CN113856661A - Ag3PO4/Bi2WO6Preparation method and application of/rGO visible light catalyst - Google Patents
Ag3PO4/Bi2WO6Preparation method and application of/rGO visible light catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims description 5
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000012855 volatile organic compound Substances 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 230000000593 degrading effect Effects 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 238000005406 washing Methods 0.000 claims description 25
- 239000012153 distilled water Substances 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 7
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 7
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims 2
- 238000001816 cooling Methods 0.000 claims 1
- 239000012467 final product Substances 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 6
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 238000007598 dipping method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 230000004298 light response Effects 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 5
- 229910000397 disodium phosphate Inorganic materials 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000159 acid neutralizing agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/8687—Organic components
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
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- B01D2257/708—Volatile organic compounds V.O.C.'s
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- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/802—Visible light
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Abstract
Ag3PO4/Bi2WO6A preparation method and application of a/rGO visible light catalyst relate to a preparation method of a synthetic catalyst. The invention is thatSolves the problem of the Bi prepared at present2WO6When the catalyst is used for degrading VOCs in a photocatalytic manner, the technical problems of small visible light response range and easy recombination of electrons and holes exist. Preparation of Bi by hydrothermal method2WO6Then synthesizing ternary Ag by dipping and stirring3PO4/Bi2WO6and/rGO is washed and dried after reaction to obtain the nano photocatalytic material. The present invention prepares catalysts by varying the loading of rGO. The invention has simple operation, no toxicity and single Bi2WO6Compared with the photocatalyst with higher photocatalytic activity, the photocatalyst has the best effect when the loading of the rGO is 5%.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and discloses Ag3PO4/Bi2WO6Preparation method and application of/rGO visible light catalyst.
Background
The rapid development of the Chinese socioeconomic industry has led to an increase in the concentration of Volatile Organic Compounds (VOCs) released into the atmosphere year by year. VOCs entering the air, even at low concentrations, can cause significant harm to the health of the human body. In 2020, the ministry of environmental protection issues '2020 volatile organic compound treatment and hardness-attacking scheme', and treatment of VOCs is enhanced through accurate, scientific and legal pollution treatment. In recent years, people pay attention to the application of semiconductor photocatalysis technology, and the photocatalysis technology has the characteristics of low energy consumption, mild experimental conditions, no secondary pollution and the like and is widely used for degrading volatile organic pollutants. Among many semiconductor photocatalytic materials, conventional photocatalysts such as TiO2And ZnO and the like have larger forbidden band width and low sunlight utilization rate, and can only realize 4% of visible light, and in recent years, researchers strive to develop novel visible light catalysts. Bi2WO6Bi is used due to the proper forbidden band width and high photocatalytic activity under visible light2WO6The catalytic material opens up a new way for removing volatile organic pollutants.
Ag3PO4Is a semiconductor photocatalyst emerging in recent years, has the forbidden band width of 2.36-2.43 eV, the absorption sideband can reach 530 nm, and the absorption lambda can be absorbed<The quantum efficiency of 530 nm ultraviolet-visible light can reach 92%, the photoresponse efficiency is far higher than that of other photocatalysts, and the photocatalyst has excellent organic matter degradation performance.
Graphene is a monolayer of carbon atoms in sp2The hybrid tracks are connected to form a stable benzene six-membered ring structure, and the benzene six-membered ring structure has a large specific surface area and ultrahigh carrier mobility. The graphene oxide is obtained by chemically oxidizing and stripping graphene, contains a large number of oxygen-containing functional groups such as-OH, C-O-C and-COOH on the surface and the edge, and has the characteristics of large specific surface area and high electron mobility.
According to the performance advantages of the three components, a heterojunction is formed, and the effective separation of electrons and holes is promoted, so that the performance of degrading toluene by photocatalysis is improved.
Disclosure of Invention
The invention aims to prepare Bi by adopting a hydrothermal method2WO6The rGO/Bi is prepared by reducing with a reducing agent2WO6Then loading Ag by dipping method3PO4To obtain a three-way catalyst Ag3PO4/Bi2WO6rGO, a method for greatly improving the capability of degrading VOCs by photocatalysis.
The visible light catalyst Ag3PO4/Bi2WO6The preparation method of/rGO comprises the following steps:
step 1, Bi2WO6The preparation method comprises the steps of dissolving bismuth nitrate, sodium tungstate and hexadecyl trimethyl ammonium bromide in 80ml of distilled water, stirring the solution for 1 hour under magnetic stirring, uniformly stirring the solution, transferring the solution to a polytetrafluoroethylene-lined high-pressure reaction kettle, setting certain hydrothermal temperature and hydrothermal time, finishing the reaction, centrifuging, washing with water, washing with alcohol, and freeze-drying.
Further, the molar ratio of bismuth nitrate to sodium tungstate in step 1 was 2:1, and the content of cetyltrimethylammonium bromide was 0.05 g.
And further, transferring the product obtained by stirring for 1 hour in the step 1 to a polytetrafluoroethylene-lined high-pressure reaction kettle, carrying out hydrothermal temperature of 160 ℃ and hydrothermal time of 24 hours, after the reaction is finished, carrying out centrifugal washing on the product, and carrying out freeze drying treatment.
Further, in step 1, the catalyst is centrifugally washed at a centrifugal speed of 10000 rpm/min, and the washing is carried out by exchanging and washing with ethanol and distilled water for three times respectively.
Further, GO is pressed (Ag) in step 23PO4+ Bi2WO6) The mass ratio loads are 3%, 5% and 7%.
Further, the GO solution is dripped into the GO in the step 2 at a rate of 20-30 drops/min.
Further, the neutralization agent in the step 2 is centrifugally washed, the centrifugal speed is 10000 rpm/min, and the washing is respectively washed three times by exchanging ethanol and distilled water.
Further, Ag in step 33PO4And Bi2WO6The molar ratio is 1: 2.
further, NH in step 33·H2The O concentration was 2 wt%.
Further, the pH value of the mixed solution in the step 3 is adjusted by adopting 1M HNO3。
Further, step 3 is Na2HPO4·12H2The O solution is dropped into the solution at a rate of 20 to 30 drops/min.
Further, the catalyst in step 3 was washed with water by centrifugation at a rate of 10000 rpm/min.
The visible light catalyst Ag3PO4/Bi2WO6Application of/rGO in catalytic degradation of VOCs under visible light conditions, lightThe source was a 1000W xenon lamp, 10 cm above the reaction system.
The invention prepares Ag3PO4/Bi2WO6The charge separation efficiency of the/rGO photocatalytic material in the forming process is relatively pure Bi2WO6Certain change occurs, and the catalytic performance of the material is improved. The material obtained in the step 3 is detected to be Ag3PO4/Bi2WO6/rGO。
Drawings
FIG. 1 shows Ag3PO4/Bi2WO6、Ag3PO4And Bi2WO6An XRD pattern of (a);
FIG. 2 shows Ag loading for different GO in examples 1-33PO4/Bi2WO6XRD patterns of/rGO and rGO;
FIG. 3 shows Ag in the example3PO4/Bi2WO6/rGO、Ag3PO4And Bi2WO6Photocatalytic toluene degradation performance curve under visible light.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
Step 1, Bi2WO6The preparation method comprises the steps of dissolving bismuth nitrate, sodium tungstate and hexadecyl trimethyl ammonium bromide in 80ml of distilled water, stirring the solution for 1 hour under magnetic stirring, uniformly stirring the solution, transferring the solution to a polytetrafluoroethylene-lined high-pressure reaction kettle, setting certain hydrothermal temperature and hydrothermal time, finishing the reaction, centrifuging, washing with water, washing with alcohol, and freeze-drying.
Example 2
Step 1, Bi2WO6The preparation method comprises the steps of dissolving bismuth nitrate, sodium tungstate and hexadecyl trimethyl ammonium bromide in 80ml of distilled water, stirring the solution for 1 hour under magnetic stirring, uniformly stirring the solution, transferring the solution to a polytetrafluoroethylene-lined high-pressure reaction kettle, setting certain hydrothermal temperature and hydrothermal time, finishing the reaction, centrifuging, washing with water, washing with alcohol, and freeze-drying.
Example 3
Step 1, Bi2WO6The preparation method comprises the steps of dissolving bismuth nitrate, sodium tungstate and hexadecyl trimethyl ammonium bromide in 80ml of distilled water, stirring the solution for 1 hour under magnetic stirring, uniformly stirring the solution, transferring the solution to a polytetrafluoroethylene-lined high-pressure reaction kettle, setting certain hydrothermal temperature and hydrothermal time, finishing the reaction, centrifuging, washing with water, washing with alcohol, and freeze-drying.
Claims (9)
1. Ag3PO4/Bi2WO6the/rGO visible light catalyst is characterized by consisting of 3-7wt% (Ag)3PO＋Bi2WO6) And the balance rGO, wherein Ag3PO4：Bi2WO6The molar ratio is 1: 2.
2. the Ag of claim 13PO4/Bi2WO6The preparation method of the/rGO visible light catalyst is characterized by comprising the following steps:
step 1, adopting water heatingMethod for preparing Bi2WO6: dissolving bismuth nitrate, sodium tungstate and hexadecyl trimethyl ammonium bromide in distilled water, magnetically stirring for 1 h, transferring the mixed solution to a polytetrafluoroethylene-lined high-pressure reaction kettle, setting the hydrothermal reaction temperature to 160 ℃, carrying out hydrothermal reaction for 24 h, and after the hydrothermal reaction is finished, centrifugally washing, washing with water, washing with alcohol, and freeze-drying to obtain Bi2WO6；
Step 2, Bi obtained in the step 1 is added2WO6Dissolving GO in distilled water, and respectively performing ultrasonic treatment for 1 h; adding Bi2WO6Transferring the solution to a three-neck flask, slowly adding the GO solution into the three-neck flask, and stirring the mixed solution for 1 h; as m (hydrazine hydrate): m (GO) =7:10 hydrazine hydrate is added, and stirring is carried out at 95 ℃ for 12 hours; cooling the solution, then carrying out suction filtration, centrifugal washing, water washing and alcohol washing;
step 3, AgNO3The solution was dropped into NH 2wt%3·H2O solution, then HNO is dropped3Dissolving to obtain mixed solution A, adjusting pH of the mixed solution A to neutral with 1M HNO3, adding the product obtained in step 2 into the mixed solution A, stirring for 30min, and adding Na dropwise at a rate of 20-30 drops/min2HPO4·12H2And stirring, centrifuging, washing, freeze-drying and finally grinding the O solution to obtain a final product.
3. Ag according to claim 23PO4/Bi2WO6The preparation method of the/rGO visible light catalyst is characterized by comprising the following steps: in the step 1, the molar ratio of bismuth nitrate to sodium tungstate is 2:1, and the content of cetyl trimethyl ammonium bromide is 0.5 wt%.
4. Ag according to claim 23PO4/Bi2WO6The preparation method of the/rGO visible light catalyst is characterized by comprising the following steps: in the step 1, centrifugally washing a product after the hydrothermal reaction is finished, wherein the centrifugal speed is 10000 rpm/min; the water washing and the alcohol washing are alternately carried out for three times.
5. The method of claim 2Ag of (A)3PO4/Bi2WO6The preparation method of the/rGO visible light catalyst is characterized by comprising the following steps: in the step 2 according to (Ag)3PO4+Bi2WO6) GO is required to be added when the load is 3-7 wt%.
6. Ag according to claim 23PO4/Bi2WO6The preparation method of the/rGO visible light catalyst is characterized by comprising the following steps: and in the step 2, the GO solution is dripped at a rate of 20-30 drops/min.
7. Ag according to claim 23PO4/Bi2WO6The preparation method of the/rGO visible light catalyst is characterized by comprising the following steps: the centrifugal rate is 10000 rpm/min when the centrifugal washing in the step 2 is carried out; the water washing and the alcohol washing are alternately carried out for three times.
8. Ag according to claim 23PO4/Bi2WO6The preparation method of the/rGO visible light catalyst is characterized by comprising the following steps: in the step 3, Ag is added3PO4In an amount corresponding to Bi in step 22WO6The molar ratio is 1: 2 is added.
9. The Ag of claim 13PO4/Bi2WO6The application of the/rGO visible light catalyst is used for catalyzing and degrading VOCs under the condition of visible light.
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| CN116550350A (en) * | 2023-05-14 | 2023-08-08 | 广州绿固环保科技有限公司 | Environment-friendly formaldehyde purifying agent and preparation method and application thereof |
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| 姚慧等: ""全固态Z型Ag3PO4/RGO/Bi2WO6三元复合光催化剂可见光驱动高效降解四环素"", 《化学试剂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116550350A (en) * | 2023-05-14 | 2023-08-08 | 广州绿固环保科技有限公司 | Environment-friendly formaldehyde purifying agent and preparation method and application thereof |
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Application publication date: 20211231 |