CN106311256B - A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst - Google Patents
A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 48
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 150000001875 compounds Chemical class 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 229910002402 SrFe12O19 Inorganic materials 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 21
- 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 9
- 238000003756 stirring Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003475 lamination Methods 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 23
- 230000015556 catabolic process Effects 0.000 abstract description 11
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 238000004064 recycling Methods 0.000 abstract description 11
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 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 abstract description 9
- 229940043267 rhodamine b Drugs 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- QGUBTCKXCHGNIU-UHFFFAOYSA-N [BiH2][Sr] Chemical compound [BiH2][Sr] QGUBTCKXCHGNIU-UHFFFAOYSA-N 0.000 description 3
- 239000011218 binary composite Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- 239000000463 material Substances 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
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000006615 aromatic heterocyclic group Chemical group 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram 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
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- -1 sodium alkyl benzene Chemical class 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000002351 wastewater Substances 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/843—Arsenic, antimony or bismuth
- B01J23/8437—Bismuth
-
- 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
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst belongs to the technical field of catalyst.The present invention is with graphene, bismuth nitrate and SrFe12O19For raw material, a step thermal reduction is impregnated using solution, product is made.Present invention process step is simple, and device therefor is few, short preparation period, production safety and at low cost；The product photocatalysis performance prepared using the method for the present invention is excellent, reaches 99.5% or more to the degradation rate of rhodamine B in 50min under visible light；Furthermore the product magnetic performance is good, coercivity is 4142.6G, and anti-demagnetization capability is stronger, and magnetic recycling still can achieve 90.2% to the degradation rate of rhodamine B after reusing 4 times, be conducive to the recycling and reuse of catalyst, therefore industrial production cost can be saved.Photocatalytic degradation organic pollutants in water body can be widely used for using the product that the present invention is prepared.
Description
Technical field
The invention belongs to catalyst technical fields, and in particular to graphene/β-Bi2O3/SrFe12O19Tri compound magnetism light
The preparation method of catalyst.
Background technique
Graphene has big specific surface area and excellent electric conductivity, light induced electron can be transferred in its lamella,
To prevent light induced electron from accumulating in semiconductor surface, the compound of photo-generate electron-hole pairs is avoided, to improve photocatalysis
Efficiency has obtained extensively in photocatalysis fields such as photocatalytic hydrogen production by water decomposition, photocatalysis degradation organic contaminant and photochemical cells
General application.
In light-catalyzed reaction, graphene combined oxidation bismuth (Bi2O3) catalyst activity can be enhanced, it carries out simultaneously
Tax magnetic is difficult to recycle after can solving the problems, such as reaction and recycling is not thorough caused secondary pollution.Currently, many researchers have succeeded
Prepare a nanometer Bi2O3Catalyst has simultaneously carried out the work of related modified aspect, but generally existing synthetic yield is low, pollution is big, at
The problems such as this height and complex procedures.Therefore, it is environmental-friendly, reduce cost under conditions of, prepare convenient for recycling it is efficient
Bi2O3Catalyst is of great significance.
The existing compound Bi of graphene2O3The preparation method of photochemical catalyst, such as " Journal of Alloys and
Compounds " 2015 years " Visible light photocatalytic degradation in 872-877 pages of volume 649
of dyes byβ-Bi2O3/ grapheme nanocomposites " (documents 1) text, disclosed method is: using molten
Glue-gel method disperses nitric acid for bismuth nitrate first using graphene, bismuth nitrate, citric acid, ethyl alcohol and acrylamide as raw material
In solution；Then citric acid and acrylamide monomer is added, is heated to 80 DEG C of formation gels under magnetic stirring；Then 120
It is DEG C dry and heated two hours in 600 DEG C and obtain β-Bi2O3；Finally by resulting β-Bi2O3With graphene dispersion in ethyl alcohol,
And ultrasound 10min, then final product is obtained in 60 DEG C of air drying 10h.The major defect of this method is: (1) this is compound
Photochemical catalyst needs to prepare β-Bi first2O3, then with graphene carry out it is inorganic mix, used herein is simple ultrasound
Method, this method is unsuitable for the effective compound of inorganic matter, to reduce the catalysis efficiency of photochemical catalyst；(2) composite photo-catalyst
Performance it is lower, be only 65% to the degradation rate of methylene blue in 240min, and do not investigate to more difficult to degrade under visible light
Dyestuff such as rhodamine B stress efficacy；(3) recycling and repeat performance of photochemical catalyst are not investigated in the experiment, this is unfavorable
In the usage economy of catalyst, and the catalyst belongs to nanometer materials, is not easy to recycling and uses, it is therefore possible to cause
Secondary pollution.
In addition, to Bi2O3The modified research of magnetic photocatalyst is concentrated mainly on binary composite foundation, such as Patent No.
The patent " a kind of preparation method and its bismuthino strontium magnetic photocatalyst of bismuthino strontium magnetic photocatalyst " of 1034470224 A of CN
With bismuth nitrate and strontium ferrite (SrFe in (documents 2) text12O19) it is raw material, it is dispersing agent with neopelex,
The presoma of bismuthino strontium magnetic photocatalyst is first prepared, then drying roasts to obtain bismuth oxide/strontium ferrite (Bi2O3/
SrFe12O19) binary composite photo-catalyst.This method is disadvantageous in that: (1) needing to use a large amount of 12 in preparation process
The neopelex of sodium alkyl benzene sulfonate, high-purity is expensive, therefore is not suitable for large-scale production；(2) work
Skill preparation process is cumbersome, takes a long time, and in addition needs to carry out the roasting of 3-5h during the preparation process at a high temperature of 500-600 DEG C
It burns, therefore will cause final products sintering seriously, particle is larger, influences catalysis efficiency, and long-time high-temperature roasting is to instrument
Equipment requirement it is higher and meanwhile also result in energy consumption it is more, it is difficult to reach industrialization power conservation requirement；(3) the binary composite magnetic photocatalysis
The active component of agent is the Bi of α type2O3, relative to β type Bi2O3Catalytic performance is lower, under visible light to the methylene of 10mg/L
For blue solution degradation rate needs 4h when 98%.
Summary of the invention
The purpose of the present invention is be directed to existing binary Bi2O3Composite photo-catalyst preparation method complexity and photocatalysis efficiency
Low problem proposes a kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst, preparation
Graphene/β-Bi2O3/SrFe12O19Tri compound magnetic photocatalyst photocatalysis efficiency with higher under visible light, and
The method for preparing catalyst is simple, can aromatic heterocyclic dye organic pollutant effectively in degrading waste water.The method of the present invention has
Materials safety, process flow is environmentally friendly, and production cost is low, and obtained catalyst recycles convenient and reusable equal spies
Point.
Graphene of the present invention/β-Bi2O3/SrFe12O19Tri compound magnetic photocatalyst the preparation method is as follows:
(1) graphene/β-Bi2O3/SrFe12O19The preparation of presoma
Weigh the Bi (NO of 8mmol3)3.5H2O is in the nitric acid of 1mol/L, and stirring 0.5h to bismuth nitrate is completely dissolved, then
The SrFe that mass fraction is 15% is added12O19, 2h is stirred, then above-mentioned solution is added dropwise to 80ml, 0.6mol/L sodium carbonate
In solution, graphene oxide and β-Bi are pressed later2O3/SrFe12O19Suitable oxidation is added dropwise for 0.5~5: 100 in mass ratio
Graphene (GO) continues to stir 12h to solution in brown, and after standing, solution generates lamination, and filtering, filter cake is through washing, alcohol
After washing for several times, the dry 10h in 80 DEG C.
(2) graphene/β-Bi2O3/SrFe12O19The preparation of tri compound magnetic photocatalyst
It takes the sample in (1) after drying to be placed in mortar to grind, then moves in Muffle furnace, vacuumize, in nitrogen protection
Under, control heating rate is 4 DEG C/min, and holding temperature is 380 DEG C, sample is taken out after roasting 10min, cooled to room temperature,
Up to graphene/β-Bi2O3/SrFe12O19Tri compound magnetic photocatalyst.
The present invention by adopting the above technical scheme, mainly has the following effects:
(1) tri compound magnetic photocatalyst prepared by the present invention, under visible light to the rhodamine B solution of 10mg/l into
Row irradiates, and ultraviolet-uisible spectrophotometer fails to detect rhodamine B after 50min, illustrates that degradation rate reaches 99.5% or more, this
Degradation efficiency is apparently higher than the degradation efficiency in documents 1,2 to methylene blue.
(2) materials safety that the method for the present invention is selected is easy to get, and process flow is simple, and device therefor is few, thus production safety,
It is at low cost；In addition long-time high-temperature roasting, energy conservation and environmental protection, therefore the method for the present invention is not needed to be extremely suitable for being mass produced.
(3) the tri compound magnetic photocatalyst of the method for the present invention preparation, magnetic performance degree is good, and coercivity is
4142.6G, anti-demagnetization capability is stronger, after reusing 4 times, still reaches in 50min to the degradation rate of rhodamine B under visible light
90.2%, this is conducive to the recycling and recycling of catalyst, therefore can save industrial production cost.
(4) the tri compound magnetic photocatalyst that the method for the present invention is prepared, belongs to multifunctional composite, enriches magnetic
The scope of property catalyst.
Detailed description of the invention
Fig. 1 is graphene/β-Bi that embodiment 1 is prepared2O3/SrFe12O19The X of tri compound magnetic photocatalyst is penetrated
Ray diffraction diagram spectrum；
Fig. 2 is graphene/β-Bi that embodiment 1 is prepared2O3/SrFe12O19Tri compound magnetic photocatalyst is swept
Retouch electron microscope picture；
Fig. 3 is graphene/β-Bi that embodiment 1 is prepared2O3/SrFe12O19The magnetic of tri compound magnetic photocatalyst
Hysteresis curves for the ease of comparing, while appending β-Bi2O3/SrFe12O19The hysteresis loop of binary magnetic photochemical catalyst.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst, specific steps are such as
Under:
(1) graphene/β-Bi2O3/SrFe12O19The preparation of presoma
Weigh the Bi (NO of 8mmol3)3·5H2O is in the nitric acid of 1mol/L, and stirring 0.5h to bismuth nitrate is completely dissolved, so
The SrFe that mass fraction is 15% is added afterwards12O19, 2h is stirred, then above-mentioned solution is added dropwise to 80ml, 0.6mol/L carbonic acid
In sodium solution, by graphene oxide and β-Bi2O3/SrFe12O19Mass ratio is to be added dropwise graphene oxide (GO) at 2: 100, after
Continuous stirring 12h is in brown to solution, and after standing, solution generates lamination, and filtering, filter cake is after washing, alcohol are washed for several times, 80
Dry 10h in DEG C.
(2) graphene/β-Bi2O3/SrFe12O19The preparation of tri compound magnetic photocatalyst
It takes the sample in (1) after drying to be placed in mortar to grind, then moves back into Muffle furnace, vacuumize, protected in nitrogen
Under shield, control heating rate is 4 DEG C/min, and soaking time is 380 DEG C, takes out sample after roasting 10min, naturally cools to room
Temperature is to get graphene/β-Bi2O3/SrFe12O19Tri compound magnetic photocatalyst.
Embodiment 2
A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst, specific steps are such as
Under:
(1) graphene/β-Bi2O3/SrFe12O19The preparation of presoma
Weigh the Bi (NO of 8mmol3)3·5H2O is dissolved in the nitric acid of 1mol/L, and stirring 0.5h to bismuth nitrate is completely dissolved,
Then the SrFe that mass fraction is 15% is added12O19, 2h is stirred, then above-mentioned solution is added dropwise to 80ml, 0.6mol/L carbon
In acid sodium solution, by graphene oxide and β-Bi2O3/SrFe12O19Mass ratio is to be added dropwise graphene oxide at 0.5: 100
(GO), continue to stir 12h to solution in brown, after standing, solution generates lamination, filtering, and filter cake is washed for several times through washing, alcohol
Afterwards, the dry 10h in 80 DEG C.
(2) with 1 (2) step of embodiment.
Embodiment 3
A kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst, specific steps are such as
Under:
(1) graphene/β-Bi2O3/SrFe12O19The preparation of presoma
Weigh the Bi (NO of 8mmol3)3·5H2O is in the nitric acid of 1mol/L, and stirring 0.5h to bismuth nitrate is completely dissolved, so
The SrFe that mass fraction is 15% is added afterwards12O19, stirring 2h, then above-mentioned solution is added dropwise to 80ml, 0.6mol/L carbonic acid
In sodium solution, by graphene oxide and β-Bi2O3/SrFe12O19Mass ratio is to be added dropwise graphene oxide (GO) at 5: 100, after
Continuous stirring 12h is in brown to solution, and after standing, solution generates lamination, and filtering, filter cake is after washing, alcohol are washed for several times, 80
Dry 10h in DEG C.
(2) with 1 (2) step of embodiment.
Experimental result
X-ray diffraction test, X-ray diffraction are carried out with the tri compound magnetic photocatalyst that embodiment 1 is prepared
Map is as shown in Figure 1；The tri compound magnetic photocatalyst Analysis of Surface Topography that embodiment 1 is prepared is as shown in Figure 2；With reality
The tri compound magnetic photocatalyst that example 1 is prepared is applied, magnetic performance test is carried out, hysteresis loop is as shown in Figure 3；With reality
The tri compound magnetic photocatalyst that example 1 is prepared is applied, photocatalytic activity test and recycling are carried out.
From fig. 1, it can be seen that graphene/β-Bi2O3/SrFe12O19In the X ray diffracting spectrum of tri compound magnetic photocatalyst
25.71 °, 27.95 °, 31.76 °, 32.69 ° and 46.22 ° respectively correspond tetragonal system β-Bi2O3(210) (201) (002)
(220) and (200) crystal face diffraction, illustrate graphene and SrFe12O19β-Bi can't be changed2O3Crystal form, to ensure that three
The crystallization of effective active component is complete in first composite magnetic photochemical catalyst.In addition, do not have to find the peak of graphene in spectrogram, it is former
Because being since the load capacity of graphene is too low (only 2%).In order to further verify the effective compound of graphene, surface sweeping electricity has been carried out
Sub- microscopic characterization, as a result as shown in Fig. 2, can be deposited under high power field with the graphene of two-dimensional layered structure visible in detail
?.The tri compound magnetic photocatalyst that embodiment 1 is prepared, is under visible light irradiated rhodamine B solution, 50min
Ultraviolet-uisible spectrophotometer fails to detect rhodamine B afterwards, illustrates that degradation rate reaches 99.5% or more；Hysteresis loop shows three
The coercivity of first composite magnetic photochemical catalyst is 4142.6G, and the coercivity compared to binary magnetic photochemical catalyst does not occur
Change, illustrates that the introducing of graphene will not influence its magnetic performance, and coercitive size reflects anti-move back to a certain extent
Magnetic energy power, this illustrates that the anti-demagnetization capability of the catalyst is stronger, is conducive to the catalyst and carries out magnetic recovery recycling.Pass through repetition
After recycling 4 times, the tri compound magnetic photocatalyst still reaches the degradation rate of rhodamine B under the same conditions for discovery
90.2%, illustrate using tri compound magnetic photocatalyst prepared by the present invention photocatalytic activity with higher and stability.
It is easily operated in conclusion the process conditions of technical solution of the present invention are simple, can be made magnetic performance preferably, catalytic activity
High, performance stablizes excellent graphene/β-Bi2O3/SrFe12O19Tri compound magnetic photocatalyst.
Claims (1)
1. a kind of graphene/β-Bi2O3/SrFe12O19The preparation method of tri compound magnetic photocatalyst, it is characterised in that described
Specific step is as follows for method:
(1) graphene/β-Bi2O3/SrFe12O19The preparation of presoma
Weigh the Bi (NO of 8mmol3)3·5H2In the nitric acid of 1mol/L, stirring 0.5h is completely dissolved to bismuth nitrate O, then plus
Enter the SrFe that mass fraction is 15%12O19, 2h is stirred, then above-mentioned solution is added dropwise to the sodium carbonate of 80mL, 0.6mol/L
In solution, by graphene oxide and β-Bi2O3/SrFe12O19Graphene oxide is added dropwise for 0.5~5: 100 in mass ratio, continues
It is in brown that 12h, which is stirred, to solution, and after standing, solution generates lamination, and filtering, filter cake is after washing, alcohol are washed for several times, at 80 DEG C
Middle dry 10h；
(2) graphene/β-Bi2O3/SrFe12O19The preparation of tri compound magnetic photocatalyst
It takes the sample in (1) after drying to be placed in mortar to grind, then moves in Muffle furnace, vacuumize, under nitrogen protection, control
Heating rate processed is 4 DEG C/min, and holding temperature is 380 DEG C, takes out sample after roasting 10min, cooled to room temperature is to get stone
Black alkene/β-Bi2O3/SrFe12O19Tri compound magnetic photocatalyst.
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| CN102899122A (en) * | 2012-10-19 | 2013-01-30 | 深圳大学 | Bi2O3/oxidized graphene composite powder and preparation method thereof |
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