CN110038572A - A kind of α-Fe for degradable organic pollutant2O3/ Fe photochemical catalyst and preparation method thereof - Google Patents
A kind of α-Fe for degradable organic pollutant2O3/ Fe photochemical catalyst and preparation method thereof Download PDFInfo
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- CN110038572A CN110038572A CN201910369715.7A CN201910369715A CN110038572A CN 110038572 A CN110038572 A CN 110038572A CN 201910369715 A CN201910369715 A CN 201910369715A CN 110038572 A CN110038572 A CN 110038572A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims abstract description 27
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 18
- 239000011941 photocatalyst Substances 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 16
- 239000002114 nanocomposite Substances 0.000 claims description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- -1 boron hydrogen salt Chemical class 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 229910052796 boron Inorganic materials 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000010907 mechanical stirring Methods 0.000 claims description 6
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 230000033116 oxidation-reduction process Effects 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 230000031709 bromination Effects 0.000 claims description 2
- 238000005893 bromination reaction Methods 0.000 claims description 2
- 229960004756 ethanol Drugs 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- LGRLWUINFJPLSH-UHFFFAOYSA-N methanide Chemical compound [CH3-] LGRLWUINFJPLSH-UHFFFAOYSA-N 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims 1
- 229910000104 sodium hydride Inorganic materials 0.000 claims 1
- 239000012312 sodium hydride Substances 0.000 claims 1
- 238000006731 degradation reaction Methods 0.000 abstract description 22
- 230000015556 catabolic process Effects 0.000 abstract description 20
- 239000005416 organic matter Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 238000005286 illumination Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000010815 organic waste Substances 0.000 abstract description 2
- 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 16
- 229940043267 rhodamine b Drugs 0.000 description 16
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000002135 nanosheet Substances 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 238000003795 desorption Methods 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000002703 mutagenesis Methods 0.000 description 1
- 231100000350 mutagenesis Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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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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- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- 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
- C02F1/722—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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
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- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/36—Organic compounds containing halogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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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
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- C02F2305/10—Photocatalysts
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Abstract
The present invention provides a kind of α-Fe for degradable organic pollutant2O3/ Fe photochemical catalyst and preparation method thereof, the present invention prepared by catalyst α-Fe2O3/ Fe is nanometer chip architecture, when considerably increasing reaction and the contact area and active site quantity of organic pollutant, improves the degradation rate of organic matter；The driving force of degradation of organic substances is illumination, does not need the consumption of other extra powers, is a kind of efficient, energy-saving and environmental protection organic matter degradation process；Photochemical catalyst according to the present invention is versatile, has good degradation effect to the organic waste Organic substance in water within the scope of larger pH.
Description
Technical field
The present invention provides a kind of α-Fe for degradable organic pollutant2O3/ Fe photochemical catalyst and preparation method thereof, can answer
For advanced treatment of wastewater field.
Background technique
With dyestuff and pigment weaving, printing, in terms of extensive use, cause environment especially water to provide
Source is contaminated.Most of dyestuffs have carcinogenic, mutagenesis and micro- toxicity, even if concentration is very low in water, also to the mankind and
Aquatic ecosystem has serious harm.Currently, from sewage remove and handle organic pollutant method mainly have physical method,
Chemical method and bioanalysis, such as the methods of micro-filtration, ultrafiltration, reverse osmosis, ion exchange, aerobic and Anaerobic Treatment.These methods are being gone
Except being possible to generate more stronger than original hazard of contaminant secondary pollution in the process.In various minimizing technologies, advanced oxidation
Technique (AOPs) has been generally considered a low in cost and effective method, by generating the hydroxyl radical free radical of high activity,
To realize that degradable organic pollutant, reduction secondary pollution generate (J.Mater.Chem.A.2015,3:8537-8544).
Conductor photocatalysis is the Advantageous techniques for solving energy crisis and problem of environmental pollution, is a kind of efficient, green
Heliotechnics.In recent years, α-Fe2O3It is inexpensive due to its rich content, corrosion resistance, good chemical stability, and
The characteristics such as excellent environment compatibility are widely used in photocatalysis (photocatalytic water and light degradation organic matter), gas sensor, field
The fields such as ballistic device, electrode of lithium cell.Importantly, α-Fe2O3Possess relatively narrow band gap (2.1eV), can make full use of
Visible light.However, although possessing these advantages, α-Fe2O3There is also some defects, such as slower kinetics, weak electricity
Lotus transport with stalling characteristic and very small hole-diffusion length (2-4nm), be very restricted its practical application.Cause
And so far, more and more researchs are dedicated to such as adjusting α-Fe by various strategies and method2O3Texture and pattern
(increasing light absorption and specific surface area) (adjusts band structure, promotes photoproduction current-carrying with other semiconductor materials building heterojunction structure
Son is transported and is separated) etc. (Inorg.Chem.2011,50:10143-10151), to prepare high catalytic activity α-Fe2O3Base light is urged
Agent is to overcome these disadvantages.
Summary of the invention
To improve α-Fe2O3The separation of photo-generated carrier solves the problems, such as that kinetic reaction is slow, needs to construct efficient stable
α-Fe2O3Base composite photocatalyst.The present invention provides a kind of α-Fe for degradable organic pollutant2O3/ Fe nanocomposite
Photochemical catalyst, the ability with good photocatalytic degradation of organic matter.α-Fe2O3/ Fe photochemical catalyst is nanometer chip architecture, compares table
Area is 60~150m2/ g, nanometer sheet diameter is 50~300nm, with a thickness of 2~8nm, wherein α-Fe2O3It is selected along (110) direction
Tachyauxesis, α-Fe2O3Mass ratio with Fe is 1: 0.5~1: 1.5.
A kind of α-Fe for degradable organic pollutant provided by the present invention2O3/ Fe nano composite material photocatalyst
Preparation method the following steps are included:
1) Fe nanometer sheet is prepared using oxidation-reduction method；
1.1) soluble ferrite aqueous solution and alcoholic solvent are uniformly mixed to get mixed solution I, the solubility is sub-
Molysite aqueous solution concentration is 0.01~0.05mol/L, and alcoholic solvent is one or more of ethyl alcohol, ethylene glycol, glycerine, volume
For 300~500mL/L.
1.2) organic salt is added in mixed solution I and obtains mixed solution I I, the organic salt is sodium acetate, methyl
One or more of sodium, four butylamine of bromination, the mass concentration of addition are 2~6g/L.
1.3) boron hydrogen salt aqueous solution is added rapidly to obtain suspension solution III in mixed solution I I, the boron hydrogen salt
The concentration of water aqueous solution is 0.05~0.4mol/L, and boron hydrogen salt used is one or both of potassium borohydride, sodium borohydride.
The above experimentation carries out in water-bath, and bath temperature is 30~55 DEG C, and keeps mechanical stirring.
1.4) precipitation and separation in suspension III, resulting precipitating dehydrated alcohol and deionized water are rinsed respectively, from
Heart separation, and keep the temperature in a vacuum drying oven, Fe nanometer sheet is obtained, the temperature of the vacuum oven is 40~80 DEG C, is protected
The warm time is 10~30h.
2) the Fe nanometer sheet that step 1) obtains is annealed under air atmosphere, annealing temperature is 300~600 DEG C, when annealing
Between be 2~120min, obtain α-Fe2O3/ Fe nanosheet photocatalyst.
Utilize the α-Fe2O3The method of/Fe nanosheet photocatalyst progress organic pollutant degradation are as follows: to be processed
Prepared α-Fe is added in organic wastewater2O3/ Fe photochemical catalyst (additional amount is 0.1~10g/L), it is mechanical under dark condition
Stirring a period of time to reach absorption/desorption equilibrium, then utilizes visible light exposure and continues to stir, after stabilized intensity, to
H is added in solution2O2(additional amount is 10~70mL/L), continuous light can be by the organic matter removal in waste water to be processed.
With it is existing for the catalyst of degradable organic pollutant compared with, the invention has the following advantages that
(1) present invention is utilizing α-Fe2O3On the basis of photocatalysis performance, photochemical catalyst and H are also used2O2Between
Fenton meal is answered, and is generated the hydroxyl radical free radical (OH) with strong oxidizing property, is promoted the degradation of organic pollutant；With pure α-
Fe2O3Nanometer sheet is compared, α-Fe2O3/ Fe composite material has the Fe ion (0 valence and+trivalent) of different valence state simultaneously, hence it is evident that enhancing
Fenton effect, greatly improves degradation rate；
(2) with pure α-Fe2O3Nanometer sheet is compared, and the present invention utilizes α-Fe2O3Interfacial contact effect between Fe is formed
Space-charge region, improves the separating capacity of photo-generated carrier, to improve the stability of photocatalysis efficiency and photochemical catalyst；
(3) α-Fe that the present invention obtains2O3/ Fe photochemical catalyst is nano-sheet, when considerably increasing reaction and organic contamination
The contact area and active site quantity of object, improve degradation rate；
(4) driving force of catalyst degradation organic matter according to the present invention is illumination, and degradation speed is fast, does not need other
Extra power consumption is a kind of efficient, energy-saving and environmental protection organic matter degradation process；
(5) catalyst according to the present invention is versatile, has to the organic waste Organic substance in water within the scope of larger pH
Good degradation effect.
Detailed description of the invention
α-Fe prepared by Fig. 1 embodiment 12O3The transmission electron microscope photo of/Fe nanosheet photocatalyst；
The rhodamine B degradation curve of Fig. 2 embodiment 1；
The rhodamine B degradation curve of Fig. 3 embodiment 2；
Specific embodiment
The present invention is further explained in the light of specific embodiments, but the present invention is not limited by following embodiment.
Embodiment 1:
Prepare α-Fe2O3The step of/Fe nano composite photo-catalyst:
1) Fe nanometer sheet is prepared using oxidation-reduction method:
1.1) by the FeSO of 50mL4·7H2O (5mmol) aqueous solution and 40mL ethylene glycol are uniformly mixed to get mixed solution I；
1.2) sodium methide of 0.5g is added in mixed solution I and obtains mixed solution I I；
1.3) it is added rapidly to the potassium borohydride of 30mL (0.04mol) aqueous solution to obtain suspension solution in mixed solution I I
III；
The above experimentation carries out in water-bath, and keeps mechanical stirring, and bath temperature is 40 DEG C；
1.4) precipitation and separation in suspension III, resulting precipitating dehydrated alcohol and deionized water are rinsed respectively, from
Heart separation, and kept the temperature for 24 hours in 50 DEG C of vacuum ovens, obtain Fe nanometer sheet；
2) the Fe nanometer sheet that step 1) obtains is annealed under air atmosphere, obtains α-Fe2O3@Fe nanosheet photocatalyst,
The annealing temperature is 450 DEG C, annealing time 8min；
α-the Fe being prepared2O3The micro-structure of/Fe is characterized using transmission electron microscope, as a result as specification is attached
Shown in Fig. 1.It can see α-Fe2O3/ Fe is flake, and the diameter of thin slice is about 200nm, and thickness is about 3nm.
Use α-Fe2O3/ Fe photochemical catalyst degrades to organic pollutant rhodamine B, the method used are as follows:
Radiation source is the 300W xenon lamp with the following edge filter of 400nm wavelength, power 100mW/cm2(1 mould
The quasi- sun).
To the α-Fe that 50mg preparation is added in 100mL rhodamine B solution (concentration 10mg/L)2O3/ Fe photochemical catalyst,
Under dark condition then the double-deck beaker is moved under visible light to reach absorption/desorption equilibrium and irradiates and continue by mechanical stirring 1h
The H of 3mL is added into rhodamine B solution after stabilized intensity for stirring2O2, 30min is stirred, every 10min draws 3mL with dropper
Dispersing liquid and centrifugation, take its supernatant, in characteristic wavelength be using ultraviolet/visible spectrophotometer test rhodamine B
The absorption value of 550nm, the variation of the reacting condition rhodamine B concentration of this absorption value, thus living to measure the photocatalysis of catalyst
Property.
Resulting α-the Fe of embodiment 12O3/ Fe photochemical catalyst is to the degradation curve of rhodamine B as shown in Figure of description 2.It can
To see that at illumination 10 minutes, the degradation rate of rhodamine B reached 92%, shows very high degradation rate.
Embodiment 2:
Prepare α-Fe2O3The step of/Fe nano composite photo-catalyst:
1) Fe nanometer sheet is prepared using oxidation-reduction method:
1.1) by the FeSO of 100mL4·7H2O (0.01mol) aqueous solution and the glycerine of 50mL ethylene glycol and 50mL are uniform
It is mixed to get mixed solution I；
1.2) sodium acetate of 1g is added in mixed solution I and obtains mixed solution I I；
1.3) it is added rapidly to the sodium borohydride of 50mL (0.05mol) aqueous solution to obtain suspension solution in mixed solution I I
III；
The above experimentation carries out in water-bath, and keeps mechanical stirring, and bath temperature is 35 DEG C；
1.4) precipitation and separation in suspension III, resulting precipitating dehydrated alcohol and deionized water are rinsed respectively, from
Heart separation, and 18h is kept the temperature in 40 DEG C of vacuum ovens, obtain Fe nanometer sheet；
2) the Fe nanometer sheet that step 1) obtains is annealed under air atmosphere, obtains α-Fe2O3/ Fe nanosheet photocatalyst,
The annealing temperature is 500 DEG C, annealing time 5min；
Use α-Fe2O3/ Fe photochemical catalyst degrades to organic pollutant rhodamine B, the method used are as follows:
Radiation source is the 300W xenon lamp with the following edge filter of 400nm wavelength, power 100mW/cm2(1 mould
The quasi- sun).
To the α-Fe that 50mg preparation is added in 50mL rhodamine B solution (concentration 10mg/L)2O3@Fe photochemical catalyst, black
Under dark condition then the double-deck beaker is moved to reach absorption/desorption equilibrium and irradiates under visible light and persistently stir by mechanical stirring 1h
It mixes, after stabilized intensity, the H of 7mL is added into rhodamine B solution2O2, 1h is stirred, every 10min draws the dispersion of 3mL with dropper
Liquid is simultaneously centrifuged, and takes its supernatant, using ultraviolet/visible spectrophotometer test rhodamine B in the suction that characteristic wavelength is 550nm
Receipts value, the variation of the reacting condition rhodamine B concentration of this absorption value, thus to measure the photocatalytic activity of catalyst.
Resulting α-the Fe of embodiment 22O3/ Fe photochemical catalyst is to the degradation curve of rhodamine B as shown in Figure of description 3.It can
When seeing illumination 10 minutes, when the degradation rate of rhodamine B reaches 85%, illumination 30 minutes, degradation rate reaches 96%, shows
Very high degradation rate.
It is described above sufficiently to have illustrated the photochemical catalyst preparation and application involved in the present invention arrived, it should be pointed that
, to those of ordinary skill in the art, can be in the case where not departing from claims of the present invention range
Some modifications and polishing are made, these modifications and polishing also belong to the scope of the present invention.
Claims (9)
1. a kind of α-Fe for degradable organic pollutant2O3/ Fe nano composite material photocatalyst, it is characterised in that described
α-Fe2O3/ Fe photochemical catalyst is nanometer chip architecture, and nanometer sheet diameter is 50~300nm, with a thickness of 2~8nm, specific surface area 60
~150m2/g。
2. α-Fe as described in claim 12O3/ Fe nano composite material photocatalyst, it is characterised in that the α-Fe2O3Edge
(110) direction preferential growth, α-Fe2O3Mass ratio with Fe is 1: 0.5~1: 1.5.
3. α-Fe as described in claim 12O3/ Fe nano composite material photocatalyst, it is characterised in that the photochemical catalyst
Preparation method the following steps are included:
3.1) Fe nanometer sheet is prepared using oxidation-reduction method；
3.1.1 soluble ferrite aqueous solution and alcoholic solvent uniformly) are mixed to get mixed solution I；
3.1.2) organic salt is added in mixed solution I and obtains mixed solution I I；
3.1.3 it) is added rapidly to boron hydrogen salt aqueous solution to obtain suspension solution III in mixed solution I I；
3.1.4 the precipitation and separation in suspension III, resulting precipitating dehydrated alcohol and deionized water are rinsed respectively), are centrifuged
Separation, and keep the temperature in a vacuum drying oven, obtain Fe nanometer sheet；
3.2) the Fe nanometer sheet that step 3.1) obtains is annealed under air atmosphere, obtains α-Fe2O3/ Fe nanocomposite light
Catalyst.
4. α-Fe as claimed in claim 32O3/ Fe nano composite material photocatalyst preparation method, it is characterised in that described
Preparation step 3.1.1) soluble ferrite concentration of aqueous solution be 0.01~0.05mol/L, alcoholic solvent be ethyl alcohol, ethylene glycol,
One or more of glycerine, volume are 300~500mL/L.
5. α-Fe as claimed in claim 32O3/ Fe nano composite material photocatalyst preparation method, it is characterised in that described
Preparation step 3.1.2) organic salt be one or more of sodium acetate, sodium methide, four butylamine of bromination, mass concentration be 2~
6g/L。
6. α-Fe as claimed in claim 32O3/ Fe nano composite material photocatalyst preparation method, it is characterised in that described
Preparation step 3.1.3) boron hydrogen salt aqueous solution concentration be 0.05~0.4mol/L, boron hydrogen salt used be potassium borohydride, boron
One or both of sodium hydride.
7. α-Fe as claimed in claim 32O3/ Fe nano composite material photocatalyst preparation method, it is characterised in that described
Preparation step 3.1.1), 3.1.2), 3.1.3) reaction temperature be 30~55 DEG C, whole process keep mechanical stirring.
8. α-Fe as claimed in claim 32O3/ Fe nano composite material photocatalyst preparation method, it is characterised in that described
Preparation step 3.1.4) vacuum oven temperature be 40~80 DEG C, keep the temperature 10~30h.
9. α-Fe as claimed in claim 32O3/ Fe nano composite material photocatalyst preparation method, it is characterised in that described
Preparation step 3.2) annealing temperature be 300~600 DEG C, annealing time be 2~120min.
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