CN106824210B - A kind of magnetic Fe3O4@C/TiO2-In2O3Composite photo-catalyst and preparation method and purposes - Google Patents
A kind of magnetic Fe3O4@C/TiO2-In2O3Composite photo-catalyst and preparation method and purposes Download PDFInfo
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 60
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 36
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000004098 Tetracycline Substances 0.000 claims abstract description 17
- 229960002180 tetracycline Drugs 0.000 claims abstract description 17
- 229930101283 tetracycline Natural products 0.000 claims abstract description 17
- 235000019364 tetracycline Nutrition 0.000 claims abstract description 17
- 150000003522 tetracyclines Chemical class 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000013019 agitation Methods 0.000 claims abstract description 12
- 241000235342 Saccharomycetes Species 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 8
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000001632 sodium acetate Substances 0.000 claims abstract description 7
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000012265 solid product Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 230000000593 degrading effect Effects 0.000 claims abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000002604 ultrasonography Methods 0.000 claims description 8
- 239000002351 wastewater Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims 2
- 229940047670 sodium acrylate Drugs 0.000 claims 2
- 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 claims 1
- 229960000583 acetic acid Drugs 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 229960004249 sodium acetate Drugs 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 18
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 238000000643 oven drying Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 239000012467 final product Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000005276 aerator Methods 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000006652 catabolic pathway Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- -1 includes hydrolysis Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/825—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 gallium, indium or thallium
-
- 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
- B01J35/33—Electric or magnetic properties
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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
-
- 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
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of magnetic Fes3O4@C/TiO2‑In2O3Composite photo-catalyst and preparation method and purposes, preparation step is as follows: saccharomycete, ferric chloride hexahydrate, acrylic acid being received, sodium acetate is added in ethylene glycol/diethylene glycol (DEG) mixed liquor, ultrasonic treatment, magnetic agitation after mixing to be dissolved, is transferred in the reaction kettle of polytetrafluoroethyllining lining and carries out solvent thermal reaction, after completion of the reaction, solid product is washed, drying obtains Fe3O4@C；By Fe3O4@C is scattered in dehydrated alcohol, ultrasonic disperse, adds In (NO3)3, butyl titanate and deionized water, magnetic agitation is uniform, obtains mixed liquor, and mixed liquor is transferred in the reaction kettle of polytetrafluoroethyllining lining and carries out solvent thermal reaction；After completion of the reaction, solid product is washed, drying obtains magnetic Fe3O4@C/TiO2–In2O3Composite photo-catalyst.Material prepared by the present invention has good photocatalyst for degrading effect to tetracycline.
Description
Technical field
The present invention relates to the magnetic carbon-based materials prepared using saccharomycete as carbon source to load TiO2-In2O3Composite photo-catalyst,
And preparation-obtained magnetic composite photocatalyst to be used for the research of tetracycline in wastewater by photocatalysis.Belong to environmentally conscious materials
Preparation technical field.
Background technique
Tetracycline antibiotics are currently that the whole world is most widely used, and the maximum a kind of antibiotic of dosage has relatively strong
Persistence, the features such as bioaccumulation and bio-refractory, long-term existence in human body and animal body, to human health and
Ecological environment brings potentially hazardous.Currently, the medical pollutant of residual in the environment affects ring in various ways
Organism in border.
The degradation pathway of tetracycline mainly includes hydrolysis, photocatalytic degradation and biodegrade.Wherein Photocatalyst
It is a kind of means of most prospect.It is known that TiO2It is a kind of semiconductor material with excellent photocatalysis performance, Er Qieqi
The advantages that itself is more stable, without secondary pollution is as the hot spot studied at present, but TiO2There is also some disadvantages, such as band
Gap can be excessive, and light absorption wavelength range is mainly in ultra-violet (UV) band.In2O3As a kind of low-gap semiconductor, forbidden bandwidth is
2.8eV is a kind of efficient sensitizer, can effectively extend the light abstraction width of oxide semiconductor catalysis material, institute
With by TiO2With In2O3It is compound to increase TiO2Absorption to visible light improves photocatalytic activity.Furthermore, it is contemplated that photocatalysis
The practical application of agent, easily separated and recyclable recycle is highly important, therefore we are prepared for using saccharomycete as carbon source
Fe3O4@C/TiO2–In2O3Magnetic composite photocatalyst, not only with magnetism but also with good photocatalytic activity, this, which is solved, is urged
Agent is difficult to the problem of recycling and reusing and TiO2The problem low to visible light utilization efficiency, to improve the effect of photocatalytic degradation
Rate.
Summary of the invention
The purpose of the present invention is prepare magnetic Fe using hydro-thermal method as technological means3O4@C/TiO2–In2O3Composite photocatalyst
Agent.
The present invention is achieved through the following technical solutions:
A kind of magnetic Fe3O4@C/TiO2-In2O3Composite photo-catalyst, the composite photo-catalyst are by Fe3O4、C、TiO2
And In2O3It is combined, Fe3O4Surface coats one layer C layers, forms Fe3O4@C；Fe3O4@C Surface coats one layer of TiO2, formed
Fe3O4@C/TiO2；In2O3It is in granular form, is supported on Fe3O4@C/TiO2Surface.
A kind of magnetic Fe3O4@C/TiO2-In2O3The preparation method of composite photo-catalyst, steps are as follows:
Step 1, magnetic Fe3O4The preparation of@C:
Saccharomycete, ferric chloride hexahydrate, acrylic acid are received, sodium acetate is added in ethylene glycol/diethylene glycol (DEG) mixed liquor, ultrasound
Processing, magnetic agitation after mixing to be dissolved, are transferred in the reaction kettle of polytetrafluoroethyllining lining and carry out solvent thermal reaction, react
After, solid product is washed, drying obtains magnetic Fe3O4@C；
Step 2, magnetic Fe3O4@C/TiO2–In2O3The preparation of composite photo-catalyst:
By Fe3O4@C is scattered in dehydrated alcohol, ultrasonic disperse, adds In (NO3)3, butyl titanate and deionization
Water, magnetic agitation is uniform, obtains mixed liquor, and it is anti-that mixed liquor is transferred to progress solvent heat in the reaction kettle of polytetrafluoroethyllining lining
It answers；After completion of the reaction, solid product is washed, drying obtains magnetic Fe3O4@C/TiO2–In2O3Composite photo-catalyst.
In step 1, the saccharomycete, ferric chloride hexahydrate, acrylic acid are received, sodium acetate is in ethylene glycol/diethylene glycol (DEG) mixed liquor
In mass concentration ratio be 1~5:24:34:34；In the ethylene glycol/diethylene glycol (DEG) mixed liquor, the volume ratio of ethylene glycol, diethylene glycol (DEG)
For 1:1.
In step 1, the temperature of the solvent thermal reaction is 200 DEG C, reaction time 10h.
In step 2, used Fe3O4@C, dehydrated alcohol, In (NO3)3, butyl titanate and deionized water amount ratio
For 0.2g:40mL:0.1~0.9mmol:0.2mL:0.1mL.
In step 2, the temperature of the solvent thermal reaction is 180 DEG C；Reaction time is 12 hours.
The magnetic Fe that preparation method as described above obtains3O4@C/TiO2–In2O3Composite photo-catalyst is applied to drop
Solve the tetracycline in waste water.
The utility model has the advantages that
The present invention prepares magnetic Fe by carbon source of saccharomycete3O4@C/TiO2–In2O3Composite material, and successfully as light
Tetracycline in catalyst degradation waste water.The introducing of magnetic photocatalyst can be such that photochemical catalyst returns using externally-applied magnetic field quick separating
It receives, avoids secondary pollution caused by photochemical catalyst remains in the solution, this method will not result in waste of resources and additional pollution
Formation, and easy to operate, cost is relatively low, is a kind of environmentally protective efficient process technology.
Detailed description of the invention
Fig. 1 is Fe3O4@C/TiO2–In2O3TEM figure, wherein figure b be figure a partial enlarged view；
Fig. 2 is Fe3O4@C/TiO2–In2O3Photocatalytic degradation tetracycline absorption spectrum variation diagram；
Fig. 3 is that the photochemical catalyst of different carbon contents is containing the photocatalytic degradation effect figure in tetracycline wastewater；
Fig. 4 is magnetic Fe3O4@C/TiO2–In2O35 circulation lights of composite photo-catalyst photocatalytic degradation tetracycline
Catalytic effect diagram；
Fig. 5 is the Magneto separate characteristic spectrogram of composite photo-catalyst.
Specific embodiment
Below with reference to specific implementation example, the present invention will be further described.
The photocatalytic activity evaluation of prepared photochemical catalyst in the present invention: in DW-01 type photochemical reactor (purchased from raising
State Science and Technology Ltd., university city) in carry out, simulated solar irradiation irradiation, will 100mL tetracycline simulated wastewater be added reactor in
And its initial value is measured, then it is added photochemical catalyst obtained, magnetic agitation simultaneously opens aerator and is passed through air and keep catalysis
Agent is in suspension or afloat, is spaced 10min sampling analysis in During Illumination, takes supernatant liquor in light splitting light after centrifuge separation
Absorbance is measured at degree meter λ max=357nm, and passes through formula: Dr=(C0-C)×100/C0Its degradation rate Dr is calculated, wherein C0
To reach concentration after adsorption equilibrium, C is the concentration of the tetracycline of t moment measurement, and t is the reaction time.
Embodiment 1:
(1) magnetic Fe3O4The preparation of@C nano microballoon
A. 0.1g saccharomycete, 2.4g ferric chloride hexahydrate are weighed, 3.4g acrylic acid is received, and 3.4g sodium acetate is dissolved in 22.5mL
In the beaker of ethylene glycol and 22.5mL diethylene glycol (DEG), mixed solution ultrasound about 1 hour, magnetic agitation shifted solution after to be dissolved
Into the reaction kettle of 100ml polytetrafluoroethyllining lining, 10h is reacted at 200 DEG C, after being cooled to room temperature, by product deionized water
It is washed respectively three times with dehydrated alcohol, is put into 65 DEG C of baking oven drying.(2)Fe3O4@C/TiO2–In2O3The preparation of composite photo-catalyst
Weigh 0.2g Fe3O4@C is dissolved in the beaker of 40ml dehydrated alcohol, and mixed solution ultrasound about 30min divides completely
It dissipates.Secondly, weighing the In of different molal weights (0.1mmol, 0.3mmol, 0.5mmol, 0.7mmol, 0.9mmol) respectively
(NO3)3, 0.2mL butyl titanate and 0.1mL deionized water are added to magnetic agitation 10min in above-mentioned solution.Gained suspension
It is transferred in the reaction kettle of 100ml polytetrafluoroethyllining lining, 180 DEG C of holding 12h, after being cooled to room temperature, by product deionization
Water and dehydrated alcohol are washed three times respectively, 65 DEG C of baking oven drying are put into, according to In (NO3)3Dosage, final product is successively denoted as
Fe3O4@C/TiO2–In2O3-0.1；Fe3O4@C/TiO2–In2O3-0.3；Fe3O4@C/TiO2–In2O3-0.5； Fe3O4@C/TiO2–
In2O3-0.7；Fe3O4@C/TiO2–In2O3-0.9。
Embodiment 2:
B. 0.3g saccharomycete, 2.4g ferric chloride hexahydrate are weighed, 3.4g acrylic acid is received, and 3.4g sodium acetate is dissolved in 22.5mL
In the beaker of ethylene glycol and 22.5mL diethylene glycol (DEG), mixed solution ultrasound about 1 hour, magnetic agitation shifted solution after to be dissolved
Into the reaction kettle of 100ml polytetrafluoroethyllining lining, 10h is reacted at 200 DEG C, after being cooled to room temperature, by product deionized water
It is washed respectively three times with dehydrated alcohol, is put into 65 DEG C of baking oven drying.(2)Fe3O4@C/TiO2–In2O3The preparation of composite photo-catalyst
Weigh 0.2g Fe3O4@C is dissolved in the beaker of 40ml dehydrated alcohol, and mixed solution ultrasound about 30min divides completely
It dissipates.Secondly, weighing the In of different molal weights (0.1mmol, 0.3mmol, 0.5mmol, 0.7mmol, 0.9mmol) respectively
(NO3)3, 0.2mL butyl titanate and 0.1mL deionized water are added to magnetic agitation 10min in above-mentioned solution.Gained suspension
It is transferred in the reaction kettle of 100ml polytetrafluoroethyllining lining, 180 DEG C of holding 12h, after being cooled to room temperature, by product deionization
Water and dehydrated alcohol are washed three times respectively, are put into 65 DEG C of baking oven drying, final product is successively denoted as Fe3O4@C/TiO2–In2O3-
0.1； Fe3O4@C/TiO2–In2O3-0.3；Fe3O4@C/TiO2–In2O3-0.5；Fe3O4@C/TiO2–In2O3-0.7； Fe3O4@C/
TiO2–In2O3-0.9。
Embodiment 3:
C. 0.5g saccharomycete, 2.4g ferric chloride hexahydrate are weighed, 3.4g acrylic acid is received, and 3.4g sodium acetate is dissolved in 22.5mL
In the beaker of ethylene glycol and 22.5mL diethylene glycol (DEG), mixed solution ultrasound about 1 hour, magnetic agitation shifted solution after to be dissolved
Into the reaction kettle of 100ml polytetrafluoroethyllining lining, 10h is reacted at 200 DEG C, after being cooled to room temperature, by product deionized water
It is washed respectively three times with dehydrated alcohol, is put into 65 DEG C of baking oven drying.(2)Fe3O4@C/TiO2–In2O3The preparation of composite photo-catalyst
Weigh 0.2g Fe3O4@C is dissolved in the beaker of 40ml dehydrated alcohol, and mixed solution ultrasound about 30min divides completely
It dissipates.Secondly, weighing the In of different molal weights (0.1mmol, 0.3mmol, 0.5mmol, 0.7mmol, 0.9mmol) respectively
(NO3)3, 0.2mL butyl titanate and 0.1mL deionized water are added to magnetic agitation 10min in above-mentioned solution.Gained suspension
It is transferred in the reaction kettle of 100ml polytetrafluoroethyllining lining, 180 DEG C of holding 12h, after being cooled to room temperature, by product deionization
Water and dehydrated alcohol are washed three times respectively, are put into 65 DEG C of baking oven drying, final product is successively denoted as Fe3O4@C/TiO2–In2O3-
0.1； Fe3O4@C/TiO2–In2O3-0.3；Fe3O4@C/TiO2–In2O3-0.5；Fe3O4@C/TiO2–In2O3-0.7； Fe3O4@C/
TiO2–In2O3-0.9。
Embodiment 4:
It is carried out by the same step of 1 preparation process of embodiment, the difference is that weighing the Fe of 0.1g in (2)3O4@C/TiO2–
In2O3- 0.1 photochemical catalyst is placed on progress photocatalytic degradation test in photochemical reactor, measures the photochemical catalyst to tetracycline
Degradation rate reach 34% in 60min.
Embodiment 5:
It is carried out by the same step of 1 preparation process of embodiment, the difference is that weighing the Fe of 0.1g in (2)3O4@C/TiO2–
In2O3- 0.3 photochemical catalyst is placed on progress photocatalytic degradation test in photochemical reactor, measures the photochemical catalyst to tetracycline
Degradation rate reach 54% in 60min.
Embodiment 6:
It is carried out by the same step of 1 preparation process of embodiment, the difference is that weighing the Fe of 0.1g in (2)3O4@C/TiO2–
In2O3- 0.5 photochemical catalyst is placed on progress photocatalytic degradation test in photochemical reactor, measures the photochemical catalyst to tetracycline
Degradation rate reach 72% in 60min.
Embodiment 7:
It is carried out by the same step of 1 preparation process of embodiment, the difference is that weighing the Fe of 0.1g in (2)3O4@C/TiO2–
In2O3- 0.7 photochemical catalyst is placed on progress photocatalytic degradation test in photochemical reactor, measures the photochemical catalyst to tetracycline
Degradation rate reach 48% in 60min.
Embodiment 8:
It is carried out by the same step of 1 preparation process of embodiment, the difference is that weighing the Fe of 0.1g in (2)3O4@C/TiO2–
In2O3- 0.9 photochemical catalyst carries out photocatalytic degradation test in photochemical reactor, measures the photochemical catalyst to tetracycline
Degradation rate reaches 32% in 60min.
It can be seen that from FIG. 1 a that Fe3O4Surface successfully coats one layer of carbon-coating, as can be seen that Fe from enlarged drawing 1b3O4@
The surface C successfully coats a thin layer of TiO2, and can be seen that In2O3It is graininess, is supported on its surface.
From in Fig. 2 abosrption spectrogram as can be seen that by after 60 minutes, tetracycline has been decomposed, and explanation is urged
Agent has activity well.
From figure 3, it can be seen that as the In (NO that 0.9mmol is added3)3When, catalyst activity is worst, reaches 32%, when adding
Enter the In (NO of 0.5mmol3)3When, preferably, degradation rate reaches 72% to the activity of photochemical catalyst.
Fig. 4, which is shown, passes through 5 circulation experiments, magnetic Fe3O4@C/TiO2–In2O3The photocatalysis of -0.5 composite photo-catalyst is dropped
Solution rate varies less, and illustrates prepared magnetic Fe3O4@C/TiO2–In2O3- 0.5 composite photo-catalyst has good photochemical
Learn stability.
As can be seen from Figure 5 Fe3O4Magnetic best, magnetic saturation intensity is up to 78emu/g or so, Fe3O4@C/TiO2–
In2O3Magnetic relatively weak, magnetic saturation intensity is up to 48emu/g or so, it may have preferable Magneto separate characteristic.
Claims (4)
1. a kind of magnetic Fe3O4@C/TiO2-In2O3A kind of composite photo-catalyst, which is characterized in that magnetic Fe3O4@C/TiO2-
In2O3Composite photo-catalyst, the composite photo-catalyst are by Fe3O4、C、TiO2And In2O3It is combined, Fe3O4Surface packet
One layer C layers are covered, Fe is formed3O4@C；Fe3O4@C Surface coats one layer of TiO2, form Fe3O4@C/TiO2；In2O3It is in granular form, bears
It is loaded in Fe3O4@C/TiO2Surface；Steps are as follows:
Step 1, magnetic Fe3O4The preparation of@C:
Saccharomycete, ferric chloride hexahydrate, sodium acrylate, sodium acetate are added in ethylene glycol/diethylene glycol (DEG) mixed liquor, at ultrasound
Reason, magnetic agitation after mixing to be dissolved, are transferred in the reaction kettle of polytetrafluoroethyllining lining and carry out solvent thermal reaction, reacted
Bi Hou, washs solid product, and drying obtains magnetic Fe3O4@C；The saccharomycete, ferric chloride hexahydrate, sodium acrylate, acetic acid
Mass concentration ratio of the sodium in ethylene glycol/diethylene glycol (DEG) mixed liquor is 1~5:24:34:34；The ethylene glycol/diethylene glycol (DEG) mixed liquor
In, ethylene glycol, diethylene glycol (DEG) volume ratio be 1:1；
Step 2, magnetic Fe3O4@C/TiO2–In2O3The preparation of composite photo-catalyst:
By Fe3O4@C is scattered in dehydrated alcohol, ultrasonic disperse, adds In (NO3)3, butyl titanate and deionized water, magnetic force
It stirs evenly, obtains mixed liquor, mixed liquor is transferred in the reaction kettle of polytetrafluoroethyllining lining and carries out solvent thermal reaction；Reaction
After, solid product is washed, drying obtains magnetic Fe3O4@C/TiO2–In2O3Composite photo-catalyst；Used Fe3O4@
C, dehydrated alcohol, In (NO3)3, butyl titanate and deionized water amount ratio be 0.2g:40mL:0.1~0.9mmol:
0.2mL:0.1mL。
2. a kind of magnetic Fe according to claim 13O4@C/TiO2-In2O3Composite photo-catalyst, which is characterized in that step
In 1, the temperature of the solvent thermal reaction is 200 DEG C, reaction time 10h.
3. a kind of magnetic Fe according to claim 13O4@C/TiO2-In2O3Composite photo-catalyst, which is characterized in that step
In 2, the temperature of the solvent thermal reaction is 180 DEG C；Reaction time is 12 hours.
4. magnetic Fe described in claims 1 to 3 any one3O4@C/TiO2-In2O3The purposes of composite photo-catalyst, feature
It is, the magnetic Fe3O4@C/TiO2–In2O3Composite photo-catalyst is for the tetracycline in degrading waste water.
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