CN101856628A - Conducting polymer modified magnetic photocatalyst and preparation method thereof - Google Patents
Conducting polymer modified magnetic photocatalyst and preparation method thereof Download PDFInfo
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- CN101856628A CN101856628A CN 201010165113 CN201010165113A CN101856628A CN 101856628 A CN101856628 A CN 101856628A CN 201010165113 CN201010165113 CN 201010165113 CN 201010165113 A CN201010165113 A CN 201010165113A CN 101856628 A CN101856628 A CN 101856628A
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Abstract
The invention belongs to the technical fields of photocatalysts and a preparation method thereof, in particular to a conducting polymer modified magnetic photocatalyst and a preparation method thereof. The catalyst can realize photocatalysis under visible light. The magnetic photocatalyst of the invention comprises a composite catalyst in a three-layer cladding structure, an inner core is magnetic fine particles, the outer layer is cladded with SiO2, the outer side of the SiO2 is cladded with TiO2, and the outer side of the TiO2 is cladded with a small number of conducting polymers. The preparation method mainly comprises the following steps: preparing monodisperse magnetic fine particles; preparing magnetic SiO2 core case fine particles; preparing magnetic SiO2/TiO2 composite fine particles; and preparing magnetic SiO2/TiO2 composite fine particles decorated by the conducting polymers. The preparation method of the photocatalyst with high catalyst efficiency and magnetic recovery capability of the invention has simple operation and low requirement on equipment.
Description
Technical field
The invention belongs to the technical field of photochemical catalyst and preparation method thereof, be specifically related to a kind of conducting polymer modified magnetic photocatalyst and preparation method thereof, this catalyst can carry out photocatalysis under visible light.
Background technology
Along with the energy, environmental problem are serious day by day, the raising of people's living standard and the reinforcement of environmental consciousness are to the research of waste water or sewage disposal with implement also deepening constantly and developing.Existing sewage water treatment method generally has physical filtering method, chemistry-oxidizing process, photocatalytic degradation method etc.Wherein, the photocatalytic degradation method is because of utilizing light as the energy source excitation, and semiconductor resolves into carbon dioxide, water or low molecular compound as the organic pollution in photochemical catalyst decomposition waste water or the sewage, has obtained extensive studies and application.Semiconductor light-catalyst (the TiO that is being studied
2, ZnO, Fe
2O
3, CdS, CdSe etc.) in because some compound itself has certain toxicity, and the semiconductor that has is unstable under illumination, has photoetch phenomenon in various degree, so have only TiO at present
2Be research and widely used semiconductor light-catalyst.But TiO
2There are shortcomings such as recovery is difficult, photocatalysis efficiency is low in photochemical catalyst.
Magnetic nanoparticle has the magnetic response performance, but the outside magnetic field effect reclaim down, and have characteristics such as convenient and swift, extraction efficiency height.Be called " magnetic Nano TiO as the disclosed name of CN 1562817A
2/ SiO
2/ Fe
3O
4Composite photo-catalyst purify liquid waste method and device " the Chinese invention patent application, prepare the TiO of double-coating structure
2/ SiO
2/ Fe
3O
4Composite photo-catalyst uses ultraviolet light as light source, and has invented the device that a cover is purified liquid waste, and improves cleaning water.This patent improves the photocatalysis effect by the improvement of device, but the catalytic efficiency of prepared photochemical catalyst itself is still waiting to improve.In order to improve the photo-catalysis capability of titanium dioxide, can carry out modification to it and handle, as noble metal loading, ion doping, photoactivate, surface reduction processing etc., the wherein extensible TiO of photoactivate
2Excitation wavelength range, improve long-wave radiation photon utilization rate, be to improve TiO
2One of main research contents of photo-quantum efficiency.The photolytic activity sensitizer has bigger motivating factor under visible light, under radiation of visible light, ADSORPTION STATE photolytic activity molecule absorption photon is excited, and produces free electron, and excitation state photolytic activity molecule is injected into TiO with electronics then
2Conduction band on, enlarge TiO
2The scope of excitation wavelength makes it to utilize visible light to come degradation of organic substances.Wherein, conducting polymer has conjugated structure because of it, is good sensitising agent.As disclosed Chinese invention patent application that is called " polyaniline-nano Zns Compound photocatalyst and preparation method thereof " of CN 101444751A, be skeleton with the polyaniline, loaded with nano ZnS has catalytic action under ultraviolet light and radiation of visible light.
Summary of the invention
But one of purpose of the present invention is to provide the magnetic photocatalyst of a kind of treatment effeciency height, the low magnetic recovery of cost, this catalyst can be with the organic harmful substance degraded in waste water or the sewage, waste water or sewage are purified effectively, and can carry out recycling to photochemical catalyst by applying magnetic field.
But another object of the present invention is to provide the preparation method of the magnetic photocatalyst of a kind of treatment effeciency height, the low magnetic recovery of cost, this method preparation is simple, productive rate is high.
A kind of conducting polymer modified magnetic photocatalyst of the present invention, described magnetic photocatalyst has the composite catalyst of three layers of clad structure, and its kernel is a magnetic particle, and skin is coated with SiO
2, SiO
2The outside be coated with TiO
2, TiO
2The outside be coated with a small amount of conducting polymer again.
Further, the magnetic particle material of above-mentioned kernel is tri-iron tetroxide, γ-di-iron trioxide, NiFe
2O
4, CoFe
2O
4Wherein one or more.
Further, the spherolite of the magnetic particle of above-mentioned kernel footpath size is at 100～400nm.
The preparation method of a kind of conducting polymer modified magnetic photocatalyst of the present invention is as follows:
With the magnetic particle is kernel, utilizes the principle of sol-gel chemistry, adopts silicon source precursor hydrolysis, at first coats the last layer amorphous silica on the magnetic particle surface; Utilize sol-gel process to coat layer of titanium dioxide then, through obtaining the titanium dioxide of Detitanium-ore-type after the high-temperature process at the silica laminar surface; Then be dispersed in the aqueous hydrochloric acid solution of conducting polymer monomer, add oxidizing agent solution, obtain conducting polymer modified magnetic photocatalyst powder after the reaction.
The principle of conducting polymer modified photochemical catalyst is: photochemical catalyst is under the effect of luminous energy, and the conducting polymer that is coated on photocatalyst surface absorbs photon and is excited, and produces a large amount of free electrons, then electronics is transferred to TiO
2Conduction band on, improved separation of charge efficient, therefore improved the photocatalytic activity of photochemical catalyst.Therefore this light induced electron has strong reducing property, and the low energy valence band then photohole occurs, has strong oxidability, but sterilization, sterilization, almost can all organic pollutions of oxidation.
The concrete preparation process of a kind of conducting polymer modified magnetic photocatalyst of the present invention is:
1) adopts solvent thermal method, prepare monodispersed magnetic particle.
2) preparation magnetic SiO
2Core-shell particle, method is as follows:
Take by weighing the magnetic particle of step 1), after the surface treatment of hydrochloric acid weak solution with it in ultrasonic mixed liquor that is distributed to deionized water, absolute ethyl alcohol and ammoniacal liquor (25wt%), add silicon source precursor, normal temperature mechanical agitation 1～10h, the mass ratio of the magnetic particle in the reaction system, silicon source precursor, deionized water, ethanol, ammoniacal liquor (25wt%) is 0.1: 0.1～0.4: 10～30: 40～100: 1～6.Reaction finishes the back Magnetic Isolation, and washs respectively 3～5 times with absolute ethyl alcohol and deionized water, and is dry in 60 ℃ of drying boxes.
Among the present invention, described inorganic nano-particle saturation magnetization height has good magnetic response performance, good dispersion.The size of particulate is at 100～400nm, and the material of this particulate is tri-iron tetroxide (Fe
3O
4), γ-di-iron trioxide (γ-Fe
2O
3), NiFe
2O
4, CoFe
2O
4Wherein one or more.Described silicon source is one or more in ethyl orthosilicate (TEOS), the methyl silicate (TMOS).
3) preparation magnetic SiO
2/ TiO
2Composite particles:
Take by weighing step 2) preparation magnetic SiO
2The core-shell particle powder is ultrasonic to be dispersed in the ethanolic solution of butyl titanate, the normal temperature magnetic agitation, and the mixture (volume ratio is 1: 3～1: 10) with water and ethanol is added drop-wise in the above-mentioned solution then, drips the back and continues to stir 1～6h.Wherein in the reaction system, magnetic SiO
2The mass ratio of core-shell particle, butyl titanate, ethanol, deionized water is 0.1: 0.5～2.0: 10～50: 0.2～0.5.React the Magnetic Isolation that finishes, the ethanol washing, drying obtains magnetic SiO at 300～500 ℃ of sintering 2～5h
2/ TiO
2The composite particles powder.
4) the conducting polymer modified magnetic SiO of preparation
2/ TiO
2Composite particles:
Take by weighing the magnetic SiO of step 3) preparation
2/ TiO
2The composite particles powder is ultrasonic to be distributed in the aqueous solution of HCl, adds the conducting polymer monomer, and magnetic agitation adds the aqueous solution of oxidant then.Wherein in the reaction system, magnetic SiO
2/ TiO
2, HCl, conducting polymer monomer, deionized water, oxidant mass ratio be 0.2: 0.1～1.0: 0.003～0.01: 10～50: 0.005～0.06, stirring at normal temperature 4～18h, Magnetic Isolation, deionized water, ethanol washing are colourless to the upper strata, drying.
Described conducting polymer monomer is aniline or pyrroles, and described oxidant is potassium peroxydisulfate, ammonium persulfate or iron chloride.
As mentioned above, the present invention is under the reaction condition of gentleness, synthesized conducting polymer modified magnetic photocatalyst by mild condition, technology simple to operate, this material has following characteristics: (1) magnetisable material content height, has very strong external magnetic field response, the saturation magnetization height has separating power preferably; (2) under visible light irradiation, can good degradation capability be arranged to organic pollution.Conducting polymer modified magnetic photocatalyst does not need to add in addition other chemical agents among the present invention, in the degradation water during organic pollution, end product is carbon dioxide, water and organic molecule, can not produce secondary pollution to environment, meets " green " environmental protection requirement.And behind photocatalytic degradation, but apply external magnetic field magnetic recovery photochemical catalyst, reuse economic environmental protection.
But the preparation method of the photochemical catalyst of high catalytic efficiency magnetic recovery of the present invention is simple to operate, requires lower to equipment.
Description of drawings
Fig. 1 is Fe in the embodiment of the invention 1
3O
4The TEM photo.
Fig. 2 is the TEM photo of the magnetic photocatalyst that polyaniline is modified in the embodiment of the invention 1.
The specific embodiment
Embodiment 1:
With aniline is monomer, and ammonium persulfate is an oxidant, obtains the Fe that polyaniline is modified
3O
4/ SiO
2/ TiO
2Photochemical catalyst.
1) the utilization solvent-thermal method prepares monodispersed Fe
3O
4Particulate, spherolite directly are～200nm (as Fig. 1).
2) with Fe synthetic in the 0.10g step 1)
3O
4Particulate, in the ultrasonic HCl aqueous solution that is scattered in 50mL 0.1mol/L, Magnetic Isolation, deionized water washing 3 times is dispersed in 80mL ethanol, 20mL deionized water and 4mLNH then
3H
2In the mixed solution of O (25wt%), stir adding 0.25mL ethyl orthosilicate down, behind the stirring 6h, Magnetic Isolation, ethanol, water respectively wash 3 times, and is dry in 60 ℃ of drying boxes.
3) take by weighing 0.10g step 2) synthetic Fe
3O
4/ SiO
2Core-shell particle is ultrasonic to be dispersed in the mixed solution of 1mL butyl titanate and 35mL ethanol, and (v/v=1: mixture 5) drips the back and continues to stir 2h slowly to drip 2mL water/ethanol then under the normal temperature magnetic agitation, Magnetic Isolation, the ethanol washing, drying, 450 ℃ of sintering 2h obtain Fe
3O
4/ SiO
2/ TiO
2The composite particles powder.
4) take by weighing the synthetic Fe of 0.20g step 3)
3O
4/ SiO
2/ TiO
2Be dispersed in the HCl aqueous solution of 20mL 0.20mol/L, add the 0.006g aniline monomer; Add the aqueous solution of 1mL ammonium persulfate under the magnetic agitation, wherein the mol ratio of ammonium persulfate and aniline is 1: 1, stirring at normal temperature 12h, and Magnetic Isolation, deionized water, ethanol wash colourless to the upper strata, drying.
The Fe that the polyaniline of preparation is modified
3O
4/ SiO
2/ TiO
2Composite as shown in Figure 2, saturation magnetization is 17.5emu/g, the average diameter of particulate is 235nm, wherein Fe
3O
4The particulate average diameter is 200nm, SiO
2Average bed thickness is 10nm, TiO
2Average bed thickness is 20nm, and surperficial polyaniline granular size is about 5nm.
Embodiment 2
With pyrroles is monomer, and ammonium persulfate is an oxidant, obtains the Fe of polypyrrole modifying
3O
4/ SiO
2/ TiO
2Photochemical catalyst.
1) the utilization solvent-thermal method prepares monodispersed Fe
3O
4Particulate, the particulate average diameter is～200nm.
2) with Fe synthetic in the 0.10g step 1)
3O
4Particulate, in the ultrasonic HCl aqueous solution that is scattered in 50mL 0.1mol/L, Magnetic Isolation after the deionized water washing 3 times, is dispersed in 80mL ethanol, 20mL deionized water and 4mL NH
3H
2In the mixed liquor of O (25wt%), stir adding 0.25mL methyl silicate down, stir 6h, Magnetic Isolation, ethanol, water respectively wash 3 times, and is dry in 60 ℃ of drying boxes.
3) take by weighing 0.10g step 2) synthetic Fe
3O
4/ SiO
2Core-shell particle is ultrasonic to be dispersed in the mixed solution of 1mL butyl titanate and 35mL ethanol, and (v/v=1: mixture 5) drips the back and continues to stir 2h slowly to drip 2mL water/ethanol under the normal temperature magnetic agitation, Magnetic Isolation, the ethanol washing, drying, 450 ℃ of sintering 2h obtain Fe
3O
4/ SiO
2/ TiO
2The composite particles powder.
4) take by weighing the synthetic Fe of 0.20g step 3)
3O
4/ SiO
2/ TiO
2Be dispersed in the HCl solution of 20mL 0.20mol/L, add the 0.005g pyrrole monomer; Add the aqueous solution of 1mL potassium peroxydisulfate under the magnetic agitation, wherein potassium peroxydisulfate and pyrroles's mol ratio is 1: 1, stirring at normal temperature 12h, and Magnetic Isolation, deionization, ethanol wash colourless to the upper strata, drying.
The Fe of the polypyrrole modifying of preparation
3O
4/ SiO
2/ TiO
2Composite, saturation magnetization are 18.7emu/g, and its average diameter is 240nm, wherein Fe
3O
4The particulate average diameter is 200nm, SiO
2Bed thickness is 10nm, TiO
2Bed thickness is 20nm, and the polypyrrole particle is 10nm.
Embodiment 3:
With aniline is monomer, and ammonium persulfate is an oxidant, obtains the NiFe that polyaniline is modified
2O
4/ SiO
2/ TiO
2Photochemical catalyst.
1) the utilization solvent-thermal method prepares monodispersed NiFe
2O
4Particulate, spherolite directly are～200nm.
2) with NiFe synthetic in the 0.10g step 1)
2O
4Particulate, in the ultrasonic HCl aqueous solution that is scattered in 50mL 0.1mol/L, Magnetic Isolation after the deionized water washing 3 times, is dispersed in 80mL ethanol, 20mL deionized water and 4mLNH
3H
2In the mixed solution of O (25wt%), stir adding 0.25mL methyl silicate down, stir 6h, Magnetic Isolation, ethanol, water respectively wash 3 times, 60 ℃ of dryings.
3) take by weighing 0.10g step 2) synthetic NiFe
2O
4/ SiO
2Core-shell particle is ultrasonic to be dispersed in the mixed solution of 1mL butyl titanate and 35mL ethanol, and (v/v=1: mixture 5) drips the back and continues to stir 2h slowly to drip 2mL water/ethanol under the normal temperature magnetic agitation, Magnetic Isolation, the ethanol washing, drying, 450 ℃ of sintering 2h obtain NiFe
2O
4/ SiO
2/ TiO
2The composite particles powder.
4) take by weighing the synthetic NiFe of 0.20g step 3)
2O
4/ SiO
2/ TiO
2Be dispersed in the HCl aqueous solution of 20mL 0.20mol/L, add the 0.006g aniline monomer then; Add the aqueous solution of 1mL ammonium persulfate under the magnetic agitation, wherein the mol ratio of ammonium persulfate and aniline is 1: 1, stirring at normal temperature 12h, and Magnetic Isolation, deionized water, ethanol wash colourless to the upper strata, drying.
The NiFe that the polyaniline of preparation is modified
2O
4/ SiO
2/ TiO
2Composite particles, saturation magnetization are 23.9emu/g, and average diameter is 235nm, wherein NiFe
2O
4The particulate average diameter is 200nm, SiO
2Average bed thickness is 10nm, TiO
2Average bed thickness is 20nm, and surperficial polyaniline granular size is 5nm.
Embodiment 4:
With aniline is monomer, and potassium peroxydisulfate is an oxidant, obtains the CoFe that polyaniline is modified
2O
4/ SiO
2/ TiO
2Photochemical catalyst.
1) the monodispersed CoFe of utilization Hydrothermal Preparation
2O
4Particulate, spherolite directly are～200nm.
2) with CoFe synthetic in the 0.10g step 1)
2O
4Particulate, in the ultrasonic HCl aqueous solution that is scattered in 50mL 0.1mol/L, Magnetic Isolation, deionized water washing 3 times is dispersed in 80mL ethanol, 20mL deionized water and 4mL NH then
3H
2In the mixed solution of O (25wt%), stir adding 0.25mL ethyl orthosilicate down, stir 6h, Magnetic Isolation, ethanol, water respectively wash 3 times, and is dry in 60 ℃ of drying boxes.
3) take by weighing 0.10g step 2) synthetic CoFe
2O
4/ SiO
2Core-shell particle is ultrasonic to be dispersed in the mixed solution of 1mL butyl titanate and 35mL ethanol, and (v/v=1: mixture 5) drips the back and continues to stir 2h slowly to drip 2mL water/ethanol under the normal temperature magnetic agitation, Magnetic Isolation, the ethanol washing, drying, 450 ℃ of sintering 2h obtain CoFe
2O
4/ SiO
2/ TiO
2The composite particles powder.
4) take by weighing the synthetic CoFe of 0.20g step 3)
2O
4/ SiO
2/ TiO
2Be dispersed in the HCl aqueous solution of 20mL 0.20mol/L, add the 0.006g aniline monomer then; Add the aqueous solution of 1mL ammonium persulfate under the magnetic agitation, wherein the mol ratio of ammonium persulfate and aniline is 1: 1, stirring at normal temperature 12h, and Magnetic Isolation, deionized water, ethanol wash colourless to the upper strata, drying.
The CoFe that the polyaniline of preparation is modified
2O
4/ SiO
2/ TiO
2Composite particles, saturation magnetization are 20.1emu/g, and average diameter is 235nm, wherein CoFe
2O
4The particulate average diameter is 200nm, SiO
2Average bed thickness is 10nm, TiO
2Average bed thickness is 20nm, and the polyaniline particle on surface is 5nm.
Claims (8)
1. conducting polymer modified magnetic photocatalyst, it is characterized in that: described magnetic photocatalyst has the composite catalyst of three layers of clad structure, and its kernel is a magnetic particle, and skin is coated with SiO
2, SiO
2The outside be coated with TiO
2, TiO
2The outside be coated with a small amount of conducting polymer again.
2. a kind of conducting polymer modified magnetic photocatalyst according to claim 1 is characterized in that: the magnetic particle material of described kernel is tri-iron tetroxide, γ-di-iron trioxide, NiFe
2O
4, CoFe
2O
4Wherein one or more.
3. a kind of conducting polymer modified magnetic photocatalyst according to claim 1 is characterized in that: the spherolite footpath size of the magnetic particle of described kernel is at 100～400nm.
4. the preparation method of a conducting polymer modified magnetic photocatalyst is characterized in that, described method comprises the steps:
4.1 the employing solvent thermal method prepares monodispersed magnetic particle;
4.2 preparation magnetic SiO
2Core-shell particle, method is as follows: the magnetic particle that takes by weighing step 4.1 gained, after the surface treatment of hydrochloric acid weak solution with it in ultrasonic mixed liquor that is distributed to deionized water, absolute ethyl alcohol and ammoniacal liquor (25wt%), add silicon source precursor, normal temperature mechanical agitation 1～10h, the mass ratio of the magnetic particle in the reaction system, silicon source precursor, deionized water, ethanol, ammoniacal liquor (25wt%) is 0.1: 0.1～0.4: 10～30: 40～100: 1～6; Reaction finishes the back Magnetic Isolation, and washs respectively 3～5 times with absolute ethyl alcohol and deionized water, and is dry in 60 ℃ of drying boxes;
4.3 preparation magnetic SiO
2/ TiO
2Composite particles, method is as follows:
Take by weighing the magnetic SiO of step 4.2 preparation
2The core-shell particle powder is ultrasonic to be dispersed in the ethanolic solution of butyl titanate, and the normal temperature magnetic agitation is that 1: 3～1: 10 mixture is added drop-wise in the above-mentioned solution then with water and ethanol volume ratio, and drip the back and continue to stir 1-6h, wherein in the reaction system, magnetic SiO
2The mass ratio of core-shell particle, butyl titanate, ethanol, deionized water is 0.1: 0.5～2.0: 10～50: 0.2～0.5; React the Magnetic Isolation that finishes, the ethanol washing, drying obtains magnetic SiO at 300～500 ℃ of sintering 2～5h
2/ TiO
2The composite particles powder;
4.4 prepare conducting polymer modified magnetic SiO
2/ TiO
2Composite particles, method is as follows:
Take by weighing the magnetic SiO of step 4.3 preparation
2/ TiO
2The composite particles powder is ultrasonic to be distributed in the aqueous solution of HCl, adds the conducting polymer monomer, and magnetic agitation adds the aqueous solution of oxidant then, wherein in the reaction system, and magnetic SiO
2/ TiO
2, HCl, conducting polymer monomer, deionized water, oxidant mass ratio be 0.2: 0.1～1.0: 0.003～0.01: 10～50: 0.005～0.06, stirring at normal temperature 4～18h, Magnetic Isolation, deionized water, ethanol washing are colourless to the upper strata, drying.
5. the preparation method of a kind of conducting polymer modified magnetic photocatalyst according to claim 4, it is characterized in that: in the described step 4.1, the material of described magnetic particle is tri-iron tetroxide, γ-di-iron trioxide, NiFe
2O
4, CoFe
2O
4Wherein one or more.
6. the preparation method of a kind of conducting polymer modified magnetic photocatalyst according to claim 4 is characterized in that: in the described step 4.1, the spherolite of described magnetic particle footpath size is at 100～400nm.
7. the preparation method of a kind of conducting polymer modified magnetic photocatalyst according to claim 4, it is characterized in that: in the described step 4.1, described silicon source is one or more in ethyl orthosilicate, the methyl silicate.
8. the preparation method of a kind of conducting polymer modified magnetic photocatalyst according to claim 4, it is characterized in that: in the described step 4.4, described conducting polymer monomer is aniline or pyrroles, and described oxidant is potassium peroxydisulfate, ammonium persulfate or iron chloride.
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