CN110237802B - Bismuth-bismuth tungstate-bismuth oxybromide ternary compound and preparation method and application thereof - Google Patents
Bismuth-bismuth tungstate-bismuth oxybromide ternary compound and preparation method and application thereof Download PDFInfo
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- IYNWNKYVHCVUCJ-UHFFFAOYSA-N bismuth Chemical compound [Bi].[Bi] IYNWNKYVHCVUCJ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 150000001875 compounds Chemical class 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000000243 solution Substances 0.000 claims abstract description 56
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims abstract description 46
- 238000001179 sorption measurement Methods 0.000 claims abstract description 41
- VQHHOXOLUXRQFQ-UHFFFAOYSA-L dipotassium;4,5,6,7-tetrachloro-2',4',5',7'-tetraiodo-3-oxospiro[2-benzofuran-1,9'-xanthene]-3',6'-diolate Chemical compound [K+].[K+].O1C(=O)C(C(=C(Cl)C(Cl)=C2Cl)Cl)=C2C21C1=CC(I)=C([O-])C(I)=C1OC1=C(I)C([O-])=C(I)C=C21 VQHHOXOLUXRQFQ-UHFFFAOYSA-L 0.000 claims abstract description 31
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 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 abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 238000004729 solvothermal method Methods 0.000 claims abstract description 11
- 229910052797 bismuth Inorganic materials 0.000 claims description 36
- OZKCXDPUSFUPRJ-UHFFFAOYSA-N oxobismuth;hydrobromide Chemical compound Br.[Bi]=O OZKCXDPUSFUPRJ-UHFFFAOYSA-N 0.000 claims description 28
- 230000001699 photocatalysis Effects 0.000 claims description 23
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 19
- 239000010865 sewage Substances 0.000 claims description 17
- 239000002135 nanosheet Substances 0.000 claims description 13
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- 238000007146 photocatalysis Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 20
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- 125000002091 cationic group Chemical group 0.000 abstract description 5
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- 238000011056 performance test Methods 0.000 description 10
- 239000004065 semiconductor Substances 0.000 description 9
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 8
- 239000011941 photocatalyst Substances 0.000 description 8
- 239000003463 adsorbent Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011206 ternary composite Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000000975 dye Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 229910001451 bismuth ion Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- 239000003344 environmental pollutant Substances 0.000 description 3
- 239000002057 nanoflower Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
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- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 2
- XTHCXHPOZDCVNJ-UHFFFAOYSA-N O(Br)Br.[Bi].[Bi] Chemical compound O(Br)Br.[Bi].[Bi] XTHCXHPOZDCVNJ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000032900 absorption of visible light Effects 0.000 description 2
- 239000011218 binary composite Substances 0.000 description 2
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- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
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- 229910001507 metal halide Inorganic materials 0.000 description 2
- 150000005309 metal halides Chemical class 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
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- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
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- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- OLBRKKJBIBPJSE-UHFFFAOYSA-N bismuth;bromo hypobromite Chemical compound [Bi].BrOBr OLBRKKJBIBPJSE-UHFFFAOYSA-N 0.000 description 1
- 229940006460 bromide ion Drugs 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
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- 238000006862 quantum yield reaction Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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Abstract
The invention discloses a bismuth-bismuth tungstate-bismuth oxybromide ternary compound and a preparation method and application thereof. The method comprises the following steps: adding bismuth nitrate into ethylene glycol, and uniformly stirring to obtain a solution A; adding sodium tungstate and potassium bromide into ethylene glycol, and uniformly stirring to obtain a solution B; dropwise adding the solution B into the solution A, and uniformly stirring to obtain a mixed solution; transferring the mixed solution to a hydrothermal kettle for solvothermal reaction; wherein the molar ratio of bismuth nitrate to sodium tungstate to potassium bromide in the mixed solution is 2:1 (0.5-5). Bi/Bi with nano structure prepared by the method of the invention2WO6the/BiOBr ternary complex has strong adsorption and visible light degradation effects on the cationic dye rose bengal B in water.
Description
Technical Field
The invention belongs to the field of semiconductor nano materials, and particularly relates to a composite semiconductor nano material containing bismuth, bismuth tungstate and bismuth oxybromide, a preparation method thereof and application of the composite semiconductor nano material in sewage treatment.
Background
With the rapid development of the industry in China, the problem of water pollution is increasingly severe, and sewage treatment is widely concerned by people. The sewage treatment method is various and comprises an adsorption method, a photocatalysis method, a chemical deposition method, a chemical oxidation method, a biodegradation method and the like. Among them, the adsorption method is a simple, low-cost and high-efficiency sewage treatment technique. Commonly used adsorbents are activated carbon, graphene, natural polymer materials, etc., but the development of these materials is limited by their expensive price and complicated processing procedures. In recent years, the nano material adsorbent with controllable shape and size is favored by people. The photocatalysis technology taking the semiconductor material as the leading factor has the advantages of economy, high efficiency, environmental friendliness, wide application range and the like in sewage treatment, and is an extremely active research direction in the field of sewage treatment.
The reserves of bismuth (Bi) resources in China are at the top of the world, and Bi semiconductor family members are numerous. Bismuth oxybromide (BiOBr) is a p-type semiconductor material, has the forbidden band width of 2.75eV, has a special layered structure, high photocatalytic activity, good chemical stability and environmental friendliness. Researchers find that the BiOBr-based nano material has adsorption and photocatalysis effects on organic dyes and heavy metal ions in water, and the development of a novel high-efficiency BiOBr-based nano material is a research hotspot in the field of sewage treatment.
Bismuth tungstate (Bi)2WO6) The material is a typical n-type semiconductor, has the forbidden band width of about 2.8eV, has various shapes and good stability, can respond to most visible light in a solar spectrum, has a proper valence band position, has strong oxidizing capability and is one of the most promising photocatalytic materials. However, Bi2WO6The quantum yield of the photocatalyst is far from expectation, and the photocatalytic efficiency can be effectively improved by modifying the photocatalyst.
Disclosure of Invention
The invention aims to modify a bismuth oxybromide and bismuth tungstate composite system and construct bismuth-bismuth tungstate-bismuth oxybromide (Bi/Bi)2WO6a/BiOBr) ternary heterostructure, providing a Bi/Bi with a nano-structure2WO6the/BiOBr ternary complex has strong adsorption and visible light degradation effects on the cationic dye rose bengal B in water.
According to one aspect of the invention, a method for preparing a bismuth-bismuth tungstate-bismuth oxybromide ternary complex is provided, which comprises the following steps:
step 1, adding bismuth nitrate into ethylene glycol, and uniformly stirring to obtain a solution A;
step 3, dropwise adding the solution B into the solution A, and uniformly stirring to obtain a mixed solution;
wherein the molar ratio of bismuth nitrate to sodium tungstate to potassium bromide in the mixed solution is 2:1 (0.5-5).
Preferably, in the step 4, the temperature of the solvothermal reaction is 120-220 ℃, and the reaction time is 1-40 h.
Preferably, in the step 1, the concentration of bismuth nitrate in the solution A is 0.1-1M.
In the step 2, the concentration of sodium tungstate in the solution B is 0.05-0.5M.
Further, in the step (2), the molar ratio of sodium tungstate to potassium bromide in the solution B is 1: (0.5-5).
According to another aspect of the present invention, there is provided a bismuth-bismuth tungstate-bismuth oxybromide ternary complex prepared by the above method.
Specifically, the bismuth-bismuth tungstate-bismuth oxybromide ternary complex has a nano-sheet structure and nano-particles distributed in the nano-sheet structure. The nano-sheet structure is composed of bismuth oxybromide sheets, and the nano-particles are composed of bismuth tungstate particles and bismuth elementary substance particles.
According to another aspect of the invention, the application of the bismuth-bismuth tungstate-bismuth oxybromide ternary compound for treating sewage is provided.
The bismuth-bismuth tungstate-bismuth oxybromide ternary compound prepared by the method has a large specific surface area and a composite energy band structure, and has strong adsorption and visible light degradation effects on a cationic dye rose bengal B in water.
Drawings
Fig. 1 shows the XRD pattern of the bismuth-bismuth tungstate-bismuth oxybromide ternary complex according to example 1.
Fig. 2 shows an SEM characterization of the bismuth-bismuth tungstate-bismuth oxybromide ternary complex according to example 1.
Figure 3 shows EDS characterization plots of the bismuth-bismuth tungstate-bismuth oxybromide ternary complex according to example 1.
FIG. 4 shows N of bismuth-bismuth tungstate-bismuth oxybromide ternary complex according to example 12Adsorption and desorption curves.
Fig. 5 shows adsorption curves of bismuth tungstate, bismuth oxybromide, a binary bismuth-bismuth tungstate composite, a binary bismuth-bismuth oxybromide composite, a ternary bismuth-bismuth tungstate-bismuth oxyiodide composite, and a ternary bismuth-bismuth tungstate-bismuth oxybromide composite for rose bengal B.
Fig. 6 shows the photocatalytic degradation curves of bismuth tungstate, bismuth oxybromide, a binary bismuth-bismuth tungstate composite, a binary bismuth-bismuth oxybromide composite, a ternary bismuth-bismuth tungstate-bismuth oxyiodide composite, and a ternary bismuth-bismuth tungstate-bismuth oxybromide composite for rose bengal B.
Detailed Description
The invention provides a method for preparing a bismuth-bismuth tungstate-bismuth oxybromide ternary compound, which comprises the following steps of:
step 1, adding bismuth nitrate into ethylene glycol, and uniformly stirring to obtain a solution A;
step 3, dropwise adding the solution B into the solution A, and uniformly stirring to obtain a mixed solution;
wherein the molar ratio of bismuth nitrate to sodium tungstate to potassium bromide in the mixed solution is 2:1 (0.5-5).
Preferably, in the step 1, the concentration of bismuth nitrate in the solution A is 0.1-1M.
In the step 2, in the solution B, the concentration of sodium tungstate is 0.05-0.5M; the molar ratio of bismuth nitrate to sodium tungstate is 2: 1; the molar ratio of sodium tungstate to potassium bromide is 1 (0.5-5).
In the step 4, the temperature of the solvothermal reaction is 120-220 ℃, and the reaction time is 1-40 h.
Preferably, in the step 3, the solution B is slowly dripped into the solution A, preferably, the dripping time is 10-60 min, and the stirring time is 10-60 min.
According to a specific embodiment, in the step 4, the mixed solution is preferably transferred to a teflon inner container with a steel sleeve, and is placed in an oven for solvothermal reaction.
Preferably, after the reaction of step 4 is completed, the reactant is centrifuged, repeatedly cleaned with deionized water and ethanol by ultrasonic waves, and then vacuum-dried to obtain the above-mentioned compound in powder form.
In the above method of the present invention, bismuth nitrate, sodium tungstate and potassium bromide are first ionized in an ethylene glycol solvent, and then a part of bismuth ions (Bi) are partially ionized3+) And tungstate radical (WO)6 6-) Combining to form bismuth tungstate, and nucleating and growing; a part of bismuth ions Becomes (BiO)2 2+Ion, and bromide ion Br-The bismuth oxybromide BiOBr is combined and formed by nucleation and growth. The simple bismuth is formed because the ethylene glycol has reducibility at high temperature, so that a part of bismuth ions are reduced to the zero-valent bismuth simple substance.
Thus, semiconductor materials BiOBr and Bi2WO6The p-n heterostructure compound is compositely constructed, the pair of the photo-generated electrons and the holes is transferred to the surfaces of different substances by forming a step-type composite energy band structure, and the transfer and separation of the photo-generated electrons and the holes are effectively promoted, so that the high-efficiency photocatalyst is obtained. Meanwhile, the metal Bi has a plasma resonance effect similar to noble metals such as Au, Ag, Pt and the like, is deposited on the surface of the semiconductor material, can enhance the absorption of visible light, can play a role of an electron trap, promotes the migration and separation of photoproduction electrons and holes, and further improves the photocatalytic performance.
Bi-Bi prepared according to the invention2WO6The BiOBr ternary complex has a structure formed by assembling nano-sheet layers, such as a nano-flower structure, and nano-particles are distributed in the nano-sheet layers. Wherein the nano-sheet layer is a bismuth oxybromide sheet layer, and the nano-particles are bismuth tungstate particles andbismuth elementary substance particles. The structure can effectively improve Bi-Bi2WO6The specific surface area of the-BiOBr ternary complex is 60-100 cm2/g。
Specifically, the thickness of the nanosheet layer is 2-5 nm, and the diameter of the nanoparticle is 7-12 nm. Preferably, the nanoflower structure has a diameter of about 550 to 700 nm.
According to one embodiment of the invention, the bismuth-bismuth tungstate-bismuth oxybromide ternary complex is used for treating sewage, in particular for treating cationic dye rose bengal B in water.
Specifically, the above Bi-Bi2WO6The BiOBr ternary compound is used as an adsorbent and a photocatalyst for sewage treatment, and is used for carrying out adsorption and photocatalytic tests on pollutants in water, and the method specifically comprises the following steps: rose bengal B solution was used as a typical sewage solution, and ternary complex powder was added as an adsorbent and a photocatalyst. Under magnetic stirring, the uv-vis absorption spectrum of the solution at each time point was measured and the absorption peak recorded. Calculating the concentration of the rose bengal B in the solution at each time point according to the standard curve of the rose bengal B solution, and then calculating the adsorption capacity by the following formula:
(wherein q iseIs the equilibrium adsorption amount, C0And CeThe initial concentration and the equilibrium concentration of rose bengal B, respectively, V is the volume of the solution, and W is the mass of the sample) to determine the adsorption amount of the ternary complex to rose bengal B. And (5) drawing by using the time-adsorption quantity to obtain an adsorption curve of the ternary complex, and inspecting the adsorption performance of the ternary complex. Placing rose bengal B solution containing ternary compound and saturated in metal halide lamp, recording absorption peak value of each time point under the dual effects of simulated solar illumination and magnetic stirring, calculating solution concentration by using standard curve, and obtaining degradation rate according to concentration value
And drawing a time-degradation rate curve, and inspecting the photocatalytic performance of the ternary compound. After a certain time, in the presence of bismuth-tungstate-oxybromideUnder the adsorption and photodegradation of the bismuth oxide ternary complex, the rose bengal B solution is completely degraded, and the solution becomes transparent.
The invention adopts the bismuth-bismuth tungstate-bismuth oxybromide ternary compound prepared by the one-step solvothermal method to enable bismuth, bismuth tungstate and bismuth oxybromide to be compounded to construct a plasma heterostructure compound. The metal bismuth has a plasma resonance effect, can improve the absorption of visible light, and plays a role of an electron trap to promote the separation of photo-generated electrons and holes; by forming the step-shaped composite energy band structure, photogenerated electrons and holes can be quickly transferred to different substance surfaces and effectively separated, and the photocatalytic performance is further improved. In addition, the composite is a nanoflower structure assembled by nanosheets, and has a large specific surface area, so that the composite has good adsorption performance. Due to the specific microstructure and the composite energy band structure, the bismuth-bismuth tungstate-bismuth oxybromide ternary compound prepared by the invention can be used as an adsorbent and a photocatalyst for sewage treatment, and particularly has strong adsorption and photodegradation on pollutants in water, so that the bismuth-bismuth tungstate-bismuth oxybromide ternary compound has wide application prospects in the field of sewage treatment, and particularly has strong adsorption and visible light degradation on a cationic dye rose bengal B in water.
Specific examples of the present invention will be given below to more clearly illustrate the present invention.
Example 1
Preparation of bismuth-bismuth tungstate-bismuth oxybromide ternary compound
(1) Preparing a bismuth nitrate glycol solution A with the concentration of 0.1M;
(2) preparing 0.05M sodium tungstate glycol solution, wherein the molar ratio of bismuth nitrate to sodium tungstate is 2: 1; adding potassium bromide to ensure that the molar ratio of the sodium tungstate to the potassium bromide is 1:0.5, and uniformly stirring to obtain an ethylene glycol solution B of the sodium tungstate and the potassium bromide;
(3) slowly dripping a glycol solution B of sodium tungstate and potassium bromide into a glycol solution A of bismuth nitrate, controlling the dripping time to be 10min, and stirring for 10min to obtain a uniform mixed solution;
(4) transferring the mixed solution into a polytetrafluoroethylene inner container with a steel sleeve, and placing the inner container into an oven for solvothermal reaction at the reaction temperature of 120 ℃ for 5 hours;
(5) and centrifuging the prepared reactant, repeatedly carrying out ultrasonic cleaning for 3 times by using deionized water and ethanol, and carrying out vacuum drying overnight to obtain bismuth-bismuth tungstate-bismuth oxybromide ternary composite powder.
Performance testing
The bismuth-bismuth tungstate-bismuth oxybromide ternary complex prepared in the example 1 is used as an adsorbent and a photocatalyst for sewage treatment, and the adsorption performance and the photocatalytic performance of a sewage sample are tested.
Taking 50mg/L rose bengal B solution as a sewage sample, and adding 15mg of bismuth-bismuth tungstate-bismuth oxybromide ternary compound powder into 30mL of rose bengal B solution. Under magnetic stirring, the uv-vis absorption spectrum of the solution at each time point was measured and the absorption peak recorded. According to the standard curve of the rose bengal B solution, the concentration of the solution at each time point is calculated, the adsorption amount of the ternary complex to the rose bengal B is obtained through a calculation formula of the adsorption amount, the time-adsorption amount is plotted to obtain the adsorption curve of the ternary complex, the adsorption performance of the ternary complex is considered, and the result is shown in FIG. 5. Placing rose bengal B solution containing ternary complex, which is saturated in adsorption, under a 450W metal halide lamp, recording the absorption peak value of each time point under the dual actions of simulated solar illumination and magnetic stirring, calculating the solution concentration by using a standard curve, obtaining the degradation rate through the concentration value, drawing a time-degradation rate curve, and inspecting the photocatalytic performance of the ternary complex, wherein the result is shown in FIG. 6.
The structural representation of the bismuth-bismuth tungstate-bismuth oxybromide ternary compound is as follows:
x-ray diffraction (XRD) is adopted to characterize the structure of the bismuth-bismuth tungstate-bismuth oxybromide ternary compound, and the spectrum is shown in figure 1. Referring to fig. 1, it was confirmed that the compound was composed of three components of bismuth, bismuth tungstate and bismuth oxybromide.
The structure of the bismuth-bismuth tungstate-bismuth oxybromide ternary complex was observed by Scanning Electron Microscopy (SEM), and the results are shown in fig. 2. Fig. 2 shows that the ternary complex has a nanoflower-like structure assembled by nanosheets, and some nanoparticles are distributed in the nanosheets. The thickness of the nano-sheet layer is 2-5 nm, the diameter of the nano-flower-shaped structure is about 550-700 nm, and the diameter of the nano-particle is 7-12 nm. The structure effectively improves the specific surface area of the ternary compound, which is beneficial to exerting the adsorption performance and the photocatalytic performance of the ternary compound on pollutants.
Referring to fig. 3, the components of the ternary composite material were detected by energy spectrum (EDS), which proves that the ternary composite material consisted of four elements of bismuth, tungsten, bromine, and oxygen, and had no other impurity elements.
FIG. 4 shows N of the above ternary composite2The adsorption and desorption curve conforms to the IV-type isotherm of an H3 hysteresis loop, and the specific surface area of the bismuth-bismuth tungstate-bismuth oxybromide ternary compound is 67.1cm2/g。
And (3) testing the adsorption performance and the photocatalytic performance of the bismuth-bismuth tungstate-bismuth oxybromide ternary compound:
the adsorption performance of the ternary complex of bismuth-bismuth tungstate-bismuth oxybromide on rose bengal B in water was determined by using the ternary complex of bismuth-bismuth tungstate-bismuth oxybromide as an adsorbent, as shown in FIG. 5. Photocatalytic degradation experiments are carried out on the rose bengal B solution which is saturated in adsorption, and the photocatalytic performance of the ternary complex is examined, as shown in FIG. 6.
Example 2
Preparation of bismuth-bismuth tungstate-bismuth oxybromide ternary compound
(1) Preparing a bismuth nitrate glycol solution A with the concentration of 1M;
(2) preparing 0.5M sodium tungstate glycol solution, wherein the molar ratio of bismuth nitrate to sodium tungstate is 2: 1; adding potassium bromide to ensure that the molar ratio of the sodium tungstate to the potassium bromide is 1:5, and uniformly stirring to obtain an ethylene glycol solution B of the sodium tungstate and the potassium bromide;
(3) slowly dripping a glycol solution B of sodium tungstate and potassium bromide into a glycol solution A of bismuth nitrate, controlling the dripping time to be 40min, and stirring for 60min to obtain a uniform mixed solution;
(4) transferring the mixed solution into a polytetrafluoroethylene inner container with a steel sleeve, and placing the inner container into an oven for solvothermal reaction at the reaction temperature of 220 ℃ for 10 hours;
(5) and centrifuging the prepared reactant, repeatedly carrying out ultrasonic cleaning for 3 times by using deionized water and ethanol, and carrying out vacuum drying overnight to obtain bismuth-bismuth tungstate-bismuth oxybromide ternary composite powder.
Comparative example 1
A composite material was prepared according to the same method as in example 1, except that potassium iodide was added instead of potassium bromide. For the prepared Bi/Bi2WO6the/BiOI ternary composite was subjected to the same adsorption performance test and photocatalytic performance test of rose bengal B in water as in example 1, and the results are shown in FIGS. 5 and 6.
Comparative example 2
A composite material was prepared according to the same method as in example 1 except that the amount of potassium bromide added was zero. To the prepared binary composite material Bi/Bi2WO6The same adsorption performance test and photocatalytic performance test of rose bengal B in water as in example 1 were performed, and the results are shown in fig. 5 and 6.
Comparative example 3
A composite material was prepared according to the same method as in example 1, except that the amount of sodium tungstate added was zero. The prepared binary composite Bi/BiOBr was subjected to the same adsorption performance test and photocatalytic performance test of rose bengal B in water as in example 1, and the results are shown in fig. 5 and 6.
Comparative example 4
A composite material was prepared according to the same method as in example 1, except that the ethylene glycol solvent was replaced with deionized water and the amount of potassium bromide added was zero. For the prepared Bi2WO6The same adsorption performance test and photocatalytic performance test of rose bengal B in water as in example 1 were performed, and the results are shown in fig. 5 and 6.
Comparative example 5
A composite material was prepared according to the same method as in example 1, except that the ethylene glycol solvent was replaced with deionized water and the amount of sodium tungstate added was zero. The prepared BiOBr was subjected to the same adsorption performance test and photocatalytic performance test of rose bengal B in water as in example 1, and the results are shown in fig. 5 and 6.
Referring to FIG. 5, in the initial stage, the ternary complex is rose bengalThe adsorption rate of B was high, and the adsorption rate became slow when approaching equilibrium. Comparative bismuth tungstate Bi2WO6Bismuth oxybromide BiOBr, binary bismuth/bismuth tungstate compound Bi/Bi2WO6Binary bismuth/bismuth oxybromide Bi/BiOBr compound, ternary bismuth/bismuth tungstate/bismuth oxyiodide Bi/Bi compound2WO6Bi/BiOI and ternary bismuth-bismuth tungstate-bismuth oxybromide compound Bi/Bi2WO6BiOBr shows that Bi/Bi is bismuth-tungstate-bismuth oxybromide2WO6The adsorption performance of/BiOBr is the most excellent.
The bismuth-bismuth tungstate-bismuth oxybromide ternary complex is used as a photocatalyst, and the photocatalytic performance of the bismuth-bismuth tungstate-bismuth oxybromide ternary complex on rose bengal B in water is shown in figure 6. 53% of rose bengal B remains after adsorption equilibrium, and after 140min of photocatalytic reaction, rose bengal B is completely degraded, and the solution becomes transparent.
Referring further to fig. 6, comparing bismuth tungstate, bismuth oxybromide, a binary bismuth/bismuth tungstate composite, a binary bismuth/bismuth oxybromide composite, a ternary bismuth/bismuth tungstate/bismuth oxyiodide composite, and a ternary bismuth-bismuth tungstate-bismuth oxybromide composite, it can be seen that the ternary bismuth/bismuth tungstate/bismuth oxybromide composite firstly completely degrades rose bengal B, and has excellent photocatalytic performance.
Claims (1)
1. The application of the bismuth-bismuth tungstate-bismuth oxybromide ternary complex in sewage treatment is characterized in that the preparation of the bismuth-bismuth tungstate-bismuth oxybromide ternary complex comprises the following steps:
step 1, adding bismuth nitrate into ethylene glycol, and uniformly stirring to obtain a solution A;
step 2, adding sodium tungstate and potassium bromide into ethylene glycol, and uniformly stirring to obtain a solution B;
step 3, dropwise adding the solution B into the solution A, and uniformly stirring to obtain a mixed solution;
step 4, transferring the mixed solution to a hydrothermal kettle for solvothermal reaction;
wherein in the mixed solution, the molar ratio of bismuth nitrate to sodium tungstate to potassium bromide is 2:1 (0.5-5);
wherein the bismuth-bismuth tungstate-bismuth oxybromide ternary complex has a nano-sheet structure and nano-particles distributed in the nano-sheet structure;
wherein the ternary compound of bismuth-bismuth tungstate-bismuth oxybromide has a thickness of 60-100 cm2Specific surface area per gram;
the nano lamellar structure is composed of bismuth oxybromide lamellar layers, and the nano particles are composed of bismuth tungstate particles and bismuth elementary substance particles;
the bismuth-bismuth tungstate-bismuth oxybromide ternary compound has good adsorption and photocatalysis performances on rose bengal B solution;
in the step 4, the temperature of the solvothermal reaction is 120-220 ℃, and the reaction time is 1-40 h;
in the step 1, the concentration of bismuth nitrate in the solution A is 0.1-1M;
in the step 2, the concentration of sodium tungstate in the solution B is 0.05-0.5M;
in the step 2, the molar ratio of sodium tungstate to potassium bromide in the solution B is 1 (0.5-5).
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