CN108607584A - A kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation method - Google Patents
A kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation method Download PDFInfo
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- CN108607584A CN108607584A CN201810432581.4A CN201810432581A CN108607584A CN 108607584 A CN108607584 A CN 108607584A CN 201810432581 A CN201810432581 A CN 201810432581A CN 108607584 A CN108607584 A CN 108607584A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 49
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 34
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims description 14
- 229910002402 SrFe12O19 Inorganic materials 0.000 claims abstract description 65
- 238000002360 preparation method Methods 0.000 claims abstract description 29
- 238000010168 coupling process Methods 0.000 claims abstract description 28
- 238000005859 coupling reaction Methods 0.000 claims abstract description 28
- 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 claims abstract description 12
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 39
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 20
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 13
- 230000008878 coupling Effects 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 230000005389 magnetism Effects 0.000 claims description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002525 ultrasonication Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 abstract description 18
- 238000006731 degradation reaction Methods 0.000 abstract description 18
- 238000004064 recycling Methods 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910052724 xenon Inorganic materials 0.000 abstract description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 229910052712 strontium Inorganic materials 0.000 description 4
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 150000001621 bismuth Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005415 magnetization Effects 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001408 amides Chemical group 0.000 description 1
- 125000006615 aromatic heterocyclic group Chemical group 0.000 description 1
- 150000001622 bismuth compounds Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- FIMTUWGINXDGCK-UHFFFAOYSA-H dibismuth;oxalate Chemical compound [Bi+3].[Bi+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O FIMTUWGINXDGCK-UHFFFAOYSA-H 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052961 molybdenite Inorganic materials 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- B01J35/33—
-
- B01J35/39—
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The present invention relates to a kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10‑SrFe12O19Preparation method, belong to inorganic catalysis material field.The present invention uses hydro-thermal method, is first prepared for magnetic SrFe12O19Matrix, then it is prepared for the more bismuth visible light catalyst Bi of magnetic coupling24O31Br10‑SrFe12O19.The more bismuth visible light catalyst Bi of magnetic coupling24O31Br10‑SrFe12O19Crystalline form is good, has preferable magnetic property.Under the xenon lamp irradiation of simulated solar irradiation, the composite magnetic photochemical catalyst 0.05g of preparation, the rhodamine B solution of degradation 100mL a concentration of 20mg/L is degradable in 40min；The average recovery rate of catalyst is 87%, and photocatalytic degradation rhodamine B, the degradation rate of 0.5h still reach 90% to the catalyst after 5 recycling under the same conditions.The preparation method of the present invention is simple, and the used time is short, and device therefor is few, and production cost is low.
Description
Technical field
The present invention relates to a kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation method, belong to
In technical field of inorganic material.
Background technology
With the development of the global economy, the contradiction of the gesture of energy consumption presentation rapid growth, population and resource is more and more sharp,
Environmental issue becomes one of the important restriction factor of economy and social development.In recent years, photochemical catalyst is in water pollution treatment research
Field has received widespread attention, including the bismuth series photocatalyst including bismuth oxide, bismuthates and BiOX because it is only
Special layer structure, preferable light absorptive and it is safe and non-toxic the features such as and as the hot spot of field of photocatalytic material research, but halogen
There are the compound very fast and conduction band positions of, hole low to the visible light utilization efficiency and electronics too drawbacks such as just in bismuth oxide, make it in ring
Application in the fields such as border and the energy is restricted.As a kind of Novel bismuth series catalysts, more bismuth Bi24O31Br10Conduction band it is wide
Spend it is moderate, in compound the content increase of Bi can effectively improve conduction band positions, be conducive to generate more superoxide radicals, inhibit light
Raw electronics and hole it is compound, its photocatalytic activity can be improved.In view of during photocatalytic degradation organic wastewater, especially
It is that extensive processing waste water usually has that catalyst recycling is difficult.Photochemical catalyst recycling in order to prevent is not thorough and generates two
Secondary pollution, and use cost is reduced, photochemical catalyst is assigned into magnetic, is very necessary convenient for separating and recovering and recycling.
Strontium ferrite SrFe12O19Not only there is good magnetic property, but also synergistic effect is generated to photocatalysis；More bismuths are multiple
It closes on magnetic strontium ferrite, both improves photocatalytic activity, be conducive to the recycling of catalyst, also can avoid causing secondary pollution.
Currently, more bismuths are reported seldom with the compound research of magnetisable material.Other magnetic photocatalysts, such as Chinese patent
CN103480384A (documents 1), which is disclosed, prepares SrFe12O19/BiVO4Method, this method has the following disadvantages：(1) it makes
The degradation efficiency of standby composite catalyst photocatalytic degradation methylene blue is relatively low, and 5h degradation rates are only 93%；(2) what is prepared is compound
Catalyst circulation stability is poor, and when composite catalyst is used continuously 5 times, 5h is only 60% to the degradation rate of methylene blue.It grinds
The person of studying carefully has carried out the research of compound more bismuth compound photocatalytic activities, such as Chinese patent CN104722317A (documents 2) public affairs
Bi is opened12O17Br2-Bi24O31Br10Preparation method, but this method has the following disadvantages：(1) first hydro-thermal method synthetic bromide is used to aoxidize
Bismuth-bismuth oxalate generates Bi using calcining12O17Br2-Bi24O31Br10Hydro-thermal-roasting two step synthetic method composite photo-catalyst,
Process takes, high energy consumption；(2) recovery method and the rate of recovery of catalyst are not provided；(3) not to the degradation property of waste water from dyestuff
Height, when the composite catalyst catalytic degradation 10mg/L rhodamine B solutions of synthesis, 2h not yet degrades completely.
Invention content
It is an object of the invention to the visible light catalysis activity for bismuth series photocatalyst is not high and catalyst recycling is difficult
Defect, propose with SrFe12O19As magnetic matrix load non-stoichiometric bismuth based compound Bi24O31Br10It prepares magnetic
Compound more bismuth Bi24O31Br10-SrFe12O19Method, preparation method is simple, and the used time is few, at low cost, convenient for passing through external magnetic field point
There is high catalytic activity and stability from the catalyst with recycling catalyst, recycling.The more bismuths of obtained magnetic coupling are visible
Before photochemical catalyst has application well in the water pollution control technology of the organic pollutant degradations such as dyestuff containing aromatic heterocyclic
Scape.The method of the present invention had not only realized that resource made full use of, but also the secondary pollution for avoiding catalyst that from may bringing.
A kind of more bismuth visible light catalyst Bi of magnetic coupling of the present invention24O31Br10-SrFe12O19Preparation method it is as follows：
(1) magnetism SrFe12O19Preparation
With the quantitative SrCl of deionized water dissolving2·6H2O and FeCl3·6H2It is molten to be instilled above-mentioned mixing by O for NaOH solution
Liquid is placed in reaction kettle, and for 24 hours, cooling, filtering, Washing of Filter Cake is placed on 80 DEG C of baking ovens for 200 DEG C of water-bath heat preservations, and dry 12h is
Obtain magnetic SrFe12O19。
(2)Bi24O31Br10-SrFe12O19Preparation
In molar ratio 1:1 weighs appropriate Bi (NO3)3·5H2O and NaBr, which is dissolved separately in deionized water, obtains Bi (NO3)3
Solution and NaBr solution；Appropriate polyvinylpyrrolidone PVP is added into NaBr solution, under ultrasonication dissolving obtain mixing it is molten
Mixed solution A is added dropwise to Bi (NO by liquid A dropwise3)3In solution, stirring 0.5h obtains mixed solution B；According to mass ratio 100:5
~20 weigh the SrFe of step (1) preparation12O19Be added in mixed solution B, be used in combination sodium hydroxide solution adjust solution pH be
9~11, ultrasonic 1h obtains suspension C；Suspension C is placed in reaction kettle, 120~160 DEG C of water-baths 10~12h of heat preservation, cooling,
Filtering, Washing of Filter Cake are placed on 80 DEG C of baking ovens, and dry 12h is to get to the more bismuth Bi of magnetic coupling24O31Br10-SrFe12O19。
The present invention uses above-mentioned technical proposal, mainly has the following effects：
(1) the more bismuth visible light catalyst Bi of magnetic coupling prepared by the method for the present invention24O31Br10-SrFe12O19, X-ray
Difraction spectrum free from admixture peak and only Bi24O31Br10And SrFe12O19Characteristic diffraction peak；The preparation method of the present invention is simple, uses
When it is short, device therefor is few, and production cost is low.
(2) the more bismuth visible light catalyst Bi of magnetic coupling prepared by the method for the present invention24O31Br10-SrFe12O19With higher
Catalytic activity take composite visible light catalyst prepared by 0.05g to be catalyzed light degradation under the xenon lamp irradiation of simulated solar irradiation
The rhodamine B solution (being twice of rhodamine B concentration in documents 2) of a concentration of 20mg/L of 100mL is dropped completely in 40min
It solves (being not detected, this is apparently higher than the degradation effect in documents 1 and documents 2)；It is single under the same terms
Bi24O31Br10The Visible Light Induced Photocatalytic rate for being catalyzed rhodamine B is only 65%.
(3) the more bismuth visible light catalyst Bi of magnetic coupling prepared by the method for the present invention24O31Br10-SrFe12O19With good
The rate of recovery and high stability, outside plus magnetic fields under the rate of recovery be up to 87%, and 5 times recycling after catalyst in phase
The light degradation of rhodamine B is catalyzed under conditions of, degradation rate of a concentration of 20mg/L rhodamine B solutions in 0.5h still reaches
90%.
Description of the drawings
Fig. 1 is the Bi of synthesis24O31Br10、SrFe12O19、Bi24O31Br10-SrFe12O19X ray diffracting spectrum (XRD)；
Fig. 2 is the Bi of synthesis24O31Br10-SrFe12O19Infrared spectrum (FT-IR)；
Fig. 3 is the Bi of synthesis24O31Br10-SrFe12O19Scanning electron microscope diagram (SEM)；
Fig. 4 is the Bi of synthesis24O31Br10-SrFe12O19Hysteresis loop (VSM).
Specific implementation mode
With reference to embodiment, it further illustrates the present invention.
Embodiment 1
A kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation method, specific steps are such as
Under：
(1) magnetism SrFe12O19Preparation
SrCl is quantified with deionized water dissolving2·6H2O and FeCl3·6H2NaOH solution is slowly dropped into above-mentioned mixing by O
Solution is placed in reaction kettle, and for 24 hours, cooling, filtering, Washing of Filter Cake is placed on 80 DEG C of baking ovens, dry 12h for 200 DEG C of water-bath heat preservations
Obtain magnetic SrFe12O19。
(2)Bi24O31Br10-SrFe12O19Preparation
Weigh 1.94g Bi (NO3)3·5H2O and 0.204g NaBr are dissolved separately in 20ml deionized waters and obtain Bi
(NO3)3Solution and NaBr solution；0.2g polyvinylpyrrolidone PVP are added into NaBr solution, dissolves and obtains under ultrasonication
Mixed solution A is instilled Bi (NO by mixed solution A dropwise3)3In solution, stirring 0.5h obtains mixed solution B；Weigh 0.1052g
SrFe prepared by step (1)12O19It is added in mixed solution B, it is 9 to be used in combination sodium hydroxide solution to adjust the pH of solution, ultrasonic 1h
Obtain suspension C；Suspension C is placed in reaction kettle, 120 DEG C of water-baths keep the temperature 10h, cooling, filtering, and Washing of Filter Cake is placed on 80
DEG C baking oven, dry 12h is to get to the more bismuth Bi of magnetic coupling24O31Br10-SrFe12O19。
Embodiment 2
A kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation method, specific steps are such as
Under：
(1) magnetism SrFe12O19Preparation
With (1) the step of embodiment 1.
(2)Bi24O31Br10-SrFe12O19Preparation
Weigh 1.94g Bi (NO3)3·5H2O and 0.204g NaBr are dissolved separately in 20ml deionized waters and obtain Bi
(NO3)3Solution and NaBr solution；0.2g polyvinylpyrrolidone PVP are added into NaBr solution, dissolves and obtains under ultrasonication
Mixed solution A is instilled Bi (NO by mixed solution A dropwise3)3In solution, stirring 0.5h obtains mixed solution B；Weigh 0.0526g
SrFe prepared by step (1)12O19It is added in mixed solution B, it is 10 to be used in combination sodium hydroxide solution to adjust the pH of solution, ultrasound
1h obtains suspension C；Suspension C is placed in reaction kettle, 140 DEG C of water-baths keep the temperature 11h, cooling, filtering, and Washing of Filter Cake is placed on
80 DEG C of baking ovens, dry 12h is to get to the more bismuth Bi of magnetic coupling24O31Br10-SrFe12O19。
Embodiment 3
A kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation method, specific steps are such as
Under：
(1) magnetism SrFe12O19Preparation
With (1) the step of embodiment 1.
(2)MoS2/SrFe12O19Preparation
Weigh 1.94g Bi (NO3)3·5H2O and 0.204g NaBr are dissolved separately in 20ml deionized waters and obtain Bi
(NO3)3Solution and NaBr solution；0.2g polyvinylpyrrolidone PVP are added into NaBr solution, dissolves and obtains under ultrasonication
Mixed solution A is instilled Bi (NO by mixed solution A dropwise3)3In solution, stirring 0.5h obtains mixed solution B；Weigh 0.0263g
SrFe prepared by step (1)12O19It is added in mixed solution B, it is 11 to be used in combination sodium hydroxide solution to adjust the pH of solution, ultrasound
1h obtains suspension C；Suspension C is placed in reaction kettle, 160 DEG C of water-baths keep the temperature 12h, cooling, filtering, and Washing of Filter Cake is placed on
80 DEG C of baking ovens, dry 12h is to get to the more bismuth Bi of magnetic coupling24O31Br10-SrFe12O19。
Experimental result
Bi prepared by embodiment 224O31Br10-SrFe12O19Catalytic degradation activity is best.In order to facilitate comparison, it is prepared for
Bi24O31Br10Sample.Bi24O31Br10Preparation method is to be added without SrFe in 2 step of implementing regulations (2)12O19。
Bi prepared by embodiment 224O31Br10-SrFe12O19And Bi24O31Br10And SrFe12O19X-ray diffraction spectrum
(XRD) such as Fig. 1, Bi24O31Br10The diffraction maximum of sample and the standard card PDF#75-0888 of more bismuths are completely corresponding, show the sample
Product are homogeneous Bi24O31Br10；SrFe12O19Diffraction maximum and the standard card PDF#33-1340 of hexagonal crystal system strontium ferrite are completely right
It answers, shows that sample is pure SrFe12O19.The more bismuth Bi of composite magnetic24O31Br10-SrFe12O19X-ray diffraction spectrum diffraction maximum
With the feature crystal face spectral line (008), (107), (114) and (21-3) of standard card PDF#33-1340 and PDF#75-0888,
(10-10), (11-7) match, without impurity peaks, it was demonstrated that Bi24O31Br10And SrFe12O19Success is compound.
Bi prepared by embodiment 224O31Br10-SrFe12O19FT-IR spectrum such as Fig. 2, in 3431cm-1, 2921.8cm-1,
There is apparent wave crest, respectively O-H ,-CH2Stretching vibration, 530cm-1Place is Bi-O key stretching vibration peaks, 444cm-1,
544.4cm-1, 592.5cm-1The absorption peak at place is the stretching vibration characteristic peak of the ferritic Fe-O and Sr-O keys of M-type strontium；PVP's
The C=O peak positions of characteristic peak are by 1666cm-1It is moved to 1654cm to lower wave number direction-1Place；The peak of other feature peak C-N and C=C
Position does not shift.It can be obtained from above-mentioned testing result, between the C=O keys in composite magnetic catalyst in Bi-O and PVP
It is interacted, therefore in synthesis Bi24O31Br10-SrFe12O19During, PVP and Bi24O31Br10-SrFe12O19It
Between form chemical bond.1654cm-1Place is C=O stretching vibration peaks, 1291cm-1For C-N absorption peaks, 1384cm-1Left and right absorbs
Peak is amide structure C-N structure stretching vibration peaks, is all the characteristic peak of PVP.Documents show that synthesized compound includes
Bi24O31Br10And SrFe12O19Characteristic absorption peak, it was demonstrated that the sample is the more bismuth Bi of magnetic coupling24O31Br10-SrFe12O19。
Bi prepared by embodiment 224O31Br10-SrFe12O19Scanning electron microscope SEM such as Fig. 3, show monocline in figure
Bi24O31Br10The flower-shape and SrFe that sheet stacks12O19Hexagonal pattern, further prove SrFe12O19With
Bi24O31Br10It is effective compound.
Bi prepared by embodiment 224O31Br10-SrFe12O19The more bismuth visible light catalysts of magnetic coupling be used for catalytic degradation
The rhodamine B solution of a concentration of 20mg/L of 100mL, it is degradable in 40min under simulated solar irradiation irradiation, and it is single
Bi24O31Br10The degradation rate of parallel test, RhB is 65%, single SrFe12O19Corresponding degradation rate is 10%.The result shows that this
The more bismuth visible light catalysts of magnetic coupling of invention synthesis have excellent visible light photocatalysis active, magnetic matrix SrFe12O19
By further preventing the compound photocatalytic to more bismuths of light induced electron, hole that there is collaboration facilitation.This is because PVP
Addition promote Bi24O31Br10The growth of activity advantage crystal face weakens the growth of inertia crystal face, the growth side of Effective Regulation crystal face
To induce the structure of anisotropic and the generation of pattern, namely realizing the more bismuth Bi of magnetic coupling24O31Br10-
SrFe12O19Controllable synthesis.
Bi prepared by embodiment 224O31Br10-SrFe12O19VSM such as Fig. 4 of the more bismuth catalysts of magnetic coupling,
Bi24O31Br10-SrFe12O19Saturation magnetization (Ms), remanent magnetization (Mr) be respectively 3.078emu/g and
1.026emu/g, coercivity (Hc) are 753.5G, and higher coercivity shows good anti-demagnetization performance, shows that composite magnetic is more
Bismuth catalyst is a kind of hard magnetic material, has good magnetic performance, is conducive to it and detaches and return under the action of externally-applied magnetic field
It receives.Catalyst, average recovery rate 87% are recycled using externally-applied magnetic field；The catalyst of the 5th recycling is urged under the same conditions
Change the light degradation of rhodamine B, a concentration of 20mg/L rhodamine B solutions still reach 90% in the degradation rate of 0.5h.
Embodiment above describes the preparation method of the present invention, main features and advantages.The present invention is not by above-described embodiment
Limitation, under the range for not departing from the principle of the invention, method, for the present invention by sustained improvement, these each fall within protection of the present invention
In the range of.
Claims (4)
1. a kind of more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation method, feature includes following
Step：
(1) magnetism SrFe12O19Preparation
SrCl is quantified with deionized water dissolving2·6H2O and FeCl3·6H2NaOH solution is slowly dropped into above-mentioned mixed solution simultaneously by O
It is placed in reaction kettle, for 24 hours, cooling, filtering, Washing of Filter Cake is placed on 80 DEG C of baking ovens for 200 DEG C of water-bath heat preservations, and dry 12h is obtained
Magnetic SrFe12O19；
(2) the more bismuth visible light catalyst Bi of magnetic coupling24O31Br10-SrFe12O19Preparation
Weigh 1.94g Bi (NO3)3·5H2O and 0.204g NaBr, which are dissolved separately in 20ml deionized waters, obtains Bi (NO3)3It is molten
Liquid and NaBr solution；0.2g polyvinylpyrrolidone PVP are added into NaBr solution, is dissolved under ultrasonication and obtains mixed solution
Mixed solution A is instilled Bi (NO by A dropwise3)3In solution, stirring 0.5h obtains mixed solution B；Weigh 0.0526g steps (1) system
Standby SrFe12O19It is added in mixed solution B, it is 10 to be used in combination sodium hydroxide solution to adjust the pH of solution, and ultrasonic 1h obtains suspended
Liquid C；Suspension C is placed in reaction kettle, 140 DEG C of water-baths keep the temperature 11h, cooling, filtering, and Washing of Filter Cake is placed on 80 DEG C of baking ovens,
Dry 12h is to get to the more bismuth Bi of magnetic coupling24O31Br10-SrFe12O19。
2. the preparation method of the more bismuth visible light catalysts of magnetic coupling according to claim 1, it is characterised in that step (2)
It is middle that Bi is prepared using hydro-thermal method24O31Br10-SrFe12O19, method is simple, takes less, energy-efficient.
3. the preparation method of the more bismuth visible light catalysts of magnetic coupling according to claim 1, it is characterised in that step (2)
The more bismuth Bi of magnetic coupling of preparation24O31Br10-SrFe12O19Catalytic activity it is high, band gap is narrow, light induced electron, hole compound speed
Spend it is low, it is big to the absorption rate of visible light, for being catalyzed a concentration of 20mg/L rhodamine B solutions of Visible Light Induced Photocatalytic, in 40min
It is degradable.
4. the preparation method of the more bismuth visible light catalysts of magnetic coupling according to claim 1, it is characterised in that step (2)
Prepared Bi24O31Br10-SrFe12O19The stability of catalyst is high, and catalyst can be effectively recycled using externally-applied magnetic field, recycles
Obtained catalyst has excellent catalytic activity under similarity condition.
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