
3solution and concentration are the Na of 0.025mol/L
2hAsO
4after solution, pack in two separatory funnels; Be mixed with the ammoniacal liquor that concentration is 0.05mol/L with concentrated ammonia liquor; Under the condition of room temperature magnetic agitation, adopt parallel-flow precipitation legal system by AgNO
3solution and Na
2hAsO
4solution reaction is produced the orange colour sediment Ag with photocatalytic activity
3asO
4; Its speed is 2 ~ 3d/s, and in titration process, use the pH of prepared ammoniacal liquor control mixture is 5 ~ 8 simultaneously, at room temperature continues magnetic agitation 2h after titration.The mass ratio of controlling the concentration material of liquor argenti nitratis ophthalmicus, disodium hydrogen arsenate solution, ammoniacal liquor in mixture course of reaction is 4:1:2.By deionized water washing 3 times for orange colour sediment, then just obtain Ag in 60 DEG C of oven dry
3asO
4photochemical catalyst is bronzing powder.
Embodiment 3:
Take respectively AgNO
3, Na
2hAsO
4be placed in different beakers, be mixed with the AgNO that concentration is 0.4mol/L with deionized water dissolving
3solution and concentration are the Na of 0.1mol/L
2hAsO
4after solution, pack in two separatory funnels; Be mixed with the ammoniacal liquor that concentration is 0.2mol/L with concentrated ammonia liquor; Under the condition of room temperature magnetic agitation, adopt parallel-flow precipitation legal system by AgNO
3solution and Na
2hAsO
4solution reaction is produced the orange colour sediment Ag with photocatalytic activity
3asO
4; Its speed is 2 ~ 3d/s, and in titration process, use the pH of prepared ammoniacal liquor control mixture is 5 ~ 8 simultaneously, at room temperature continues magnetic agitation 2h after titration.The mass ratio of controlling the concentration material of liquor argenti nitratis ophthalmicus, disodium hydrogen arsenate solution, ammoniacal liquor in mixture course of reaction is 4:1:2.By deionized water washing 3 times for orange colour sediment, then just obtain Ag in 60 DEG C of oven dry
3asO
4photochemical catalyst is bronzing powder.
Ag prepared by the present embodiment
3asO
4the X-ray diffraction (XRD) of material is schemed as shown in Figure 1, sample Ag
3asO
4diffraction maximum and Ag
3asO
4standard diagram (JCPDS no.06-0493) completely corresponding.Ag prepared by the present embodiment
3asO
4the ESEM (SEM) of material is schemed as shown in Figure 2, and its microstructure is spherical shape as seen from the figure, and size is about 0.25 μ m.Ag prepared by the present embodiment
3asO
4the UV-Vis reflective spectrum (Uv-Vis DRS) of material is schemed as shown in Figure 3, and sample has obvious absworption peak in visible region, can absorb the visible ray that is less than 730nm.
Ag prepared by the inventive method
3asO
4the visible light catalytic performance evaluation of material is as follows:
Ag prepared by the inventive method
3asO
4the photocatalysis performance of material is by under simulation visible ray, and the situation of employing sample degradation of organic substances is evaluated, and photocatalysis experiment is carried out in light reaction device (comprising Xe lamp 300W, optical filter, magnetic stirring apparatus).Take sample prepared by 0.075g, add in liquid dyes solution (12mg/L RhB) 100mL, lucifuge condition lower magnetic force stirs 1h, reaches absorption-desorption balance.300W Xe lamp adds optical filter (λ >420nm) as analog light source, gets at regular intervals 2.5mL suspension, and gets supernatant after centrifugation (6000rpm, 5min).Use UV-2550 to measure the absorbance of supernatant.Figure 4 shows that Ag prepared by the inventive method
3asO
4the degradation curve of photochemical catalyst catalytic degradation rhodamine B under visible ray condition, as seen from Figure 4, under radiation of visible light, Ag prepared by the present invention
3asO
4the degradable rhodamine B of photochemical catalyst only needs 20min, and Ag
3pO
4, AgI required time is respectively 25,60min.Therefore, under visible ray, Ag
3asO
4the activity of rhodamine B degradation is higher than Ag
3pO
4and AgI.
Claims (3)
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| CN104383937B (en) * | 2014-12-11 | 2016-08-24 | 湖南科技大学 | A kind of solar energy photocatalytic agent and preparation method and application |
| CN105944744B (en) * | 2016-06-08 | 2018-10-12 | 湘潭大学 | A kind of visible-light response type composite photo-catalyst to bisphenol-A with high mineralization rate |
Citations (4)
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|---|---|---|---|---|
| US3485876A (en) * | 1965-11-12 | 1969-12-23 | Stamicarbon | Vapor-phase catalytic oxidation of toluene to benzaldehyde |
| JP2009078211A (en) * | 2007-09-26 | 2009-04-16 | National Institute For Materials Science | photocatalyst |
| CN101648139A (en) * | 2009-09-03 | 2010-02-17 | 福州大学 | Novel visible catalyst-silver phosphate and preparation method thereof |
| CN102716758A (en) * | 2012-06-25 | 2012-10-10 | 武汉理工大学 | Composite visible-light-driven photocatalyst Ag3PO4 and Zn3(PO4)2 and preparation method thereof |
-
2013
- 2013-02-05 CN CN201310043936.8A patent/CN103071496B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3485876A (en) * | 1965-11-12 | 1969-12-23 | Stamicarbon | Vapor-phase catalytic oxidation of toluene to benzaldehyde |
| JP2009078211A (en) * | 2007-09-26 | 2009-04-16 | National Institute For Materials Science | photocatalyst |
| CN101648139A (en) * | 2009-09-03 | 2010-02-17 | 福州大学 | Novel visible catalyst-silver phosphate and preparation method thereof |
| CN102716758A (en) * | 2012-06-25 | 2012-10-10 | 武汉理工大学 | Composite visible-light-driven photocatalyst Ag3PO4 and Zn3(PO4)2 and preparation method thereof |
Non-Patent Citations (11)
| Title |
|---|
| A Crucial Role of Bond Covalency Competition in Determining the Bandgap and Photocatalytic Performance of Silver Oxosalts;Xiaoyan Jin et al.;《The Journal of Physical Chemistry C》;20131102(第117期);第26509-26516页 * |
| A Determination of Parameters in Potassium Dihydrogen Arsenate and Silver Arsenate;Lindsay Helmholz et al.;《Journal of the American Chemical Society》;19420228;第64卷(第02期);第354-358页 * |
| An orthophosphate semiconductor with photooxidation properties under visible-light irradiation;Zhiguo Yi et al.;《Nature Materials》;20100606(第09期);第559-564页 * |
| Glass Formation and High Conductivity in the Ternary System AgI+Ag3AsO4+ AgPO3: Host to Gassy AgI ?;Steve W.Martin et al.;《The Journal of Physical Chemistry C》;19850531;第89卷(第10期);第2070-2076页 * |
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| Steve W.Martin et al..Glass Formation and High Conductivity in the Ternary System AgI+Ag3AsO4+ AgPO3: Host to Gassy AgI ?.《The Journal of Physical Chemistry C》.1985,第89卷(第10期),第2070-2076页. |
| Xiaoyan Jin et al..A Crucial Role of Bond Covalency Competition in Determining the Bandgap and Photocatalytic Performance of Silver Oxosalts.《The Journal of Physical Chemistry C》.2013,(第117期),第26509-26516页. |
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