CN110227475A - A kind of BiFeO3/Bi2Fe4O9The preparation method and applications of heterojunction structure catalyst - Google Patents
A kind of BiFeO3/Bi2Fe4O9The preparation method and applications of heterojunction structure catalyst Download PDFInfo
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- CN110227475A CN110227475A CN201910551975.6A CN201910551975A CN110227475A CN 110227475 A CN110227475 A CN 110227475A CN 201910551975 A CN201910551975 A CN 201910551975A CN 110227475 A CN110227475 A CN 110227475A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 87
- 229910002902 BiFeO3 Inorganic materials 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229910002897 Bi2Fe4O9 Inorganic materials 0.000 claims abstract description 82
- HDMGAZBPFLDBCX-UHFFFAOYSA-M potassium;sulfooxy sulfate Chemical compound [K+].OS(=O)(=O)OOS([O-])(=O)=O HDMGAZBPFLDBCX-UHFFFAOYSA-M 0.000 claims abstract description 35
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 16
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 14
- 230000002195 synergetic effect Effects 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 230000003115 biocidal effect Effects 0.000 claims description 21
- 230000008569 process Effects 0.000 claims 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 description 19
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000002351 wastewater Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 10
- 239000002957 persistent organic pollutant Substances 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 230000000593 degrading effect Effects 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 230000031709 bromination Effects 0.000 claims 1
- 238000005893 bromination reaction Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 231100000719 pollutant Toxicity 0.000 claims 1
- 238000006731 degradation reaction Methods 0.000 abstract description 47
- KIPLYOUQVMMOHB-MXWBXKMOSA-L [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O Chemical compound [Ca++].CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O.CN(C)[C@H]1[C@@H]2[C@@H](O)[C@H]3C(=C([O-])[C@]2(O)C(=O)C(C(N)=O)=C1O)C(=O)c1c(O)cccc1[C@@]3(C)O KIPLYOUQVMMOHB-MXWBXKMOSA-L 0.000 abstract description 46
- 229940063650 terramycin Drugs 0.000 abstract description 46
- 230000015556 catabolic process Effects 0.000 abstract description 37
- 230000015572 biosynthetic process Effects 0.000 abstract description 15
- 238000003786 synthesis reaction Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 230000004913 activation Effects 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 238000002835 absorbance Methods 0.000 description 10
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 description 9
- 229960001180 norfloxacin Drugs 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000000498 cooling water Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 238000005070 sampling Methods 0.000 description 6
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 238000003795 desorption Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 229910016874 Fe(NO3) Inorganic materials 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 229940088710 antibiotic agent Drugs 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000009977 dual effect Effects 0.000 description 3
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000002153 concerted effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- XWNOTOKFKBDMAP-UHFFFAOYSA-N [Bi].[N+](=O)(O)[O-] Chemical compound [Bi].[N+](=O)(O)[O-] XWNOTOKFKBDMAP-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect 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
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 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 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F2101/38—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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a kind of BiFeO3/Bi2Fe4O9The preparation method and applications of heterojunction structure catalyst, belong to technical field of sewage.BiFeO in the present invention3/Bi2Fe4O9Heterojunction structure catalyst is that one-step synthesis, preparation method are simple under hydrothermal conditions.BiFeO3/Bi2Fe4O9In heterojunction structure catalyst, BiFeO3With Bi2Fe4O9The heterojunction structure of formation can inhibit visible light catalyst BiFeO3Light induced electron and hole it is compound, while in light, Fe3+Collective effect under activation potassium hydrogen persulfate quickly and efficiently generate SO4 ·‑, under the synergistic effect of heterojunction structure light-catalyzed reaction and advanced oxidation reaction, when 40min, can reach 82.32% to the degradation rate of terramycin.
Description
Technical field
The invention belongs to catalysis material technical fields, and in particular to a kind of one-step synthesis BiFeO3/Bi2Fe4O9Hetero-junctions
The preparation method and applications of structure catalyst use BiFeO more particularly to a kind of3/Bi2Fe4O9Heterojunction structure is as photocatalysis
The application of reaction and the dual catalytic agent of advanced oxidation reaction in degradation field of antibiotics.
Background technique
China is antibiotics production and uses big country, and a large amount of antibiotic, which is directly or indirectly discharged, causes two to water environment
Secondary pollution causes significant toxic action to growth, the development of microorganism, animal and plant.Thrilling is the beginning of this year
Veterinary antibiotic has been detected in children's urine examination on the ground such as Jiangsu-zhejiang Shanghai Area Anhui.Efficient, the environmental-friendly method of one kind is found to go to remove water
Antibiotic in body is extremely urgent.
Based on potentiometric titrations (SO4 ·-) high-level oxidation technology presented in terms of degradable organic pollutant potentially
Application prospect.This is primarily due to compared with Fenton oxidation is reacted based on SO4 ·-High-level oxidation technology have following advantage:
a.SO4 ·-With higher oxidizing potential；B. reacting is influenced to want small relatively by pH value；C. SO is generated4 ·-Persulfate at room temperature
The advantages that stability height, good water solubility, easily stored and transport.
For example, Chinese Patent Application No. is 201510181466.0, application publication date is the patent Shen on July 1st, 2015
Please file disclose a kind of method that light helps bismuth ferrite activation potassium hydrogen persulfate degradation of organic waste water.With perovskite knot in the patent
Structure BiFeO3For photochemical catalyst, light-catalyzed reaction occurs and generates light induced electron and hole degradable organic pollutant, while to system
Middle introducing potassium hydrogen persulfate (PMS), BiFeO3Middle Fe3+It activates PMS and generates SO4 ·-Advanced oxidation reaction occurs, in light-catalyzed reaction
With degradable organic pollutant under the synergistic effect of advanced oxidation reaction.But narrow bandgap semiconductor material BiFeO3Photoproduction electricity
Son and hole are easy compound, affect the efficiency of light-catalyzed reaction in concerted reaction.
Bi2Fe4O9It is BiFeO3The association phase being easy to appear in synthesis process, on April 17th, 2017, " ACS
Sustainable Chemistry&Engineering " 2017 years volume 5 the 6th the 4630-4636 pages of the phase, Wei Jianhong et al. public affairs
An entitled " Facial Synthesis and Photoreaction Mechanism of BiFeO is opened3/
Bi2Fe4O9Heterojunction Nanofibers " (is based on BiFeO3/Bi2Fe4O9The interfacial polymerization of hetero-junctions nanofiber
And its research of light reaction mechanism) article, this article find BiFeO3With Bi2Fe4O9Z-type heterojunction structure can be formed, in light
Higher performance is shown in terms of hydrogen production by water decomposition under catalytic degradation rhodamine and visible light.But using method of electrostatic spinning
Prepare BiFeO3/Bi2Fe4O9Hetero-junctions catalyst process is complicated, needs the high static pressure electricity and higher synthesis temperature of volts up to ten thousand,
And low output.
Therefore, it needs to develop a kind of one-step synthesis BiFeO3/Bi2Fe4O9The method of heterojunction structure catalyst, and made
It applies for dual catalyst in Degradation of Antibiotics field, to improve the degradation efficiency of antibiotic.
Summary of the invention
1. to solve the problems, such as
For existing BiFeO3/Bi2Fe4O9Heterojunction structure composite catalyst synthesis process complexity is cumbersome, synthesis condition controls
Difficult big problem, the present invention provide a kind of using hydro-thermal method one-step synthesis BiFeO3/Bi2Fe4O9Heterojunction structure composite catalyst
Method, synthesis process is simple, and makes BiFeO3/Bi2Fe4O9Heterojunction structure catalyst is anti-in light-catalyzed reaction and advanced oxidation
Should act synergistically lower degradation antibiotic, provide wide application prospect for the efficient degradation of antibiotic.
2. technical solution
To solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
A kind of BiFeO3/Bi2Fe4O9The preparation method of heterojunction structure catalyst, prepares with the following method: by bismuth nitrate
It is soluble in water, after addition cetyl trimethylammonium bromide is sufficiently stirred, ferric nitrate is added, sodium hydroxide conduct is added after stirring
Mineralizer puts into mixed solution in reaction kettle after being sufficiently stirred, is warming up to 200 DEG C of reaction 6h, product is through deionized water and second
Alcohol is extremely neutral after sufficiently washing, and in 60 DEG C of dry 5h, obtains brown sample, as BiFeO3/Bi2Fe4O9Heterojunction structure catalysis
Agent.
Further, BiFeO3/Bi2Fe4O9Heterojunction structure catalyst is prepared with the following method:
(1) preparation of bismuth nitrate solution: the bismuth nitrate for being 10~18mmol/L by bismuth nitrate formation concentration soluble in water is molten
Liquid；
(2)BiFeO3/Bi2Fe4O9The synthetic reaction process of heterojunction structure catalyst: to step (1) prepared bismuth nitrate
Ferric nitrate is added in solution, adds ferric nitrate, stirs and sodium hydroxid is added after 10~40min as mineralizer, wherein nitric acid
Bismuth: ferric nitrate: cetyl trimethylammonium bromide: the mass ratio of sodium hydroxid is 1:(0.6~1.0): (0.4~0.8): (4.7
~16.7) mixed solution is put into reaction kettle after, being sufficiently stirred, compactedness 60~80%, is warming up to 160~200 DEG C of reactions 3
~7h, obtains product；
(3) product obtained in step (2) is sufficiently washed through deionized water, ethyl alcohol to neutrality, in 60 DEG C of dry 5h, is obtained
To brown sample, as BiFeO3/Bi2Fe4O9Heterojunction structure catalyst.
Further, the preferred 18mmol/L of the bismuth nitrate solution, the bismuth nitrate: ferric nitrate: cetyl trimethyl
Ammonium bromide: the mass ratio of sodium hydroxid is preferably 1:1:0.6:13.
A kind of BiFeO3/Bi2Fe4O9Heterojunction structure catalyst is in the application of degradable organic pollutant, wherein BiFeO3/
Bi2Fe4O9Heterojunction structure catalyst is prepared using the above method.
Further, by the BiFeO3/Bi2Fe4O9Heterojunction structure catalyst is sufficiently mixed with organic pollutant wastewater
After reaching adsorption-desorption balance, oxidant is added into system, is cooperateed in heterojunction structure light-catalyzed reaction and advanced oxidation reaction
The lower organic pollutants of degrading of effect.
Further, the concentration that the heterojunction structure catalyst is formed in the reaction system is 0.5~1.5g/L.
Further, the organic pollutant is antibiotic.
Further, the concentration of the antibiotic waste water is 5~50mg/L.
Further, BiFeO3/Bi2Fe4O9The mass ratio of heterojunction structure catalyst and oxidant is 1: (0.6~1.6).
Further, the oxidant is potassium hydrogen persulfate, and the concentration of hydrogen persulfate potassium solution is 1.0~6.0mmol/
L；
3. beneficial effect
Compared with the prior art, the invention has the benefit that
(1) BiFeO prepared by the present invention3/Bi2Fe4O9Heterojunction structure catalyst belongs to one-step synthesis, and preparation method is simple,
And sample specific surface area is larger, stability is good, itself can be used as catalysis material reuse；
(2) BiFeO of the present invention3/Bi2Fe4O9In heterojunction structure catalyst, BiFeO3/Bi2Fe4O9Form heterojunction structure, suppression
Light induced electron processed and hole it is compound, effectively raise the efficiency of light-catalyzed reaction part in concerted reaction；
(3) BiFeO of the present invention3/Bi2Fe4O9In heterojunction structure catalyst, due to Fe3+Potassium hydrogen persulfate sulfuric acid can be activated
Salt generates SO4 ·-, so that antibiotic is degraded under advanced oxidation reaction and the synergistic effect of light-catalyzed reaction, effectively raise
Degradation efficiency；
(4) present invention uses hydro-thermal method one-step synthesis BiFeO3/Bi2Fe4O9Heterojunction structure catalyst, utilizes BiFeO3With
Bi2Fe4O9The heterojunction structure of formation inhibits BiFeO in light-catalyzed reaction3Light induced electron and hole it is compound, solve narrow band gap
Semiconductor material BiFeO3The easily compound problem of light induced electron and hole, while in light, Fe3+Collective effect under activate over cure
Potassium hydrogen phthalate quickly and efficiently generates SO4 ·-, make light-catalyzed reaction and advanced oxidation reaction synergistic effect degradation antibiotic, be antibiosis
The efficient degradation of element provides wide application prospect.
Detailed description of the invention
Fig. 1 is BiFeO produced by the present invention3/Bi2Fe4O9The XRD diagram of heterojunction structure；
Fig. 2 is BiFeO produced by the present invention3/Bi2Fe4O9The SEM figure of heterojunction structure (enlargement ratio is 2000 times)；
Fig. 3 is BiFeO produced by the present invention3/Bi2Fe4O9The SEM figure of heterojunction structure (enlargement ratio is 5000 times)；
Fig. 4 is BiFeO produced by the present invention3/Bi2Fe4O9The Raman spectrogram of heterojunction structure；
Fig. 5 is for different catalysts to the degradation effect figure of terramycin under PMS existence condition；
Fig. 6 is BiFeO3/Bi2Fe4O9、PMS、BiFeO3/Bi2Fe4O9Degradation effect figure of/the PMS to terramycin.
Specific embodiment
For a better understanding of the present invention, the content that the present invention is furture elucidated in the following with reference to the drawings and specific embodiments,
But the contents of the present invention are not limited solely to embodiment below.
Embodiment 1
One, BiFeO3/Bi2Fe4O9The preparation of heterojunction structure catalyst
Embodiment 1-1
18mmol/L bismuth nitrate solution 240ml is measured to be added after addition 1g cetyl trimethylammonium bromide is sufficiently stirred
22.5g sodium hydroxid is added as mineralizer, mixed solution after being sufficiently stirred after stirring 30min in 1.7g Fe(NO3)39H2O
It puts into reaction kettle, compactedness 80% is warming up to 200 DEG C of reaction 6h, and product adjusts pH extremely after deionized water, ethyl alcohol sufficiently wash
Neutrality obtains brown sample, as BiFeO in 60 DEG C of dry 5h3/Bi2Fe4O9Heterojunction structure catalyst.
Wherein, Fig. 1 BiFeO3、Bi2Fe4O9、BiFeO3/Bi2Fe4O9The XRD spectra of heterojunction structure.According to standard diagram
(BiFeO3JCPDS74-2016 and Bi2Fe4O974-1098) compare the BiFeO it is found that prepared3/Bi2Fe4O9Composite material is only
Contain BiFeO3And Bi2Fe4O9Two-phase, no other impurity peaks occur.Fig. 2 and Fig. 3 is BiFeO obtained3/Bi2Fe4O9Hetero-junctions
The SEM of structure schemes, it can be seen that sample is mainly formed by the particle aggregation of cuboid and irregular shape.Utilize Raman spectroscopy
Sample is characterized, as a result as shown in Figure 4.In 139cm-1、173cm-1、217cm-1、471cm-1The Raman peaks of appearance belong to
Perovskite structure BiFeO3Vibration mode, in 277cm-1、324cm-1、361cm-1、427cm-1、547cm-1、637cm-1Occur
Raman peaks belong to orthohormbic structure Bi2Fe4O9Vibration mode, it is consistent with the analysis result of XRD in Fig. 1.
Embodiment 1-2
10mmol/L bismuth nitrate solution 125ml is measured to add after addition 0.3g cetyl trimethylammonium bromide is sufficiently stirred
Enter the Fe(NO3)39H2O of 0.36g, 7.83g sodium hydroxid is added as mineralizer, mixing after being sufficiently stirred after stirring 10min
Solution is put into reaction kettle, and compactedness 60% is warming up to 160 DEG C of reaction 3h, and product is adjusted after deionized water, ethyl alcohol sufficiently wash
PH obtains brown sample, as BiFeO in 60 DEG C of dry 5h to neutrality3/Bi2Fe4O9Heterojunction structure catalyst.
Embodiment 1-3
14mmol/L bismuth nitrate solution 118ml is measured to add after addition 0.6g cetyl trimethylammonium bromide is sufficiently stirred
Enter the Fe(NO3)39H2O of 0.64g, 13g sodium hydroxid is added as mineralizer after stirring 25min, is sufficiently stirred rear molten mixing
Liquid is put into reaction kettle, and compactedness 70% is warming up to 180 DEG C of reaction 5h, and product adjusts pH after deionized water, ethyl alcohol sufficiently wash
Brown sample, as BiFeO are obtained in 60 DEG C of dry 5h to neutrality3/Bi2Fe4O9Heterojunction structure catalyst.
Embodiment 1-4
16mmol/L bismuth nitrate solution 129ml is measured to add after addition 0.8g cetyl trimethylammonium bromide is sufficiently stirred
Enter the Fe(NO3)39H2O of 1g, 16g sodium hydroxid is added as mineralizer, mixed solution after being sufficiently stirred after stirring 40min
It puts into reaction kettle, compactedness 80% is warming up to 200 DEG C of reaction 7h, and product adjusts pH extremely after deionized water, ethyl alcohol sufficiently wash
Neutrality obtains brown sample, as BiFeO in 60 DEG C of dry 5h3/Bi2Fe4O9Heterojunction structure catalyst.
Embodiment 2
Two, using BiFeO3/Bi2Fe4O9The effect assessment of heterojunction structure catalyst degradation antibiotic waste water
Embodiment 2-1
Using BiFeO3/Bi2Fe4O9Heterojunction structure catalyst and potassium hydrogen persulfate (PMS) combination carry out antibiotic waste water
Degradation, process object is concentration C0For the terramycin aqueous solution 200mL of 5mg/L, heterojunction structure catalyst, which is added, toward reactor makes
Its concentration is 1.0g/L, and 30min is stirred under the conditions of being protected from light, and so that terramycin is reached suction-desorption with catalyst surface and reaches
To balance, potassium hydrogen persulfate (PMS) is then added under conditions of being sufficiently stirred makes its concentration 5mmol/L, opens 500W xenon
Lamp opens simultaneously cooling water, carries out degradation reaction, wherein BiFeO3/Bi2Fe4O9Heterojunction structure catalyst and potassium hydrogen persulfate
Mass ratio is 1: 1.54.It is sampled every 10min, every sub-sampling 5mL, tests the suction in 353nm with ultraviolet-visible spectrophotometer
Shading value calculates the degradation rate of terramycin solution by the variation of absorbance value.With C/C0It indicates in different moments solution
The remaining ratio of terramycin, wherein C0Represent when not being added catalyst the i.e. 5mg/L terramycin solution without experiment process at the beginning of
Beginning concentration, C represent the concentration of different moments terramycin solution after addition catalyst.
In 1 embodiment 2-1 of table when 10min terramycin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 50.35 | 34.40 | 27.68 | 19.38 |
Embodiment 2-2
Using BiFeO3/Bi2Fe4O9Heterojunction structure catalyst and potassium hydrogen persulfate combination carry out the degradation of antibiotic waste water,
Process object is concentration C0For the terramycin aqueous solution 200mL of 27mg/L, heterojunction structure catalyst, which is added, toward reactor keeps its dense
Degree is 0.5g/L, and 30min is stirred under the conditions of being protected from light, and so that terramycin is reached suction-desorption with catalyst surface and reaches flat
Weighing apparatus, potassium hydrogen persulfate is then added under conditions of being sufficiently stirred makes its concentration 1mmol/L, opens 500W xenon lamp and opens simultaneously
Cooling water carries out degradation reaction, wherein BiFeO3/Bi2Fe4O9The mass ratio of heterojunction structure catalyst and potassium hydrogen persulfate is 1:
0.61.It samples every 10min, every sub-sampling 5mL, with ultraviolet-visible spectrophotometer test in the absorbance value of 353nm, leads to
The variation for crossing absorbance value calculates the degradation rate of terramycin solution.With C/C0Indicate that terramycin is remaining in different moments solution
Ratio, wherein C0Represent when not being added catalyst the i.e. initial concentration of the 27mg/L terramycin solution without experiment process, C
Represent the concentration of different moments terramycin solution after catalyst is added.
In 2 embodiment 2-2 of table when 10min terramycin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 56.89 | 39.41 | 32.86 | 26.65 |
Embodiment 2-3
Using BiFeO3/Bi2Fe4O9Heterojunction structure catalyst and potassium hydrogen persulfate combination carry out the degradation of antibiotic waste water,
Process object is concentration C0For the terramycin aqueous solution 200mL of 50mg/L, heterojunction structure catalyst, which is added, toward reactor keeps its dense
Degree is 1.5g/L, and 30min is stirred under the conditions of being protected from light, and so that terramycin is reached suction-desorption with catalyst surface and reaches flat
Weighing apparatus, potassium hydrogen persulfate is then added under conditions of being sufficiently stirred makes its concentration make its concentration 6mmol/L, opens 500W xenon
Lamp opens simultaneously cooling water, carries out degradation reaction, wherein BiFeO3/Bi2Fe4O9Heterojunction structure catalyst and potassium hydrogen persulfate
Mass ratio is 1: 1.23.It is sampled every 10min, every sub-sampling 5mL, tests the suction in 353nm with ultraviolet-visible spectrophotometer
Shading value calculates the degradation rate of terramycin solution by the variation of absorbance value.With C/C0It indicates in different moments solution
The remaining ratio of terramycin, wherein C0Represent when not being added catalyst the i.e. 50mg/L terramycin solution without experiment process
Initial concentration, C represent the concentration of different moments terramycin solution after addition catalyst.
In 3 embodiment 2-3 of table when 10min terramycin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 52.28 | 33.63 | 26.96 | 17.68 |
Embodiment 3
Three, using BiFeO3/Bi2Fe4O9The effect assessment of heterojunction structure catalyst degradation Norfloxacin waste water
Using BiFeO3/Bi2Fe4O9Heterojunction structure catalyst and PMS combination carry out the degradation of Norfloxacin waste water, processing
Object is concentration C0For the Norfloxacin aqueous solution 200mL of 5mg/L, heterojunction structure catalyst, which is added, toward reactor makes its concentration
1.0g/L stirs 30min under the conditions of being protected from light, and so that Norfloxacin and catalyst surface is reached suction-desorption and reaches balance,
Then PMS is added under conditions of being sufficiently stirred makes its concentration make its concentration 5mmol/L, opens 500W xenon lamp and opens simultaneously
Cooling water carries out degradation reaction, wherein BiFeO3/Bi2Fe4O9The mass ratio of heterojunction structure catalyst and potassium hydrogen persulfate is 1:
1.54.It is sampled every 10min, every sub-sampling 5mL tests its absorbance value with ultraviolet-visible spectrophotometer, passes through absorbance
The variation of value calculates the degradation rate of Norfloxacin.With C/C0Indicate the remaining ratio of Norfloxacin in different moments solution,
Wherein, C0Represent when not being added catalyst that i.e. the initial concentration of the 5mg/L Norfloxacin without experiment process, C represent addition and urge
The concentration of different moments Norfloxacin after agent.
In 4 embodiment 3 of table when 10min Norfloxacin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 41.63 | 25.21 | 18.94 | 9.86 |
Comparative example 1
This comparative example and embodiment 2-1 are essentially identical, the difference is that: it uses and is individually added into catalyst BiFeO3Into
The degradation of row antibiotic waste water, process object are the terramycin aqueous solution 200mL that concentration is 5mg/L, are added into reactor
BiFeO3Making its concentration 1g/L, potassium hydrogen persulfate, which is added, toward reactor makes its concentration make its concentration 5mmol/L, and other
Part and embodiment 2-1 are same.
In 5 comparative example 1 of table when 10min terramycin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 74.42 | 60.56 | 42.51 | 34.41 |
Comparative example 2
This comparative example and embodiment 2-1 are essentially identical, the difference is that: it uses and is individually added into Bi2Fe4O9Resisted
The oxidative degradation of raw element waste water, process object are the terramycin aqueous solution 200mL that concentration is 5mg/L, and over cure is added toward reactor
Potassium hydrogen phthalate, other conditions are same with embodiment 2-1.
In 6 comparative example 2 of table when 10min terramycin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 72.38 | 55.97 | 39.41 | 31.12 |
Above by the performance of different catalysts degradation terramycin in embodiment 2-1 and comparative example 1,2 as shown in figure 5, by Fig. 5
It can be seen that: BiFeO3/Bi2Fe4O9Heterojunction structure is shown when doing dual catalyst compared with high degradability energy, degradation of the 40min to terramycin
Rate can reach 80.62%, hence it is evident that be higher than BiFeO3And Bi2Fe4O9Degradation rate when catalyst is done, illustrates BiFeO3/Bi2Fe4O9Shape
At heterojunction structure be more advantageous to light-catalyzed reaction and advanced oxidation reaction Synergistic degradation antibiotic.
Comparative example 3
This comparative example and embodiment 2-1 are essentially identical, the difference is that: only addition potassium hydrogen persulfate (PMS).
Specific degradation process are as follows:
The degradation of antibiotic waste water is carried out using potassium hydrogen persulfate (PMS), process object is concentration C0It is mould for the soil of 5mg/L
Plain aqueous solution 200mL, potassium hydrogen persulfate, which is added, under conditions of being sufficiently stirred makes its concentration 5mmol/L, opens cooling water, into
Row degradation reaction.It is sampled every 10min, every sub-sampling 5mL, tests the absorbance in 353nm with ultraviolet-visible spectrophotometer
Value, the degradation rate of terramycin solution is calculated by the variation of absorbance value.With C/C0Indicate that soil is mould in different moments solution
The remaining ratio of element, wherein C0The initial concentration of the 5mg/L terramycin solution without experiment process is represented, C, which is represented, is added over cure
The concentration of different moments terramycin solution after potassium hydrogen phthalate.
In 7 comparative example 3 of table when 10min terramycin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 79.25 | 69.81 | 59.40 | 57.14 |
Above by the performance for terramycin of degrading in embodiment 2-1 and comparative example 3 as shown in fig. 6, as seen from Figure 6: BiFeO3/
Bi2Fe4O9Heterojunction structure catalyst is shown compared with high degradability energy, and 40min can reach 80.62% to the degradation rate of terramycin, bright
The aobvious degradation rate being higher than when using potassium hydrogen persulfate (PMS).
Comparative example 4
This comparative example and embodiment 2-1 are essentially identical, the difference is that: only addition BiFeO3/Bi2Fe4O9Hetero-junctions
Structure catalyst.
Specific degradation process are as follows:
Using BiFeO3/Bi2Fe4O9Heterojunction structure catalyst carries out the degradation of antibiotic waste water, and process object is concentration C0
For the terramycin aqueous solution 200mL of 5mg/L, 0.2g heterojunction structure catalyst is added toward reactor, is stirred under the conditions of being protected from light
30min makes in solution terramycin and catalyst surface reach suction-desorption and reaches balance, and opening 500W xenon lamp opens simultaneously cooling
Water carries out degradation reaction.It samples every 10min, every sub-sampling 5mL, is tested with ultraviolet-visible spectrophotometer 353nm's
Absorbance value calculates the degradation rate of terramycin solution by the variation of absorbance value.With C/C0It indicates in different moments solution
The middle remaining ratio of terramycin, wherein C0Represent when not being added catalyst the i.e. 5mg/L terramycin solution without experiment process
Initial concentration, C represent the concentration of different moments terramycin solution after addition catalyst.
In 8 comparative example 4 of table when 10min terramycin residual concentration percentage
| Time/min | 0 | 10 | 20 | 30 | 40 |
| C/C0 | 100 | 93.41 | 88.30 | 86.76 | 84.02 |
It is worth noting that comparative example 3 and comparative example 4 can be obtained compared with embodiment 2-1, potassium hydrogen persulfate oxidative degradation is only added
When terramycin, the degradation rate of 40min is 42.86%；Only addition BiFeO3/Bi2Fe4O9Photocatalytic degradation soil when composite catalyst
It is 15.98% in the degradation rate of 40min when mycin；Work as BiFeO3/Bi2Fe4O9Composite catalyst and potassium hydrogen persulfate be combined into
When the degradation of row terramycin, it is 80.62% in the degradation rate of 40min, illustrates in heterojunction structure light-catalyzed reaction and advanced oxidation
The degradation rate of terramycin can be greatly improved under the synergistic effect of reaction.
Claims (9)
1. a kind of BiFeO3/Bi2Fe4O9The preparation method of heterojunction structure catalyst a, it is characterised in that: step is closed with the following method
At: bismuth nitrate is soluble in water, after cetyl trimethylammonium bromide stir process is added, ferric nitrate is added, after stir process
Sodium hydroxide is added as mineralizer, is sufficiently stirred after handling mixed solution to put into reaction kettle and be put into baking oven and reacts, from
So for product to neutrality after deionized water and ethyl alcohol are sufficiently washed, drying obtains brown sample, as BiFeO after cooling3/
Bi2Fe4O9Heterojunction structure catalyst.
2. a kind of BiFeO according to claim 13/Bi2Fe4O9The preparation method of heterojunction structure catalyst, it is characterised in that
It prepares with the following method:
(1) preparation of bismuth nitrate solution: by the bismuth nitrate concentration soluble in water that formed for the bismuth nitrate solution of 10~18mmol/L；
(2)BiFeO3/Bi2Fe4O9The synthetic reaction process of heterojunction structure catalyst: to step (1) prepared bismuth nitrate solution
After middle first addition cetyl trimethylammonium bromide stir process, ferric nitrate is added, hydroxide is added after stirring 10~40min
Receive as mineralizer, wherein bismuth nitrate: ferric nitrate: cetyl trimethylammonium bromide: the mass ratio of sodium hydroxid is 1:(0.6
~1.0): (0.4~0.8): (4.7~16.7) are put into mixed solution in reaction kettle after stir process, and compactedness 60~
80%, 160~200 DEG C of 3~7h of reaction are warming up to, product is obtained；
(3) product obtained in step (2) is sufficiently washed through deionized water, ethyl alcohol to neutrality, in 60 DEG C of dry 5h, obtains palm fibre
Tinctorial pattern product, as BiFeO3/Bi2Fe4O9Heterojunction structure catalyst.
3. a kind of BiFeO according to any one of claims 1 or 23/Bi2Fe4O9The preparation side of heterojunction structure catalyst
Method, it is characterised in that: the preferred 18mmol/L of bismuth nitrate solution, the bismuth nitrate: ferric nitrate: cetyl trimethyl bromination
Ammonium: the mass ratio of sodium hydroxid is preferably 1:1:0.6:13.
4. a kind of BiFeO3/Bi2Fe4O9Application of the heterojunction structure catalyst in degradable organic pollutant, it is characterised in that: described
BiFeO3/Bi2Fe4O9Heterojunction structure catalyst be with the method for claims 1 or 2 or 3 be prepared into come.
5. a kind of BiFeO according to claim 43/Bi2Fe4O9The application of heterojunction structure catalyst, it is characterised in that: will
The BiFeO3/Bi2Fe4O9Heterojunction structure catalyst and organic pollutant wastewater, which are sufficiently mixed, reaches adsorption-desorption balance
Afterwards, oxidant is added into system, has in water of degrading under heterojunction structure light-catalyzed reaction and advanced oxidation reaction synergistic effect
Machine pollutant.
6. a kind of BiFeO according to claim 53/Bi2Fe4O9The application of heterojunction structure catalyst, it is characterised in that: institute
The concentration that the heterojunction structure catalyst stated is formed in the reaction system is 0.5~1.5g/L.
7. a kind of BiFeO according to claim 53/Bi2Fe4O9The application of heterojunction structure catalyst, it is characterised in that: institute
The organic pollutant stated is antibiotic, and the concentration of the antibiotic waste water is 5~50mg/L.
8. a kind of BiFeO according to claim 53/Bi2Fe4O9The application of heterojunction structure catalyst, it is characterised in that: institute
The BiFeO stated3/Bi2Fe4O9The mass ratio of heterojunction structure catalyst and oxidant is 1: (0.6~1.6).
9. according to a kind of BiFeO described in claim 5 or 8 any one3/Bi2Fe4O9The application of heterojunction structure catalyst,
Be characterized in that: the oxidant is potassium hydrogen persulfate, and the concentration of hydrogen persulfate potassium solution is 1.0~6.0mmol/L.
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