CN106268830A - A kind of Fe2o3/ ZnFe2o4composite photo-catalyst and its preparation method and application - Google Patents

A kind of Fe2o3/ ZnFe2o4composite photo-catalyst and its preparation method and application Download PDF

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CN106268830A
CN106268830A CN201610644343.0A CN201610644343A CN106268830A CN 106268830 A CN106268830 A CN 106268830A CN 201610644343 A CN201610644343 A CN 201610644343A CN 106268830 A CN106268830 A CN 106268830A
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znfe
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CN106268830B (en
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李永庆
田丽
孔令茹
韩晓鹏
吕佳男
范晓星
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Liaoning University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts 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
    • B01J23/80Catalysts 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 zinc, cadmium or mercury
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/33Electric or magnetic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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Abstract

The present invention proposes a kind of Fe2O3/ZnFe2O4Composite photo-catalyst and its preparation method and application.First with ferric nitrate as raw material, hydro-thermal method is utilized to prepare the Fe of appearance rule2O3Ball, then with ferric nitrate and ZnCl2For raw material, hydro-thermal method is utilized to prepare mesoporous ZnFe2O4Nano material.Last at Fe2O3By the method for calcining on the basis of ball, prepare Fe further2O3With ZnFe2O4Composite semiconductor.This composite photo-catalyst efficiently separates electron hole pair, reduces recombination rate, can effectively improve photocatalytic activity, the method low cost, operation simple, convenient.Utilize its isopropanol of degrading under visible light illumination.

Description

A kind of Fe2O3/ZnFe2O4Composite photo-catalyst and its preparation method and application
Technical field
The invention belongs to catalysis material technical field, be specifically related to a kind of Fe2O3/ZnFe2O4Composite photo-catalyst and Its preparation method and application.
Background technology
Photocatalysis technology is a kind of environmentally friendly technology, and catalysis material can utilize sunlight hydrogen production by water decomposition to obtain Regenerative resource, additionally can apply to the depollution of environment, solves energy and environmental problem that human development is faced.Titanium dioxide Titanium, as a kind of semiconductor light-catalyst, has nontoxic, cheap, the advantage of non-secondary pollution, and it divides at environmental pollution degraded, light Solve the fields such as water hydrogen manufacturing to have wide practical use.
ZnFe2O4It is a kind of stable spinel, there is relatively small band gap and stable photochemical properties, The fields such as the anode material of pigment, magnetic material, photochemical breakdown water hydrogen manufacturing and lithium ion battery suffer from being widely applied, and And ZnFe2O4Or the high efficiency photocatalyst of Visible Light Induced Photocatalytic organic pollution.Existing advantage improves it the most further Photocatalysis efficiency becomes the emphasis of people's research.
Summary of the invention
It is an object of the invention to provide a kind of Fe2O3/ZnFe2O4The preparation method of composite photo-catalyst, this preparation method letter List, convenience, low cost, mild condition, the most extensive preparation.
The technical solution used in the present invention is: a kind of Fe2O3/ZnFe2O4Composite photo-catalyst, preparation method includes as follows Step:
1)Fe2O3Prepared by ball: add ferric nitrate in dimethyl formamide solution, under magnetic agitation, add acid-conditioning solution PH value is 2-3, continue stirring, gained solution is put in Muffle furnace, at 100-150 DEG C react 10-15h, product by centrifugation, Clean, drying obtains Fe2O3Ball;
2)ZnFe2O4Preparation: by ferric nitrate deionized water dissolving, add ZnCl2Stirring, to dissolving, adds NaOH Stirring is to dissolving;Gained solution is put in Muffle furnace, at 150-200 DEG C, reacts 15-20h, product by centrifugation, clean, dry Dry obtain ZnFe2O4
3)Fe2O3/ZnFe2O4Composite photo-catalyst: by Fe2O3Ball and ZnFe2O4After mixing, add organic solvent and surpass Sound disperses, and dries, the pressed powder obtained is put roasting in a vacuum furnace, obtains Fe at 65-75 DEG C2O3/ZnFe2O4Compound Photocatalyst.
Above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst, the concentration expressed in percentage by volume of described dimethyl formamide solution is 60-70%.
Above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst, described acid is nitric acid.
Above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst, step 2) in, in molar ratio, ferric nitrate: ZnCl2=1.5- 2.5:1。
Above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst, step 3) in, in molar ratio, Fe2O3Ball: ZnFe2O4=1:1.
Above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst, step 3) in, described organic solvent is ethanol or methanol.
Above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst, step 3) in, in vacuum drying oven, at temperature is 180-200 DEG C, Roasting 2-3h.
Above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst application in degradable organic pollutant.Method is as follows: can Under seeing that light irradiates, in the container containing organic pollution, add above-mentioned Fe2O3/ZnFe2O4Composite photo-catalyst, can be by Organic substance is degraded.
The method have the advantages that
Fe2O3It is a kind of non-metal N type quasiconductor, owing to it has good chemical stability, thermal stability and light Electrical characteristics and get more and more people's extensive concerning, its energy gap is 2.1eV, can with absorbing wavelength less than the visible ray of 600nm, but Being that its photo-generate electron-hole is easily combined, quantum efficiency is low.In order to widen Fe2O3Spectral response range, the present invention is by Fe2O3With ZnFe with its level-density parameter2O4It is combined mutually, utilizes the energy level difference between two kinds of quasiconductors that photo-generated carrier can be made partly to be led by one The energy level of body microgranule is injected on the energy level of another kind of quasiconductor, makes photo-generate electron-hole efficiently separate, improves two kinds of quasiconductors Photo-quantum efficiency.
Fe2O3And ZnFe2O4Light produces electronics and hole, ZnFe after irradiating2O4The electronics produced is injected into Fe2O3's Conduction band, and Fe2O3Valence band in hole be injected into ZnFe2O4Valence band, thus promote light induced electron and separate with hole, Improve photocatalysis effect.In addition to this it is possible to utilize ZnFe2O4Magnetomechanical effects carry out effective recycling, permissible It is applied to large-scale production.
Accompanying drawing explanation
Fig. 1 is the Fe obtained in embodiment 12O3The XRD figure of ball.
Fig. 2 is the ZnFe obtained in embodiment 12O4XRD figure.
Fig. 3 is the Fe obtained in embodiment 12O3/ZnFe2O4The XRD figure of composite photo-catalyst.
Fig. 4 is the Fe obtained in embodiment 12O3The SEM figure of ball.
Fig. 5 is the ZnFe obtained in embodiment 12O4SEM figure.
Fig. 6 is the Fe obtained in embodiment 12O3/ZnFe2O4The SEM figure of composite photo-catalyst.
Fig. 7 is Fe2O3、ZnFe2O4And Fe2O3/ZnFe2O4Composite photo-catalyst is in the work of photocatalytic degradation isopropanol gas Property comparison diagram.
Detailed description of the invention
Embodiment 1 Fe2O3/ZnFe2O4Composite photo-catalyst
(1) Fe2O3The preparation of ball:
1) measure 10ml deionized water and 20ml dimethylformamide respectively, pour the 50ml beaker with magnetic rotor into In, magnetic agitation 20min is uniformly dissolved to solution, obtains dimethyl formamide solution.
2) in dimethyl formamide solution, 5g nine water ferric nitrate, magnetic agitation 30min are added.Then, in solution by Being added dropwise to salpeter solution, the pH value of regulation solution is to 2, then magnetic agitation 30min.
3) by step 2) solution that obtains pours in 50ml water heating kettle, and in the Muffle furnace of 120 DEG C, pyroreaction 10h (rises Temperature speed is 3 DEG C/min).
4) after hydro-thermal reaction completes, centrifugal, clean 3 times with deionized water, dry in the baking oven of 70 DEG C, after being dried Grind the Fe obtaining appearance rule2O3Ball.
The Fe that will obtain2O3Ball carries out XRD test, result as it is shown in figure 1, as can be seen from the figure sample have preferably Degree of crystallinity;Again by Fe2O3Ball carries out SEM test, and as shown in Figure 4, as can be seen from the figure sample is spherical to result.
(2) ZnFe2O4Preparation:
1) being added in 30ml deionized water solution by the nine water ferric nitrates of 4.04g (0.01mol), magnetic agitation 30min is extremely It is uniformly dissolved.
2) to step 1) solution that obtains adds 0.68g (0.005mol) ZnCl2, magnetic agitation to being uniformly dissolved, then Adding 4.40g (0.110mol) NaOH, magnetic agitation is to being uniformly dissolved, and stirring 2h is until solution dissolves the most energetically Even.
3) by step 2) solution that obtains transfers to, in 50ml reactor, put in Muffle furnace, reacts 17 little at 180 DEG C Time (heating rate is 3 DEG C/min).
4) after hydro-thermal reaction completes, centrifugal, clean 3 times with deionized water, dry in the baking oven of 70 DEG C, after being dried Grinding obtains mesoporous ZnFe2O4
The sample ZnFe that will obtain2O4Carry out XRD test, result as in figure 2 it is shown, as can be seen from the figure sample have relatively Good degree of crystallinity;The sample ZnFe that will obtain2O4Carry out SEM test, result as it is shown in figure 5, as seen from Figure 5 sample be mesoporous, Granular size, the most well-regulated pattern.
(3) Fe2O3/ZnFe2O4The preparation of composite photo-catalyst
1) 1:1 in molar ratio, takes step 1) Fe for preparing2O3Ball and step 2) ZnFe for preparing2O4, join with turning In the beaker of son, add ethanol solution and carry out ultrasonic disperse about 120min.
2) Fe is treated2O3Ball and ZnFe2O4After being completely dispersed, transfer in culture dish, dry in 70 DEG C of baking ovens.
3) by step 2) pressed powder that obtains is at the vacuum kiln roasting 2h (5 DEG C/min of heating rate) of 200 DEG C.Finally Obtain Fe2O3/ZnFe2O4Composite photo-catalyst.
Sample F e that will obtain2O3/ZnFe2O4Composite photo-catalyst carries out XRD test, and result is as it is shown on figure 3, from figure Can be seen that sample has preferable degree of crystallinity.Sample F e that will obtain2O3/ZnFe2O4Composite photo-catalyst carries out SEM test, Result as shown in Figure 6, as can be seen from the figure Fe2O3And ZnFe2O4It is combined together.
Embodiment 2 Fe2O3/ZnFe2O4The application of composite photo-catalyst
The Fe respectively prepared by embodiment 12O3Ball, ZnFe2O4And Fe2O3/ZnFe2O4Composite photo-catalyst carries out photocatalysis Agent material performance test.
Test process is: Fe embodiment 1 prepared respectively2O3Ball, ZnFe2O4And Fe2O3/ZnFe2O4Composite photo-catalyst It is put in different 4cm2In glass guide channel, the glass guide channel of photocatalyst-bearing is respectively put into and includes an atmospheric air In 224ml reactor, with 300W xenon lamp as light source, photoelectric current is adjusted to 20mA position, and regulation light strong center is just being irradiated to sample Surface, fixes position, injects 10ul isopropanol liquid, after illumination 30min, extract the first pin in the most backward reactor, this Sample extracted a pin every 30 minutes, tested, and the peak area of record isopropanol, result is as shown in Figure 7.
As it is shown in fig. 7, as can be seen from the figure within 150min, Fe2O3Degrade the isopropanol gas of 50%, ZnFe2O4Degrade the isopropanol gas of 60%, Fe2O3/ZnFe2O4The composite photocatalyst for degrading isopropanol gas of 80%, It will thus be seen that Fe2O3/ZnFe2O4The photocatalytic activity of composite photo-catalyst compares Fe2O3And ZnFe2O4Want height.

Claims (10)

1. a Fe2O3/ZnFe2O4Composite photo-catalyst, it is characterised in that preparation method comprises the steps:
1)Fe2O3The preparation of ball: add ferric nitrate in dimethyl formamide solution, under magnetic agitation, add the pH of acid-conditioning solution Value is 2-3, continues stirring, puts in Muffle furnace by gained solution, reacts 10-15h at 100-150 DEG C, and product is by centrifugation, clearly Wash, dry and obtain Fe2O3Ball;
2)ZnFe2O4Preparation: by ferric nitrate deionized water dissolving, add ZnCl2Stirring, to dissolving, adds NaOH stirring To dissolving;Gained solution is put in Muffle furnace, at 150-200 DEG C, reacts 15-20h, product by centrifugation, clean, dry To ZnFe2O4
3)Fe2O3/ZnFe2O4Composite photo-catalyst: by Fe2O3Ball and ZnFe2O4After mixing, add organic solvent and carry out ultrasonic point Dissipate, dry at 65-75 DEG C, the pressed powder obtained is put roasting in a vacuum furnace, obtains Fe2O3/ZnFe2O4Complex light is urged Agent.
Fe the most according to claim 12O3/ZnFe2O4Composite photo-catalyst, it is characterised in that dimethyl formamide solution Concentration expressed in percentage by volume 60-70%.
Fe the most according to claim 12O3/ZnFe2O4Composite photo-catalyst, it is characterised in that described acid is nitric acid.
Fe the most according to claim 12O3/ZnFe2O4Composite photo-catalyst, it is characterised in that step 2) in, by mole Ratio, ferric nitrate: ZnCl2=1.5-2.5:1.
Fe the most according to claim 12O3/ZnFe2O4Composite photo-catalyst, it is characterised in that step 3) in, by mole Ratio, Fe2O3Ball: ZnFe2O4=1:1.
Fe the most according to claim 12O3/ZnFe2O4Composite photo-catalyst, it is characterised in that step 3) in, described has Machine solvent is ethanol or methanol.
Fe the most according to claim 12O3/ZnFe2O4Composite photo-catalyst, it is characterised in that step 3) in, in vacuum drying oven In, at temperature is 180-200 DEG C, roasting 2-3h.
8. the Fe described in claim 12O3/ZnFe2O4Composite photo-catalyst application in degradable organic pollutant.
Application the most according to claim 8, it is characterised in that method is as follows: under visible light illumination, to containing organic dirt The container of dye thing adds the Fe described in claim 12O3/ZnFe2O4Composite photo-catalyst, degrades.
Application the most according to claim 9, it is characterised in that described organic pollution is isopropanol.
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CN107185577A (en) * 2017-06-04 2017-09-22 吉林化工学院 Preparation method with visible light-responded heterogeneous Fenton zinc ferrite photocatalysis composite
CN112642430A (en) * 2019-10-11 2021-04-13 中国石油天然气股份有限公司 Preparation method of microspherical catalyst for preparing butadiene through oxidative dehydrogenation of butene
CN112934233A (en) * 2021-01-06 2021-06-11 天津理工大学 Composite photocatalyst and preparation method and application thereof

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CN112642430A (en) * 2019-10-11 2021-04-13 中国石油天然气股份有限公司 Preparation method of microspherical catalyst for preparing butadiene through oxidative dehydrogenation of butene
CN112934233A (en) * 2021-01-06 2021-06-11 天津理工大学 Composite photocatalyst and preparation method and application thereof

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