CN108772077B - AgIO3/Ag2O heterojunction photocatalytic material and preparation method and application thereof - Google Patents
AgIO3/Ag2O heterojunction photocatalytic material and preparation method and application thereof Download PDFInfo
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910000108 silver(I,III) oxide Inorganic materials 0.000 title description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000002351 wastewater Substances 0.000 claims abstract description 5
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 4
- 229940088710 antibiotic agent Drugs 0.000 claims abstract description 4
- 238000000643 oven drying Methods 0.000 claims abstract description 4
- 239000004098 Tetracycline Substances 0.000 claims description 18
- 229960002180 tetracycline Drugs 0.000 claims description 18
- 229930101283 tetracycline Natural products 0.000 claims description 18
- 235000019364 tetracycline Nutrition 0.000 claims description 18
- 150000003522 tetracyclines Chemical class 0.000 claims description 18
- 238000013329 compounding Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 230000003115 biocidal effect Effects 0.000 claims description 4
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- -1 silver ions Chemical class 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 2
- 239000010815 organic waste Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 description 14
- 238000006731 degradation reaction Methods 0.000 description 14
- 239000011941 photocatalyst Substances 0.000 description 14
- 239000004065 semiconductor Substances 0.000 description 10
- 238000007146 photocatalysis Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
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- 238000005516 engineering process Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 229910001961 silver nitrate Inorganic materials 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
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- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000012855 volatile organic compound Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
- 239000001230 potassium iodate Substances 0.000 description 1
- 235000006666 potassium iodate Nutrition 0.000 description 1
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- 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
- B01J27/06—Halogens; Compounds thereof
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F2101/34—Organic compounds containing oxygen
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Abstract
The invention belongs to the technical field of photocatalytic materials, and particularly relates to AgIO3/Ag2The O heterojunction photocatalytic material is prepared from AgIO3With Ag2And O is compounded. Also relates to a preparation method of the photocatalytic material, and KIO is stirred3The solution is slowly dripped dropwise to AgNO3Adding white precipitate into the solution, gradually adding NaOH solution dropwise to obtain brown flocculent precipitate, stirring, standing to completely precipitate silver ions, washing with distilled water repeatedly, vacuum filtering, and oven drying to obtain AgIO3/Ag2An O heterojunction photocatalytic material. Finally relates to the application of the photocatalytic material, which is used for photocatalytic degradation of antibiotics in wastewater under visible light. The preparation method provided by the invention has the advantages of simple process, easiness in control, lower cost, greenness and no pollution; prepared AgIO3/Ag2The O heterojunction photocatalytic material is tested by ultraviolet visible diffuse reflection, and the photoresponse of the O heterojunction photocatalytic material moves to a visible light area, so that the utilization rate of sunlight is effectively improved, and the application of the O heterojunction photocatalytic material in photocatalytic degradation of volatile organic waste gas can be further expanded.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to AgIO3/Ag2O heterojunction photocatalytic material and preparation method and application thereof.
Background
The photocatalysis technology is a clean light energy utilization substance conversion technology, and the application fields of the photocatalysis technology comprise hydrogen production by photolysis water, photocatalytic degradation, antibiosis and deodorization, organic pollutants, degradation of Volatile Organic Compounds (VOCs) in air, metal ions in treatment and the like. The technology of realizing photocatalytic reaction by means of semiconductor materials is more and more widely concerned, the semiconductor materials can generate electron-hole pairs under illumination, one part of electrons and holes meet in a bulk phase or on the surface to be compounded, and the other part of electrons migrate to the surface of the semiconductor, have stronger reducing capacity and can be combined with adsorbed oxygen to generate free radicals with strong oxidizing property; the holes transferred to the surface of the semiconductor have strong oxidizing power and can be combined with OH-and H adsorbed on the surface of the semiconductor2O is combined to form, for example, OH, HO2、H2O2And O2 -The free radicals can directly react with reactants and oxidize and decompose the reactants, and secondary pollution is avoided. In semiconductor photocatalysis technology, the key to improving photocatalysis efficiency is to reduce forbidden bandwidth, improve the utilization rate of light quantum, improve the visible light responsibility of semiconductor and avoid the recombination of photo-generated electron-hole pairs.
As is well known, Ag-based semiconductor catalysts are an important class of photocatalysts having visible light-responsive properties. The silver oxide belongs to a p-type semiconductor, has a forbidden band width of 1.3eV, has a response wavelength in a visible light region, has strong absorption, and is one of high-activity and high-selectivity narrow-band-gap photocatalytic materials. But Ag alone2The O-photocatalyst has poor separation efficiency of photo-generated electrons-holes, thus limiting its ultimate photocatalytic efficiency.
Disclosure of Invention
The invention aims to solve the technical problem of providing an AgIO3/Ag2O-heterojunction photocatalytic material and preparation method and application thereof, and Ag is prepared by mixing Ag2O and AgIO3Hybridization is carried out to form the composite photocatalyst, and the application of the composite photocatalyst in the field of photocatalysis is expanded.
The invention is realized by the following steps:
the invention firstly provides an AgIO3/Ag2The O heterojunction photocatalytic material is prepared from AgIO3With Ag2And O is compounded.
Wherein, AgIO3With Ag2The compounding proportion of O is 100-200%, the compounding proportion is a molar ratio, and the meaning of the compounding proportion is AgIO3Is in Ag2Molar weight ratio of O.
More preferably, AgIO3With Ag2The compounding ratio of O was 125%.
Further, the Ag2The O is prepared from sodium hydroxide solution and silver nitrate solution by room temperature liquid phase precipitation method.
Further, the AgIO3Is synthesized by taking silver nitrate and potassium iodate as raw materials and utilizing a precipitation method.
The invention also provides a preparation method of the photocatalytic material, which comprises the following steps:
mixing KIO under stirring3The solution is slowly dripped dropwise to AgNO3Adding white precipitate into the solution, gradually adding NaOH solution dropwise to obtain brown flocculent precipitate, stirring, standing to completely precipitate silver ions, washing with distilled water repeatedly, vacuum filtering, and oven drying to obtain AgIO3/Ag2An O heterojunction photocatalytic material.
Wherein the concentration of the NaOH solution is 0.2 mol/L.
Finally, the invention provides application of the photocatalytic material to photocatalytic degradation of antibiotics in wastewater under visible light.
The antibiotic comprises tetracycline.
The invention has the following advantages:
(1) the preparation method provided by the invention has the advantages of simple process, easiness in control, lower cost, greenness and no pollution;
(2) AgIO prepared by the invention3/Ag2The O heterojunction photocatalytic material is tested by ultraviolet visible diffuse reflection, and the light response of the O heterojunction photocatalytic material moves to a visible light area, so that the utilization rate of sunlight is effectively improved. Its visible light catalytic activity ratio AgIO3And Ag2The O is obviously improved, and the degradation rate of 20mg/L tetracycline in the wastewater within 60min is good under the irradiation of a xenon lamp light source with a 420nm optical filter.
(3) AgIO prepared by the invention3/Ag2O heterojunction photocatalyst and pure AgIO in photocurrent test3And Ag2Compared with O, the O has larger photocurrent, and the special heterojunction structure accelerates the separation efficiency of photon-generated carriers, reduces the recombination probability of photon-generated electron-hole pairs, improves the visible light catalytic activity and stability of the photocatalyst, improves the utilization rate of visible light, and can further expand the application of the photocatalyst in the photocatalytic degradation of volatile organic waste gas.
Drawings
The invention will be further described with reference to the following examples with reference to the accompanying drawings.
FIG. 1 is an X-ray diffraction (XRD) pattern of a sample prepared according to the present invention, the abscissa of the pattern being 2 θ (angle) in degrees (°); intensity on the ordinate, in a.u. (absolute units);
fig. 2 is a scanning electron microscope (FESEM) photograph of a sample prepared according to the present invention, wherein a: ag2O，B：AgIO3，C：AgIO3/Ag2O＝1：1，D：AgIO3/Ag2O＝1.25：1，E：AgIO3/Ag2O＝1.75： 1，F：AgIO3/Ag2O＝2：1；
FIG. 3 is a graph of the ultraviolet-visible diffuse reflectance spectrum (UV-DIS) of a sample prepared in accordance with the present invention, wherein the abscissa is the Wavelength (Wavelength) in nm (nanometers) and the ordinate is the Absorbance (Absorbance) in a.u. (absolute units);
FIG. 4 shows (. alpha.h v) of a sample prepared by the present invention1/2Hs v spectrogram with abscissa h v, unit eV (electron volts) and ordinate (α h v)0.5The unit is dimensionless;
FIG. 5 is a graph of the change of tetracycline degradation by photocatalysis of a sample prepared by the present invention with the abscissa being Time in min (minutes) and the ordinate being C/C0，C0Initial concentration of tetracycline before reaction initiation, C is samplingThe concentration of tetracycline over time;
FIG. 6 shows AgIO prepared according to the present invention3：Ag2The x-ray visible absorption spectrum of the sample with O ═ 125%, the lines from top to bottom in the picture represent the sampling times of-30 min, 0min, 10min, 20min, 30min, 40min, 50min, and 60min, respectively, with the abscissa being Wavelength (Wavelength) and the unit being nm (nanometers) and the ordinate being absorbanc (absorbance) and the unit being a.u (absolute unit).
Detailed Description
Example 1
Mixing a certain proportion of AgNO3And KIO3(AgIO3:Ag2O ═ 1:1, 1.25:1, 1.5:1, 1.75:1, 2:1) were dissolved in 20ml and 10ml of distilled water, respectively, and a 0.2mol/L NaOH solution was prepared. KIO is stirred under a magnetic stirrer3The solution is slowly dripped dropwise into the corresponding AgNO containing solution3In the beaker of the solution, a white precipitate appeared (AgIO)3) After the reaction is completed, respectively dropping 20ml of NaOH solution gradually to form brown flocculent precipitate (producing Ag)2O). Stirring for 1 hr, standing to precipitate silver ion completely, washing with distilled water repeatedly, vacuum filtering, and drying at 60 deg.C to obtain AgIO with different proportions3:Ag2An O heterojunction composite material.
Comparative example 1: ag2Preparation of O
Preparing Ag by adopting a simple room-temperature liquid-phase precipitation method2And (4) O sample. Dissolving 4mmol of silver nitrate in 20ml of water, preparing 20.0ml of 0.2mol/L sodium hydroxide solution, dropwise and slowly dropping the sodium hydroxide solution into the silver nitrate solution under magnetic stirring, continuously stirring for 5min after the dropwise addition is finished, and standing to completely precipitate silver ions. Repeatedly washing with ethanol and distilled water, filtering, collecting, and oven drying at 60 deg.C to obtain Ag2And (4) O sample.
Comparative example 2: AgIO3Preparation of
Preparation of AgIO by precipitation3. 2mmol of AgNO3And KIO3Respectively dissolved in 30ml of deionized water and stirred continuously until the solution is dissolved. Mixing KIO3The solution is dropwise added to AgNO3In solution, there was a white precipitateAnd (3) precipitating, continuously stirring for 30min until the reaction is complete, repeatedly washing the sample with ethanol and distilled water, filtering and collecting, and drying at 60 ℃ for 10h to obtain the sample.
Photocatalytic activity test method of the above examples, comparative examples:
a PLS-SXE300 xenon lamp light source is adopted, 50mg of photocatalyst is weighed and added into 200ml of 20mg/L tetracycline solution, dark reaction is carried out for 30min, and the light source is started after adsorption balance is achieved. The tetracycline solution concentration was measured by an ultraviolet-visible spectrophotometer, and the degradation efficiency was calculated (degradation efficiency was C/C0, C0 was the initial concentration of tetracycline before the start of the reaction, and C was the concentration of tetracycline at the time of sampling).
And (4) analyzing results:
FIG. 1 shows AgIO prepared at different molar ratios3/Ag2And O, sample XRD spectrum. AgIO can be seen from the figure3、Ag2Diffraction peaks of O and AgIO of orthorhombic crystal form3(JCPDS45-0880)、Ag2O (JCPDS41-1104) is consistent and no impurity peak exists, which indicates that AgIO is successfully prepared by the experiment3And Ag2And O. And the diffraction peak shapes of the two substances are sharp, which shows that the crystallinity is good. By AgIO3/Ag2The diffraction peak spectra of the composite materials with O1: 1, 1.25:1 and 1.5:1 show that the heterojunction composite contains AgIO3And Ag2Diffraction peak of O, and no impurity peak, wherein diffraction peaks at 2 θ of 38.1 °, 54.9 ° and 65.5 ° correspond to Ag, respectively2The (200), (220) and (311) crystal planes of O, and along with Ag2The content of O in the heterojunction is increased, and the peak intensity is increased, which is consistent with the synthesis result.
For further discussion of the different molar ratios AgIO3/Ag2And (4) observing the sample by adopting SEM (scanning electron microscope) under the influence of the micro-morphology of the O sample. FIG. 2A and FIG. 2B show Ag2O and AgIO3The electron micrograph of Ag2O is aggregated particles having a diameter of about 50 to 100 nm; AgIO3It is an irregular sheet structure with smooth surface, flat cuboid appearance, 3 micron length and 1 micron width. FIG. 2C-FIG. 2F are all AgIO3/Ag2O complexComposite materials with AgIO3The proportion is increased, the shape of the sample is not basically changed, but the Ag with agglomeration growth is visible in the visual field2Flat cuboid AgIO in O particles3Increased amount of Ag2The heterojunction interface formed by O increases.
FIG. 3 is AgIO3、Ag2O and synthetic AgIO3/Ag2An ultraviolet-visible diffuse reflectance spectrum of an O-heterojunction photocatalyst sample. AgIO in the figure3The absorption peak of the monomer is around 380nm, and Ag2The absorption peak of O covers the UV to visible region, indicating AgIO3Ag responsive only to UV light2The photoresponsive region of O extends from the ultraviolet to the visible region. AgIO3Carrying Ag2After O, AgIO3/Ag2Absorption peak edge of O composite material is compared with pure Ag2O and AgIO3All move to the visible light area, show that it has stronger visible light absorbing capacity, has improved the utilization ratio of visible light. The result shows that the light response performance of the hybrid heterojunction photocatalyst is superior to that of monomer AgIO3And Ag2And O. The absorption peak edge is closely related to the forbidden band width of the photocatalyst, so that the method can be used for predicting the light absorption area of a sample, and can be used for estimating the forbidden band width of the sample based on the semiconductor light absorption theory and the result of UV-DIS. The forbidden bandwidth of the sample, AgIO, was calculated by the Taucplot method (FIG. 4)3And Ag2The forbidden band widths of O are respectively 3.38eV and 1.3eV, and are basically consistent with those of the two reported in other literatures.
FIG. 5 is AgIO3、Ag2O and synthetic AgIO3/Ag2A graph of the degradation efficiency of a 200ml tetracycline sample having a concentration of 20mg/l for the O heterojunction photocatalyst sample. As can be seen from the figure, the monomer AgIO3When the light degradation is carried out for 40min, the degradation rate is only 35 percent; and Ag2O has almost no degradation effect on tetracycline, and the degradation efficiency is only 10%; and AgIO3/Ag2The O heterojunction photocatalyst shows better photocatalytic effect, especially AgIO3：Ag2125% O of the sample, which is at 6The light degradation efficiency of the tetracycline in 0min reaches 97%.
FIG. 6 shows AgIO at different sampling times for 200ml tetracycline at 20mg/l concentration3: the ultraviolet-visible absorption spectrum of the sample is 125 percent Ag 2O. As can be clearly seen from the figure, as time goes on, the tetracycline is significantly degraded, the absorption peak of the tetracycline at 355nm can be seen to disappear within 60 minutes, which represents that the tetracycline is degraded to a certain extent, and the degradation rate reaches the maximum of about 97% at 60 min.
In conclusion, Ag2O and AgIO3The catalyst can not achieve good effect when independently participating in visible light photocatalytic degradation reaction, the degradation rates of the catalyst and the catalyst to antibiotics in wastewater within 60min are respectively about 10% and 35%, but AgIO is used3And Ag2After compounding of O, at AgIO3And Ag2The compound ratio of O is within 100-200%, and when AgIO is used, good photocatalysis effect can be obtained3:Ag2When the content of O is 125%, the degradation rate of the antibiotic (tetracycline) in 60min reaches 97%. AgIO prepared according to the invention3/Ag2The O heterojunction photocatalyst has great significance when being applied to the field of photocatalysis.
Although specific embodiments of the invention have been described above, it will be understood by those skilled in the art that the specific embodiments described are illustrative only and are not limiting upon the scope of the invention, and that equivalent modifications and variations can be made by those skilled in the art without departing from the spirit of the invention, which is to be limited only by the appended claims.
Claims (3)
1. AgIO3/Ag2An O heterojunction photocatalytic material, characterized in that: is made of AgIO3With Ag2Formed by O compounding, AgIO3With Ag2The compounding proportion of O is 125 percent; the preparation method comprises the following steps:
mixing KIO under stirring3The solution is slowly dripped dropwise to AgNO3White precipitate is generated in the solution, and then NaOH solution is gradually droppedLiquid with brown flocculent precipitate, stirring, standing to precipitate silver ion completely, washing with distilled water repeatedly, vacuum filtering, and oven drying to obtain AgIO3/Ag2An O heterojunction photocatalytic material.
2. The AgIO of claim 13/Ag2Use of an O-heterojunction photocatalytic material, characterized in that: the AgIO3/Ag2The O heterojunction photocatalytic material is used for photocatalytic degradation of antibiotics in wastewater under visible light.
3. The AgIO of claim 23/Ag2Use of an O-heterojunction photocatalytic material, characterized in that: the antibiotic comprises tetracycline.
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| CN113559856B (en) * | 2021-07-30 | 2023-12-22 | 陕西科技大学 | Preparation method of barium titanate/silver iodate heterojunction photocatalyst |
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