CN116237053A - alpha-Fe 2 O 3 /V 2 O 5 Preparation method of BC composite material and application of composite material - Google Patents
alpha-Fe 2 O 3 /V 2 O 5 Preparation method of BC composite material and application of composite material Download PDFInfo
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 65
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000004098 Tetracycline Substances 0.000 claims abstract description 56
- 229960002180 tetracycline Drugs 0.000 claims abstract description 56
- 229930101283 tetracycline Natural products 0.000 claims abstract description 56
- 235000019364 tetracycline Nutrition 0.000 claims abstract description 56
- 150000003522 tetracyclines Chemical class 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims abstract description 33
- 235000011613 Pinus brutia Nutrition 0.000 claims abstract description 33
- 241000018646 Pinus brutia Species 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002351 wastewater Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical class [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000007790 solid phase Substances 0.000 claims abstract description 9
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000000197 pyrolysis Methods 0.000 claims abstract description 4
- 238000005485 electric heating Methods 0.000 claims abstract description 3
- 238000001704 evaporation Methods 0.000 claims abstract 2
- 239000011259 mixed solution Substances 0.000 claims abstract 2
- 238000001914 filtration Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 230000003213 activating effect Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229910052724 xenon Inorganic materials 0.000 claims description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 3
- 239000007864 aqueous solution Substances 0.000 claims 1
- 230000001678 irradiating effect Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000003115 biocidal effect Effects 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 230000004913 activation Effects 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 16
- 230000000694 effects Effects 0.000 description 12
- 238000007792 addition Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 6
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- 230000007547 defect Effects 0.000 description 5
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000011835 investigation Methods 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 229940088710 antibiotic agent Drugs 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 2
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- 239000008399 tap water Substances 0.000 description 2
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- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 208000031295 Animal disease Diseases 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- YMGGAHMANIOXGP-UHFFFAOYSA-L disodium;oxido sulfate Chemical compound [Na+].[Na+].[O-]OS([O-])(=O)=O YMGGAHMANIOXGP-UHFFFAOYSA-L 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
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- 210000000987 immune system Anatomy 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 238000009304 pastoral farming Methods 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 238000009374 poultry farming Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- 230000009467 reduction Effects 0.000 description 1
- 230000001850 reproductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- LDLBBMMTGZHQJD-UHFFFAOYSA-N sodium metavanadate dihydrate Chemical compound O.O.[Na+].[O-][V](=O)=O LDLBBMMTGZHQJD-UHFFFAOYSA-N 0.000 description 1
- JBJWASZNUJCEKT-UHFFFAOYSA-M sodium;hydroxide;hydrate Chemical compound O.[OH-].[Na+] JBJWASZNUJCEKT-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- 238000001291 vacuum drying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- 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
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
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- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
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- C02F2101/38—Organic compounds containing nitrogen
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses an alpha-Fe 2 O 3 /V 2 O 5 A method for preparing the BC composite material comprises the following steps: s1, selecting pine needles as raw materials for preparing graphitized biochar, and crushing the pine needles to obtain pine needle powder; s2, dispersing the pine needle powder obtained in the step S1 into a mixed solution prepared from sodium metavanadate and ferric chloride, and uniformly mixing and stirring to obtain a solid-liquid reaction system; s3, evaporating the solid-liquid reaction system obtained in the step S2 on an electric heating plate, transferring the evaporated solid-liquid reaction system into a tubular furnace, and performing anaerobic co-pyrolysis reactionAnd (3) after the reaction is finished, cleaning and drying the solid-phase product to obtain the composite material. The invention also provides the alpha-Fe 2 O 3 /V 2 O 5 Application of activated persulfate of BC composite material in removing pharmaceutical antibiotic wastewater. The composite material has strong photocatalytic activation persulfate oxidation performance and wide pH application range, can efficiently remove tetracycline pollution in water, and can be used for purifying water polluted by tetracycline in pharmaceutical wastewater.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to an alpha-Fe 2 O 3 /V 2 O 5 A preparation method of a BC composite material and application of the graphitized biochar-based composite material in removing pharmaceutical antibiotic wastewater.
Background
Antibiotic factor has broad-spectrum antibacterial property and is widely used in medical treatment and livestock and poultry farming industry. Although antibiotics can effectively treat human and animal diseases and promote the growth of livestock and poultry, the organisms have poor metabolic capability, and most antibiotics entering the organisms can be discharged into the environment in the form of raw medicines through feces. At present, the presence of antibiotic contaminants has been found in environmental media such as surface water, groundwater, soil, and the like. Although the concentration in environmental bodies of water is often at trace levels, it has toxic, persistent and bioaccumulative effects, and long-term exposure can affect nerves, the immune system, etc., and even reproductive development. Therefore, the efficient removal of the antibiotic pollution attracts attention in all circles, and development of green, efficient, economically feasible treatment technology is needed to solve the serious antibiotic pollution in the environment.
The main methods for removing antibiotics are adsorption, membrane treatment, photocatalytic oxidation, biological methods, and the like. Among them, the photocatalytic oxidation method is considered as a highly efficient method that can thoroughly remove antibiotic contamination. However, the photocatalyst developed at present has some defects in the water treatment application process: 1) Limited oxidation performance; 2) The nano catalytic material has high surface tension and is easy to agglomerate; 3) The catalyst has the advantages of limited service life, complicated regeneration procedure and high regeneration cost. Therefore, aiming at the problems, it is necessary to develop a green high-efficiency photocatalytic composite material which has excellent oxidation performance, strong hydrophilicity and easy regeneration.
V 2 O 5 Is a catalytic material with narrow band gap and excellent visible light absorption and catalytic performance, gradually becomes a research hot spot in the environmental field, and is widely applied to the purification work of organic polluted water bodies. But has high photogenerated carrier recombination rate and nanometer V in the application process 2 O 5 And the defects of easy agglomeration and the like limit the engineering application of the polymer. Therefore, finding a proper heterojunction material to change the photogenerated carrier transmission path and realizing the improvement of the hydrophilic performance through the carrier loading form is a key for solving the application defect.
Disclosure of Invention
Against the existing V 2 O 5 The invention provides a technical bottleneck in the application process of a photocatalysis material, and provides an alpha-Fe 2 O 3 And graphitized biochar co-modified composite material, solving the problem of the prior V 2 O 5 The photo-generated carrier in the application process has high recombination rate and nanometer V 2 O 5 The defect of easy agglomeration is solved, and the method is applied to efficiently activating persulfate to remove antibiotic pollution in wastewater, such as tetracycline wastewater.
In order to solve the technical problems, the invention provides the following technical scheme:
alpha-Fe 2 O 3 /V 2 O 5 A method of preparing a BC composite, the method comprising the steps of:
s1, selecting pine needles as raw materials of graphitized biochar, cleaning and drying collected pine needles with tap water, and grinding by using a crusher to obtain pine needle powder; preferably, the pine needle powder has a particle size in the range of 180-250 μm.
S2, dispersing sodium metavanadate and ferric chloride and the pine needle powder obtained in the step S1 into deionized water, and uniformly mixing to obtain a solid-liquid reaction system;
preferably, the mixing condition is that pine needle powder is added after sodium metavanadate and ferric chloride are dissolved, and mechanical stirring is carried out for 10-20 minutes, wherein the mass ratio of Fe to V to pine needle powder in the solid-liquid reaction system is 0.5:0.5:10, namely the mass ratio of Fe element, V element and pine needle powder in the raw materials is 0.5:0.5:10. The heating temperature of the solid-liquid reaction system on the electric heating plate is 80 ℃, and a slurry system with the water content lower than 15% is obtained. The heating function is as follows: the ferric chloride and sodium metavanadate solution is evaporated to slurry, so that the active ingredients Fe and V are all adsorbed on the pine needle powder, and the reduction of the active ingredients caused by the loss of the solution is prevented. Then pyrolyzing to make pine needles generate biochar, and simultaneously completely converting Fe and V in ferric chloride and sodium metavanadate solution into target products. Preferably, the mass sum of the sodium metavanadate and the ferric chloride and the mass ratio of the pine needle powder are 1:1.
S3, transferring the slurry system obtained in the step S2 to a corundum boat, placing the corundum boat into a tube furnace for anaerobic co-pyrolysis reaction, and sequentially cleaning and drying the obtained black solid phase product after the reaction is finished to obtain the alpha-Fe 2 O 3 /V 2 O 5 BC composite.
Preferably, the anaerobic co-pyrolysis reaction condition is that the reaction is carried out for 4 hours under the nitrogen protection atmosphere at 500 ℃, the heating rate is controlled at 10 ℃/min, the solid phase product is washed to be neutral by absolute ethyl alcohol and deionized water, and then the solid phase product is dried.
The invention also provides the alpha-Fe 2 O 3 /V 2 O 5 The application of the BC composite material in removing tetracycline pollution in wastewater by activating persulfate.
The application of the degradation to remove tetracycline pollution in wastewater comprises the following steps:
1) Subjecting the alpha-Fe to 2 O 3 /V 2 O 5 Mixing the BC composite material, sodium peroxomonosulphate and the tetracycline solution to obtain a mixed system;
2) Magnetically stirring the mixed system under the illumination condition of a xenon lamp, sampling and filtering at intervals; detecting the concentration of the tetracycline in the filtered solution by using high performance liquid chromatography;
3) Filtering after the reaction is finished to obtain the reacted alpha-Fe 2 O 3 /V 2 O 5 Washing the composite material with NaOH water solution to neutrality, stoving to obtain regenerated alpha-Fe 2 O 3 /V 2 O 5 BC composite.
Preferably, the alpha-Fe as described in step 1) 2 O 3 /V 2 O 5 The adding amount of the BC composite material is 0.2g/L, the concentration of the tetracycline solution is 10mg/L, and the reaction pH is controlled to be 3-9. Preferably the optimal reaction pH is 3.
Preferably, the xenon lamp power in step 1) is 300-350W.
alpha-Fe used in the present invention 2 O 3 /V 2 O 5 The BC composite material has the advantages of large specific surface area, strong hydrophilicity, excellent persulfate activation effect and the like.
Compared with the prior art, the invention has the following beneficial effects:
against the existing V 2 O 5 The photocatalyst has the defects of high photon-generated carrier recombination rate, easy agglomeration and the like, and the graphitized biochar is introduced as a carrier material for solving the problem of V 2 O 5 The problems of low efficiency of activating persulfate and hydrophobic agglomeration occur in the application process, and the biochar with excellent adsorption performance can have a concentration effect on tetracycline, so that the contact opportunity with free radicals is accelerated, and the degradation efficiency is improved. The biochar raw material selected by the invention is pine needles, is fallen leaves of arbor pine tree common in the north and south, and belongs to agriculture and forestry waste. Therefore, the carrier has the advantages of wide sources, low price, green and environment-friendly performance and the like, and has great commercial application potential.
Meanwhile, the biochar has rich pore canal structure, and the surface of the biochar contains a large number of hydrophilic functional groups such as-COOH, -OH and the like, and is used as a carrier to load nano V 2 O 5 Can effectively reduce the surface tension of the composite material and improve the hydrophilic performance of the composite material. alpha-Fe 2 O 3 Has excellent electron transport propertyCan effectively promote V 2 O 5 The photo-generated carrier transmission efficiency improves the efficiency of activating persulfate. Thus, the developed alpha-Fe 2 O 3 /V 2 O 5 The BC composite material has important significance in the field of treating the pollution of the antibiotic wastewater and guaranteeing the ecological environment safety.
The invention provides alpha-Fe 2 O 3 /V 2 O 5 The preparation method of the BC composite material is simple, the photocatalytic activation persulfate has strong performance and wide pH application range, can be recycled, can efficiently remove tetracycline pollution in water, and can be used for purifying water polluted by tetracycline in wastewater.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows the various times of the alpha-Fe in test example 1 of the present invention 2 O 3 /V 2 O 5 Results of removal of tetracycline by BC.
FIG. 2 shows the α -Fe at different pH conditions in test example 2 of the present invention 2 O 3 /V 2 O 5 /BC effect on tetracycline contaminant removal performance.
FIG. 3 is a graph showing the effect of various PMS additions on tetracycline contaminant removal efficiency for test example 3 of the present invention.
FIG. 4 shows the coexisting anion pair α -Fe in test example 4 of the present invention 2 O 3 /V 2 O 5 Effect of BC removal of tetracycline contaminant performance.
FIG. 5 shows the alpha-Fe of test example 5 of the present invention 2 O 3 /V 2 O 5 BC reuse performance map.
FIG. 6 shows the alpha-Fe of test example 6 of the present invention 2 O 3 /BC、α-Fe 2 O 3 /V 2 O 5 /BC、V 2 O 5 Results of removal of tetracycline by/BC and BC.
Detailed Description
The technical solutions and the technical problems to be solved in the embodiments of the present invention will be described below in conjunction with the embodiments of the present invention. It will be apparent that the described embodiments are only some, but not all, of the embodiments of the present patent.
Example 1
α-Fe 2 O 3 /V 2 O 5 The preparation method of the BC composite material comprises the following steps:
1) Pretreatment of pine needles: selecting pine needles as graphitized biochar raw materials, cleaning and drying the purchased pine needles with tap water, and grinding by using a crusher; crushing the dried pine needles by using a crusher, and sieving the crushed pine needles by using a 60-80-mesh sieve to obtain pine needle powder with the particle size range of 180-250 mu m.
2)α-Fe 2 O 3 /V 2 O 5 Preparation of BC composite material: 1.55g of sodium metavanadate dihydrate and 2.42g of ferric trichloride hexahydrate are respectively weighed and dissolved in 100mL of deionized water, 10g of pine needle powder is added, and the mass ratio of Fe to V to pine needle powder in a reaction system is 0.5:0.5:10. After mechanical stirring for 10 minutes, heating on an electric plate at 80 ℃ and stirring while heating until the slurry mixed system with the water content lower than 15% is displayed. Transferring the mixed system into a corundum boat, putting the corundum boat into a tube furnace, introducing nitrogen for 5 minutes, starting the tube furnace, setting the reaction temperature to be 500 ℃, setting the reaction time to be 4 hours, and setting the temperature rise program to be 10 ℃/minute. The reaction was continued with nitrogen to maintain anaerobic reaction conditions. And after the reaction is finished, naturally cooling the tubular furnace to room temperature, taking out a black solid phase product, washing the solid phase product to be neutral by using absolute ethyl alcohol and deionized water, and drying for later use.
Test example 1
alpha-Fe prepared in example 1 2 O 3 /V 2 O 5 The BC composite material is applied to photocatalytic activation sodium Persulfate (PMS) oxidative degradation of tetracycline pollution in wastewater, and the application method comprises the following steps:
1)α-Fe 2 O 3 /V 2 O 5 mixing the BC composite material with an aqueous tetracycline solution: weighing 20mg of alpha-Fe according to the addition amount of 0.2g/L 2 O 3 /V 2 O 5 the/BC composite was placed in a quartz tube containing 100mL of tetracycline solution at a concentration of 10mg/L, and 1mM PMS solution was added.
2) The quartz tube was placed on a magnetic stirrer in a photocatalytic reaction device, a 2cm rotor was added, the rotation speed was controlled at 300r/min, the reaction was carried out for 120 minutes under the irradiation of a xenon lamp (300W), and after sampling 3mL at specified time intervals (5, 15, 30, 60, 90 and 120 minutes), the water sample was filtered with a 0.45 μm glass fiber filter. After the reaction is finished, the concentration of the tetracycline in the water sample is tested by utilizing HPLC under the condition of a wave band with the wavelength of 360 nm.
FIG. 1 shows a different time of alpha-Fe 2 O 3 /V 2 O 5 Results of removal of tetracycline by BC. The results show that alpha-Fe prepared by the method of example 1 2 O 3 /V 2 O 5 The BC has better removal performance for the tetracycline, and the removal rate for the tetracycline reaches 88.56% within 120 minutes.
Test example 2
Investigation of different pH vs. alpha-Fe 2 O 3 /V 2 O 5 Effect of BC composite Properties
100ml of tetracycline solution with pH of 3, 5, 7 and 9 are respectively added into a quartz tube according to the alpha-Fe of 0.2mg/L 2 O 3 /V 2 O 5 BC addition amount and PMS addition amount of 1mM to each of the tetracycline solutions of different pH 20mg of alpha-Fe 2 O 3 /V 2 O 5 BC and 1mM PMS, mixed reaction systems A1, A2, A3 and A4 are obtained.
The 4 reaction systems (A1, A2, A3 and A4) were reacted under the irradiation of a xenon lamp (300W) for 120 minutes, 3mL of each reaction system was sampled, and after filtration, the tetracycline concentration was measured by HPLC, and the tetracycline removal rate was calculated.
FIG. 2 shows the removal of tetracycline at various pH values. As can be seen from FIG. 2, in a system with pH 3, alpha-Fe 2 O 3 /V 2 O 5 /BCThe adsorption efficiency of the composite material to the tetracycline is highest, and the removal rate of the tetracycline reaches 98.36% after 120 minutes of reaction.
Test example 3
Examine the effect of PMS addition on tetracycline removal rate
100mL of tetracycline solution (pH=3) was added to each of 4 quartz tubes, and 20mg of α -Fe prepared in example 1 was weighed out in an amount of 0.2mg/L 2 O 3 /V 2 O 5 The reaction system was charged with 1mM, 2mM, 3mM and 4mM PMS solution simultaneously with the respective BC addition to the reactor to obtain 4 reaction systems (B1, B2, B3 and B4). Then, the 4 reaction systems were reacted under light (300W) for 120 minutes, 3mL of each reaction system was sampled, and after filtration, the tetracycline concentration was measured by HPLC, and the tetracycline removal rate was calculated.
FIG. 3 shows the effect of varying PMS addition on tetracycline removal. As can be seen from FIG. 3, the optimal addition amount of PMS was 4mM, and the removal rate of tetracycline was as high as 99.58%. As a result of comparing the removal rate data of the amounts of PMS added at 3mM and 2mM (99.21% and 99.11%, respectively), it was found that the removal rate of tetracycline was similar, but the amount of PMS used was smaller. Therefore, in practical use, the amount of PMS added is preferably 2 mM.
Test example 4
Investigation of coexisting anion pair alpha-Fe in wastewater 2 O 3 /V 2 O 5 Effect of BC composite Properties
Respectively configured to contain Cl - (100 mg/L) and NO 3 - (100 mg/L) two sets of 100mL tetracycline solutions (10 mg/L, pH=3), at 0.2mg/L of alpha-Fe 2 O 3 /V 2 O 5 BC addition amount, 20mg of alpha-Fe prepared in example 1 was added to the tetracycline solution, respectively 2 O 3 /V 2 O 5 And (3) the BC composite material to obtain a mixed reaction system. Meanwhile, the experimental group without adding ions was used as a blank control group. The 3 groups of experimental reaction apparatuses were reacted under irradiation of a xenon lamp (300W) for 120 minutes, 3mL of each reaction system was sampled, and after filtration, the tetracycline concentration was measured by HPLC, and the tetracycline removal rate was calculated.
FIG. 4 is a view of a water bodyCo-anion pair alpha-Fe 2 O 3 /V 2 O 5 Effect of BC composite properties. As can be seen from FIG. 4, α -Fe 2 O 3 /V 2 O 5 The BC composite material has a certain anti-interference performance on anions in the water body and NO 3 - Is stronger than Cl - . Thus, the developed alpha-Fe 2 O 3 /V 2 O 5 the/BC composite material may be suitable for antibiotic removal in a co-existing anionic aqueous environment (e.g., pharmaceutical wastewater).
Test example 5
Investigation of alpha-Fe 2 O 3 /V 2 O 5 Recycling performance of BC composite material
alpha-Fe in test example 1 2 O 3 /V 2 O 5 Based on the BC experiment, the filter membrane is used for filtering the reacted alpha-Fe 2 O 3 /V 2 O 5 Putting the BC composite material into 50mL of NaOH solution with the concentration of 1mmol/L, magnetically stirring for 30min, filtering out supernatant, washing with deionized water for 3 times, putting the BC composite material into a vacuum drying oven at 100 ℃ for drying for 12 hours, and weighing to obtain regenerated alpha-Fe 2 O 3 /V 2 O 5 BC composite. The regenerated material was subjected to a photocatalytic activation persulfate experiment, and was cycled 6 times according to the procedure of test example 1, and alpha-Fe was evaluated by calculating the tetracycline removal rate 2 O 3 /V 2 O 5 BC reuse performance.
FIG. 5 is alpha-Fe 2 O 3 /V 2 O 5 The removal rate of tetracycline after 6 times of BC repeat experiments, wherein CK is a blank group, namely a single tetracycline solution. The results show that alpha-Fe 2 O 3 /V 2 O 5 After 6 times of circulating experiments of the BC composite material, the efficiency of activating PMS to degrade four rings is still up to 91.27 percent. alpha-Fe 2 O 3 /V 2 O 5 The BC can be repeatedly used for multiple times, so that the engineering application cost of the material can be effectively reduced, and the BC has wide engineering application prospect.
Test example 6
Investigation of alpha-Fe 2 O 3 /BC、α-Fe 2 O 3 /V 2 O 5 /BC、V 2 O 5 Removal of tetracycline by/BC and BC. Wherein alpha-Fe 2 O 3 /V 2 O 5 BC was prepared as in example 1. alpha-Fe 2 O 3 /BC、V 2 O 5 BC is BC loaded with alpha-Fe only 2 O 3 Or V 2 O 5 Prepared, alpha-Fe 2 O 3 Or V 2 O 5 The loading on BC was the same as in example 1, BC being biochar. FIG. 6 is a graph showing the removal of tetracycline from the above composite material over 120 minutes. As can be seen from the figure, the alpha-Fe prepared in example 1 was used 2 O 3 /V 2 O 5 The performance of activating PMS to degrade tetracycline under the illumination condition of BC is best, and the removal rate of tetracycline reaches 88.56% within 120 minutes. Illustrating that the surface of the biochar is simultaneously loaded with alpha-Fe 2 O 3 /V 2 O 5 The resulting composite material has optimal performance in activating PMS to remove tetracycline.
Examples 2 to 5
The mass ratio of Fe and V elements in example 1 was changed, and the other preparation procedures were the same as in example 1 to obtain alpha-Fe of examples 2 to 5 2 O 3 /V 2 O 5 BC composite wherein the alpha-Fe of example 2 2 O 3 BC is 1:9, α -Fe of example 3 2 O 3 BC is 3:7, example 4. Alpha. -Fe 2 O 3 BC is 7:3, example 5. Alpha. -Fe 2 O 3 BC is 9:1.
The above composite materials were added to the tetracycline solution to react for 120 minutes by the method of test example 1, respectively, the tetracycline concentration at the end of the reaction was measured, and the tetracycline removal rate was calculated. The specific settings and test results are shown in Table 1, which illustrates that when the addition amount of pine needle powder is fixed, alpha-Fe 2 O 3 BC is 5:5, i.e. the α -Fe of example 1 2 O 3 /V 2 O 5 The BC composite material has the best photocatalytic degradation effect.
TABLE 1
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (9)
1. alpha-Fe 2 O 3 /V 2 O 5 A method for preparing a BC composite, comprising the steps of:
s1, selecting pine needles as raw materials for preparing graphitized biochar, and crushing the pine needles to obtain pine needle powder;
s2, dispersing the pine needle powder obtained in the step S1 into a mixed solution prepared from sodium metavanadate and ferric chloride, and uniformly mixing to obtain a solid-liquid reaction system;
s3, evaporating the solid-liquid reaction system obtained in the step S2 on an electric heating plate, transferring the evaporated solid-liquid reaction system into a tube furnace for reaction, and cleaning and drying a solid-phase product after the reaction is finished to obtain the alpha-Fe 2 O 3 /V 2 O 5 BC composite.
2. alpha-Fe according to claim 1 2 O 3 /V 2 O 5 The preparation method of the BC composite material is characterized in that in the step S1, the particle size range of the pine needle powder is 180-250 mu m.
3. alpha-Fe according to claim 1 2 O 3 /V 2 O 5 The preparation method of the BC composite material is characterized in that in the step S2, the mixing condition is that pine needle powder is added after sodium metavanadate and ferric chloride are dissolved, and the mixture is mechanically stirred for 10-20 minutes, wherein the mass ratio of Fe to V to pine needle powder in a solid-liquid reaction system is 0.5:0.5:10.
4. alpha-Fe according to claim 1 2 O 3 /V 2 O 5 The preparation method of the BC composite material is characterized in that in the step S3, the heating temperature of a solid-liquid reaction system on an electric plate is 80 ℃, the pyrolysis condition is that the solid-liquid reaction system reacts for 4 hours under the atmosphere of 500 ℃ nitrogen protection, the heating rate is controlled at 10 ℃/min, the solid-phase product is washed to be neutral by adopting absolute ethyl alcohol and deionized water, and then the solid-phase product is dried.
5. An alpha-Fe obtained by the process according to any one of claims 1 to 4 2 O 3 /V 2 O 5 BC composite.
6. The α -Fe of claim 5 2 O 3 /V 2 O 5 The application of the BC composite material in removing tetracycline pollution in pharmaceutical wastewater by activating persulfate.
7. The use according to claim 6, characterized in that it comprises the steps of:
1) Subjecting the alpha-Fe to 2 O 3 /V 2 O 5 Mixing the BC composite material with sodium persulfate and a tetracycline solution to obtain a mixed system;
2) Stirring the mixed system, irradiating the mixed system by using a xenon lamp, sampling and filtering at certain intervals; detecting the concentration of the tetracycline in the filtered solution by using high performance liquid chromatography;
3) By filtration of the alpha-Fe 2 O 3 /V 2 O 5 Desorbing the BC composite material with NaOH aqueous solution, washing to neutrality, and drying to obtain regenerated alpha-Fe 2 O 3 /V 2 O 5 BC composite.
8. The use according to claim 7, wherein the α -Fe of step 1) 2 O 3 /V 2 O 5 The adding amount of the BC composite material is 0.2g/L, the concentration of the tetracycline solution is 10mg/L, and the reaction pH is controlled to be 3-9.
9. The use according to claim 8, wherein the reaction pH is 3.
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