CN102350353A - Preparation method of Fe3O4/C/TiO2 composite photocatalyst - Google Patents

Preparation method of Fe3O4/C/TiO2 composite photocatalyst Download PDF

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CN102350353A
CN102350353A CN2011102447660A CN201110244766A CN102350353A CN 102350353 A CN102350353 A CN 102350353A CN 2011102447660 A CN2011102447660 A CN 2011102447660A CN 201110244766 A CN201110244766 A CN 201110244766A CN 102350353 A CN102350353 A CN 102350353A
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张青红
石福志
王宏志
李耀刚
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Donghua University
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Donghua University
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Abstract

The invention relates to a preparation method of an Fe3O4/C/TiO2 composite photocatalyst, which comprises the following steps: (1) dissolving titanium alkoxide in absolute lower alcohol to prepare a titanium alkoxide absolute alcohol solution; (2) adding Fe3O4/C nano powder into the titanium alkoxide absolute alcohol solution, carrying out ultrasonic dispersion and stirring to obtain a uniform mixture; and (3) putting the mixture into a closed container which previously contains distilled water (the mixture does not directly contact the distilled water), heating to 70-200 DEG C, keeping the temperature for 1-96 hours, cooling to room temperature, washing the powder and drying to obtain the Fe3O4/C/TiO2 composite photocatalyst. The preparation method provided by the invention is simple, and has the advantage of lower cost; and the composite photocatalyst maintains the characteristic of high catalytic activity of titanium dioxide nano crystal grains, and can be magnetically recycled, thereby providing a solution for separating and recycling nano crystal titanium dioxide.

Description

A kind of Fe 3O 4/ C/TiO 2The preparation method of composite photo-catalyst
Technical field
The invention belongs to TiO 2The preparation field of composite photo-catalyst, particularly a kind of Fe 3O 4/ C/TiO 2The preparation method of composite photo-catalyst.
Background technology
Nano titanium oxide is a kind of common photochemical catalyst, and because of its chemical stability is good, oxidation activity is high, and to the human non-toxic evil, cost is low, applied range and getting more and more people's extensive concerning.But the principal element that the restriction nano titanium oxide is used in sewage disposal has two: the one, and the titanium dioxide that catalytic activity is high, oxidability is strong often needs ultraviolet excitation; The 2nd, the nano-crystalline photocatalysis agent is active high, but cost recovery is high.The photochemical catalyst of film and multilevel hierarchy can solve its problem that reclaims difficulty, but photocatalysis efficiency is not high.Film normally is fixed on photochemical catalysts such as nano titanium oxide through physics or chemical method on the inert carriers such as glass, but this type photochemical catalyst solid-liquid contact area is little, causes its photocatalytic activity not high.The titanium dioxide nanoparticle size of multilevel hierarchy is often greater than 10 μ m, because the surface is to scattering of light and absorption, granule interior is the zone that light is difficult to shine, and it is caught optical efficiency and has much room for improvement.At present, have the further research of still needing of high activity and the photochemical catalyst that be prone to reclaim characteristic concurrently.
Recently, people introduce magnetic material in the photochemical catalyst, have prepared the magnetic photocatalyst of core/shell structure.So both keep nanocrystalline high photocatalytic activity, and utilized magnetic nuclear to be easy to the characteristics that realize that Magnetic Isolation reclaims again.Xuan etc. (J.Phys.Chem.C, 2009,113,553.) are that template has prepared Fe to gather (styrene-propene acid) 3O 4/ TiO 2Tiny balloon, in the experiment of light degradation rhodamine B, shown good light degradation and magnetic recyclability.Because TiO 2Photoetch effect meeting is examined Fe to magnetic 3O 4Cause damage (J.Phys.Chem.B, 2000,104,4387.), be unfavorable for the permanent application of magnetic photocatalyst.Song etc. (J.Am.Ceram.Soc., 2007,90,4015.) adopt sol-gel process with magnetic Fe 3O 4For magnetic is examined the photochemical catalyst that has prepared core/shell structure,, between titanium dioxide optical catalyst and magnetic nuclear, coated one deck SiO in order to prevent the photoetch of magnetic nuclear 2
Summary of the invention
Technical problem to be solved by this invention provides a kind of Fe 3O 4/ C/TiO 2The preparation method of composite photo-catalyst, this method is simple, and cost is relatively low, less demanding to equipment; The composite photo-catalyst that obtains had both kept the characteristics of titanium dioxide nanocrystalline grain high catalytic activity; In most light-catalyzed reactions, has the similar photocatalytic activity of nano titanium oxide with the vapor phase method preparation; But had the advantage of magnetic recovery again concurrently; Separation and Recovery for nano-crystalline titanium dioxide provides solution route.
A kind of Fe of the present invention 3O 4/ C/TiO 2The preparation method of composite photo-catalyst comprises:
(1) the titanium alkoxide is dissolved in the anhydrous lower alcohol, processing concentration is the titanium alkoxide anhydrous alcohol solution of 0.001～0.12mL/mL;
(2) with Fe 3O 4/ C nano-powder adds in the above-mentioned titanium alkoxide anhydrous alcohol solution, through ultrasonic dispersion and stirring, obtains uniform mixture, wherein Fe 3O 4The concentration of/C is 0.5～100.0mg/mL;
(3) said mixture is put into the closed container that fills distilled water in advance, said mixture does not directly contact with distilled water, is heated to 70～200 ℃ then, is incubated 1～96 hour, and cool to room temperature with the washing of gained powder, drying, promptly gets Fe at last again 3O 4/ C/TiO 2Composite photo-catalyst.
Titanium alkoxide in the said step (1) is one or more in tetraethyl titanate, tetraisopropyl titanate, the butyl titanate.
Lower alcohol in the said step (1) is one or more in methyl alcohol, ethanol, normal propyl alcohol, the isopropyl alcohol.
Fe in the said step (2) 3O 4/ C nano-powder is through with Fe 3O 4Microballoon obtains after magnetic field recovery, washing, alcohol are washed, dried after carbon is modified again.
Above-mentioned Fe 3O 4Microballoon is for what prepare through solvent thermal process, and concrete operation method is: with 1.35gFeCl 36H 2O, 3.6g anhydrous sodium acetate, 1g polyethylene glycol, 0.5g polyvinylpyrrolidone join in the 50mL ethylene glycol solution, through ultrasonic, stir after, place agitated reactor, after 10 hours, promptly get Fe 200 ℃ of reactions 3O 4Microballoon.
The ratio of the amount of substance of titanium elements is 20～3000 in distilled water in the said step (3) and the titanium alkoxide.
The Fe that obtains in the said step (3) 3O 4/ C/TiO 2Composite photo-catalyst is a core/shell structure, and its center is Fe 3O 4Microballoon, transition zone are the C layer, and shell is that the good anatase titania of crystallinity is nanocrystalline, and crystallite dimension is 5～20nm.
Existing relevant technological parameter to reaction is done some concrete qualifications:
(1) consumption of water: water does not directly contact with the titanium alkoxide in the bottom of closed container, water start vaporizer during heating, and finally make the whole hydrolysis of titanium alkoxide.In the reaction of reality, the ratio of the amount of substance of water and titanium is between 20 to 3000.
(2) Fe 3O 4The concentration of/C: Fe 3O 4The concentration of/C in alcoholic solution is between 0.5mg/mL～100.0mg/mL.
(3) concentration of titanium alkoxide: the concentration of titanium alkoxide in lower alcohol can change the thickness of anatase titania clad through the concentration that changes the titanium alkoxide in the scope of 0.001mL/mL～0.120mL/mL.
The thickness of anatase titania clad is that (0.010mL～1.500mL) determine, the amount difference according to the titanium alkoxide can form the titanium dioxide layer of several nanometers to hundreds of nanometer thickness by the amount of titanium alkoxide adding.
The present invention mainly provides a kind of Fe of core/shell structure 3O 4/ C/TiO 2But the preparation method of magnetic recovery composite photo-catalyst, but all can be prepared into the magnetic recovery composite photo-catalyst of core/shell structure in this way for the magnetic matrix of different size and magnetic nuclear.The composite photo-catalyst that the present invention prepares had both kept the characteristics of titanium dioxide nanocrystalline grain high catalytic activity; In most light-catalyzed reactions, has the similar photocatalytic activity of nano titanium oxide with the vapor phase method preparation; But had the advantage of magnetic recovery again concurrently; Separation and Recovery for nano-crystalline titanium dioxide provides solution route.
A kind of Fe of the present invention 3O 4/ C/TiO 2The preparation method of composite photo-catalyst utilizes Fe 3O 4/ C microballoon is a carrier, promotes the titanium hydrolysis of alkoxide through steam, at Fe 3O 4/ C microsphere surface forms the anatase phase titanium dioxide layer.This composite photo-catalyst has nucleocapsid structure, examines to be Fe 3O 4Microballoon, transition zone are the C layer, and shell is a crystalline titania, can improve the recovery characteristic of titanium dioxide with photocatalyst.
Beneficial effect
(1) preparation method of the present invention is simple, and cost is relatively low, and less demanding to equipment is produced on a large scale;
(2) magnetic photocatalyst of the present invention has kept the high characteristics of titanium dioxide nanocrystalline grain photocatalytic activity, and shell titanium dioxide is the anatase phase, and its crystal grain is 5～20nm, and is relevant with the vapor phase treatment temperature;
(3) the prepared magnetic photocatalyst of the present invention has been kept the magnetic property of its nuclear, and it can be reclaimed through magnetic field.
Description of drawings
The Fe that Fig. 1 (a) prepares for solvent-thermal method 3O 4The transmission electron microscope photo of particle (b) is the prepared Fe of instance 1 3O 4/ C/TiO 2The transmission electron microscope photo of composite photo-catalyst; (c) the high resolution electron microscopy photo of institute's favored area among Fig. 1 (b); Can significantly observe the lattice fringe of anatase titania among the figure; Show that titanium dioxide has good degree of crystallinity, the spacing of lattice of anatase (101) face is 0.35nm, and the grain size of anatase titania is about 10nm; (d) the power spectrum result of institute's favored area among Fig. 1 (b);
Fig. 2 is Fe 3O 4Particle, Fe 3O 4The Fe that/C microballoon and instance 1 are prepared 3O 4/ C/TiO 2But the hysteresis curve figure of composite photo-catalyst and the magnetic recovery photo of magnetic photocatalyst;
Fig. 3 is the prepared Fe of instance 1 3O 4/ C/TiO 2The efficiency chart of composite photo-catalyst light degradation methylene blue and its long-acting cycle efficieny figure;
Fig. 4 is the Fe of solvent thermal process preparation 3O 4The Fe that particle and instance 2 are prepared 3O 4/ C/TiO 2The X-ray diffraction result of composite photo-catalyst.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The 0.20mL butyl titanate is joined in the 8mL absolute ethyl alcohol, stirred 2 minutes, the Fe that 0.1g is prepared in advance 3O 4/ C microballoon adds in the lower alcohol, ultrasonic dispersion and stirring each 3 minutes.To contain Fe 3O 4The anhydrous alcohol solution of/C microballoon is poured in the crucible, places the top of sealable container then.Sealable container bottom is placed with 3mL distilled water in advance.With container airtight after, put into baking oven, begin to be heated to 150 ℃, heating rate is 10～20 ℃/minute, temperature reached after the temperature of setting insulation 10 hours.After insulation finishes, naturally cool to room temperature, open closed container, take out crucible, pour out powder, respectively wash 3 times, through 60 ℃ of vacuum dryings 8 hours with distilled water and absolute alcohol.
Fig. 1 (a) has provided the Fe that solvent-thermal method prepares 3O 4The transmission electron microscope photo of particle, (b) Fe 3O 4/ C/TiO 2The transmission electron microscope photo of composite photo-catalyst, (c) the high resolution electron microscopy photo of institute's favored area among Fig. 1 (b).Can significantly observe the lattice fringe of anatase titania among the figure, show that titanium dioxide has good degree of crystallinity, the spacing of lattice of anatase (101) face is 0.35nm, and the grain size of anatase titania is about 10nm.(d) the power spectrum result of institute's favored area among Fig. 1 (b).
Embodiment 2
The 0.20mL butyl titanate is joined in the 8mL absolute ethyl alcohol, stirred 2 minutes, the Fe that 0.1g is prepared in advance 3O 4/ C microballoon adds in the lower alcohol, ultrasonic dispersion and stirring each 3 minutes.To contain Fe 3O 4The anhydrous alcohol solution of/C microballoon is poured in the crucible, places the top of sealable container then.Sealable container bottom is placed with 3mL distilled water in advance.With container airtight after, put into baking oven, begin to be heated to 200 ℃, heating rate is 10～20 ℃/minute, temperature reached after the temperature of setting insulation 10 hours.Naturally cool to room temperature after insulation finishes, open closed container, take out crucible, pour out powder, respectively wash 3 times, through 60 ℃ of vacuum dryings 8 hours with distilled water and absolute alcohol.
Embodiment 3
The 0.10mL butyl titanate is joined in the 8mL absolute ethyl alcohol, stirred 2 minutes, the Fe that 0.03g is prepared in advance 3O 4/ C microballoon adds in the lower alcohol, ultrasonic dispersion and stirring each 10 minutes.To contain Fe 3O 4The anhydrous alcohol solution of/C microballoon is poured in the crucible, places the top of sealable container then.Sealable container bottom is placed with 20mL distilled water in advance.With container airtight after, put into baking oven, begin to be heated to 200 ℃, heating rate is 20～30 ℃/minute, temperature reached after the temperature of setting insulation 8 hours.Naturally cool to room temperature after insulation finishes, open closed container, take out crucible, pour out powder, respectively wash 3 times, through 90 ℃ of vacuum dryings 24 hours with distilled water and absolute alcohol.
Embodiment 4
The 0.05mL butyl titanate is joined in the 8mL absolute ethyl alcohol, stirred 2 minutes, the Fe that 0.5g is prepared in advance 3O 4/ C microballoon adds in the lower alcohol, ultrasonic dispersion and stirring each 20 minutes.To contain Fe 3O 4The anhydrous alcohol solution of/C microballoon is poured in the crucible, places the top of sealable container then.Sealable container bottom is placed with 20mL distilled water in advance.With container airtight after, put into baking oven, begin to be heated to 200 ℃, heating rate is 20～30 ℃/minute, temperature reached after the temperature of setting insulation 18 hours.Naturally cool to room temperature after insulation finishes, open closed container, take out crucible, pour out powder, respectively wash 3 times, through 90 ℃ of vacuum dryings 48 hours with distilled water and absolute alcohol.
Fe wherein 3O 4/ C nano-powder is through with Fe 3O 4Microballoon obtains described Fe again after magnetic field recovery, washing, alcohol are washed, dried after carbon is modified 3O 4Microballoon is for what prepare through solvent thermal process, and concrete operation method is: with 1.35g FeCl 36H 2O, 3.6g anhydrous sodium acetate, 1g polyethylene glycol, 0.5g polyvinylpyrrolidone join in the 50mL ethylene glycol solution, through ultrasonic, stir after, place agitated reactor, after 10 hours, promptly get Fe 200 ℃ of reactions 3O 4Microballoon.

Claims (7)

1. Fe 3O 4/ C/TiO 2The preparation method of composite photo-catalyst comprises:
(1) the titanium alkoxide is dissolved in the anhydrous lower alcohol, processing concentration is the titanium alkoxide anhydrous alcohol solution of 0.001～0.12mL/mL;
(2) with Fe 3O 4/ C nano-powder adds in the above-mentioned titanium alkoxide anhydrous alcohol solution, through ultrasonic dispersion and stirring, obtains uniform mixture, wherein Fe 3O 4The concentration of/C is 0.5～100.0mg/mL;
(3) said mixture is put into the closed container that fills distilled water in advance, said mixture does not directly contact with distilled water, is heated to 70～200 ℃ then, is incubated 1～96 hour, and cool to room temperature with the washing of gained powder, drying, promptly gets Fe at last again 3O 4/ C/TiO 2Composite photo-catalyst.
2. a kind of Fe according to claim 1 3O 4/ C/TiO 2The preparation method of composite photo-catalyst is characterized in that: the titanium alkoxide in the said step (1) is one or more in tetraethyl titanate, tetraisopropyl titanate, the butyl titanate.
3. a kind of Fe according to claim 1 3O 4/ C/TiO 2The preparation method of composite photo-catalyst is characterized in that: the lower alcohol in the said step (1) is one or more in methyl alcohol, ethanol, normal propyl alcohol, the isopropyl alcohol.
4. a kind of Fe according to claim 1 3O 4/ C/TiO 2The preparation method of composite photo-catalyst is characterized in that: the Fe in the said step (2) 3O 4/ C nano-powder is through with Fe 3O 4Microballoon obtains after magnetic field recovery, washing, alcohol are washed, dried after carbon is modified again.
5. a kind of Fe according to claim 4 3O 4/ C/TiO 2The preparation method of composite photo-catalyst is characterized in that: described Fe 3O 4Microballoon is for what prepare through solvent thermal process, and concrete operation method is: with 1.35gFeCl 36H 2O, 3.6g anhydrous sodium acetate, 1g polyethylene glycol, 0.5g polyvinylpyrrolidone join in the 50mL ethylene glycol solution, through ultrasonic, stir after, place agitated reactor, after 10 hours, promptly get Fe 200 ℃ of reactions 3O 4Microballoon.
6. a kind of Fe according to claim 1 3O 4/ C/TiO 2The preparation method of composite photo-catalyst is characterized in that: the ratio of the amount of substance of titanium elements is 20～3000 in the distilled water in the said step (3) and the titanium alkoxide.
7. a kind of Fe according to claim 1 3O 4/ C/TiO 2The preparation method of composite photo-catalyst is characterized in that: the Fe that obtains in the said step (3) 3O 4/ C/TiO 2Composite photo-catalyst is a core/shell structure, and its center is Fe 3O 4Microballoon, transition zone are the C layer, and shell is that anatase titania is nanocrystalline, and crystallite dimension is 5～20nm.
CN2011102447660A 2011-08-25 2011-08-25 Preparation method of Fe3O4/C/TiO2 composite photocatalyst Pending CN102350353A (en)

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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN103191762A (en) * 2013-04-15 2013-07-10 天津大学 Fluorinated titanium dioxide/carbon /ferroferric oxide three-layer nanometer composite material and preparation method thereof
CN103456956A (en) * 2013-09-29 2013-12-18 东华大学 Preparation method for carbon nano-tube modified manganese phosphate lithium ion cell anode materials
CN104258859A (en) * 2014-09-09 2015-01-07 天津工业大学 Preparation method of Fe3O4@TiO2 photocatalyst and application of Fe3O4@TiO2 photocatalyst in degradation of fluorescent dye
CN105107505A (en) * 2015-07-02 2015-12-02 上海应用技术学院 Magnetic TiO2-porous carbon-Fe3O4 composite visible light photocatalyst and preparation method thereof
CN106964350A (en) * 2017-03-15 2017-07-21 武汉理工大学 A kind of Fe3O4@C@TiO2The simple method for preparing of Magneto separate photochemical catalyst
CN107174980A (en) * 2017-06-07 2017-09-19 常州诺澜复合材料有限公司 A kind of preparation method of cellulose lamination antibacterial ultrafiltration membrane
CN112090425A (en) * 2020-09-24 2020-12-18 青海师范大学 Magnetic carbon-supported TiO2Photocatalyst and preparation method thereof

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103191762A (en) * 2013-04-15 2013-07-10 天津大学 Fluorinated titanium dioxide/carbon /ferroferric oxide three-layer nanometer composite material and preparation method thereof
CN103456956A (en) * 2013-09-29 2013-12-18 东华大学 Preparation method for carbon nano-tube modified manganese phosphate lithium ion cell anode materials
CN103456956B (en) * 2013-09-29 2015-12-23 东华大学 A kind of preparation method of carbon nano tube modified manganese phosphate lithium ion cell anode
CN104258859A (en) * 2014-09-09 2015-01-07 天津工业大学 Preparation method of Fe3O4@TiO2 photocatalyst and application of Fe3O4@TiO2 photocatalyst in degradation of fluorescent dye
CN105107505A (en) * 2015-07-02 2015-12-02 上海应用技术学院 Magnetic TiO2-porous carbon-Fe3O4 composite visible light photocatalyst and preparation method thereof
CN105107505B (en) * 2015-07-02 2017-11-28 上海应用技术学院 A kind of magnetic TiO2Porous carbon Fe3O4Composite visible light catalyst and preparation method thereof
CN106964350A (en) * 2017-03-15 2017-07-21 武汉理工大学 A kind of Fe3O4@C@TiO2The simple method for preparing of Magneto separate photochemical catalyst
CN106964350B (en) * 2017-03-15 2019-08-23 武汉理工大学 A kind of Fe3O4@C@TiO2The simple preparation method of Magneto separate photochemical catalyst
CN107174980A (en) * 2017-06-07 2017-09-19 常州诺澜复合材料有限公司 A kind of preparation method of cellulose lamination antibacterial ultrafiltration membrane
CN112090425A (en) * 2020-09-24 2020-12-18 青海师范大学 Magnetic carbon-supported TiO2Photocatalyst and preparation method thereof

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Application publication date: 20120215