CN102921435A - Magnetic Fe3O4/SiO2/TiO2/quantum dot compounded nanometer photocatalyst and preparation method and application thereof - Google Patents
Magnetic Fe3O4/SiO2/TiO2/quantum dot compounded nanometer photocatalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of treatment and application of nanometer materials and industrial and agricultural wastewater, and provides a magnetic Fe3O4/SiO2/TiO2/quantum dot compounded nanometer photocatalyst and a preparation method and application thereof. The preparation method comprises the following steps of: synthesizing an Fe3O4 magnetic nucleus by a coprecipitation method; preparing an SiO2 protective layer by virtue of hydrolysis reaction and polycondensation reaction of TEOS (Tetraethyl Orthosilicate); then preparing a TiO2 layer on the surface of the SiO2 protective layer by a sol-gel method; and finally modifying Fe3O4/SiO2/TiO2 nanoparticles by CdS and CdSe quantum dots. The obtained magnetic Fe3O4/SiO2/TiO2/quantum dot compounded nanometer photocatalyst has very good visible-light photocatalytic capability, can be conveniently and fast recovered and reused by an external magnetic field, and can be used for removing organic pollutants of azo dyes contained in the industrial wastewater.
Description
Technical field
The invention belongs to nano material and industrial and agricultural wastewater and process applied technical field, be specifically related to a kind of magnetic Fe
3O
4/ SiO
2/ TiO
2/ quantum dot composite Nano photochemical catalyst and its preparation method and application.
Background technology
Along with the expansion of expanding economy and population, difficult decomposing organic pollutant sharply increases in the water, and human this limited water resource is subject to severe contamination, has developed into the stage that threatens human survival.To effective control of the processing of these pollutants and environmental pollution and the significant problem of administering the institute that become countries in the world and facing and needing to be resolved hurrily.Catalysis material has light hydrogen production by water decomposition and light degradation organic pollution two large functions, the photoactivation material both can be converted into low-density solar energy storable highdensity Hydrogen Energy, also can utilize the pollutant in solar energy degraded and the mineralising environment, so it there is being important application prospect aspect the solution energy and the environmental problem.With TiO
2TiO with modification
2For there is the utilization rate of solar energy in the catalysis material that represents and the problems such as light conversion efficiency is low, poor stability, narrow, the difficult recovery of spectral response range, restricted its large-scale commercial applications application.
Summary of the invention
The present invention is exactly for weak point of the prior art, and a kind of novel Fe is provided
3O
4/ SiO
2/ TiO
2/ quantum dot composite Nano photochemical catalyst, this catalyst is with Fe
3O
4Be magnetic nuclear, thereon coated Si O
2Protective layer, again composite Ti O
2Catalysis material, and with CdS, the modification of CdSe quantum dot.This catalyst has good degradation effect to azo dyes such as rose-red, methylene blue, methyl oranges, and can utilize the quick recycling use of permanent magnet, greatly reduces production costs.
The objective of the invention is to be achieved by the following technical measures.
A kind of magnetic Fe
3O
4/ SiO
2/ TiO
2/ quantum dot composite Nano photochemical catalyst, this photochemical catalyst adopts Fe
3O
4Nano particle is magnetic nuclear, examines surperficial coated Si O at magnetic
2Protective layer, again composite Ti O
2Catalysis material is modified with CdS, CdSe quantum dot at last.
The present invention also provides a kind of above-mentioned magnetic Fe
3O
4/ SiO
2/ TiO
2The preparation method of/quantum dot composite Nano photochemical catalyst, this photochemical catalyst adopts the synthetic Fe of coprecipitation
3O
4Magnetic nuclear utilizes hydrolysis and the polycondensation reaction of tetraethyl orthosilicate (TEOS) to prepare SiO
2Protective layer is used sol-gel process composite Ti O again
2Layer namely gets Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle is modified Fe with CdS, CdSe quantum dot at last
3O
4/ SiO
2/ TiO
2Nano particle, it specifically may further comprise the steps:
(1) coprecipitation prepares magnetic nuclear Fe
3O
4Nano particle
Take by weighing 5.44 g FeCl
3With 3 g FeCl
2Be dissolved into respectively in the 50 ml deionized waters, more respectively toward FeCl
3And FeCl
2The aqueous solution in add the Macrogol 2000 of 2 g, stir with glass bar they fully dissolved; The FeCl of dissolve complete
3And FeCl
2The aqueous solution transfer in the there-necked flask, nitrogen protection, 60 ℃ of stirring in water bath add 50 ml ammoniacal liquor again in the there-necked flask, stop after stirring 1.5 h, leave standstill 0.5 h; Clean respectively above-mentioned reaction product 3 times with alcohol and deionized water after reaction is finished, the dilval magnet stronger with magnetic reclaims flushing to above-mentioned reaction product, namely gets Fe
3O
4Nano particle;
(2) hydrolysis and the polycondensation reaction of tetraethyl orthosilicate (TEOS) prepare SiO
2Protective layer
The Fe of preparation in (1)
3O
4Nano particle is dispersed in the mixed solution of ethanol and deionized water, mixed proportion 4:1,120 ml alcohol; 30 ml water; nitrogen protection is heated to 60 ℃, and 30 min stir; successively 4 ml ethyl orthosilicates (TEOS) and 4 ml ammoniacal liquor are added in the above-mentioned mixed liquor; after continue stirring 12 h, above-mentioned reaction product is shifted out, put into vacuum drying chamber after cleaning successively 3 times with alcohol and deionized water; at 60 ℃ of lower dry 24 h, namely get Fe
3O
4/ SiO
2Compound particle;
(3) sol-gel process composite Ti O
2Layer
Take by weighing the Fe of preparation in (2)
3O
4/ SiO
2Compound particle 0.65 g adds 0.5 ml isopropyl titanate in the 60 ml absolute ethyl alcohols, and the hydrochloric acid with 0.1 ml concentration 33% joins in the 40 ml absolute ethyl alcohols again, above-mentioned three is mixed the there-necked flask of transferring to 250 ml, nitrogen protection is heated to 60 ℃, stirs 30 min it is mixed; Deionized water with 9 ml joins in the there-necked flask at last, continue to stir 12 h, be put into 60 ℃ of dryings in the vacuum drying chamber after the above-mentioned reaction product that obtains cleaned 3 times successively with alcohol and deionized water, put into again 550 ℃ of annealing of annealing furnace, 1 h, namely get Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle;
(4) CdS, CdSe quantum dot are modified Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle
Take by weighing the Fe of preparation in (3)
3O
4/ SiO
2/ TiO
2Magnetic nano-particle 0.6 g is dispersed in the 300 ml deionized waters, to the CdCl that wherein adds 15 ml, 0.1 M
2The thiourea solution of the sodium citrate solution of solution, 20 ml, 0.1 M and 30 ml, 0.1 M mixes, and with ammoniacal liquor pH is transferred to about 10.5,65 ℃ of uniform stirring 2 h, centrifugal recovery with alcohol and the above-mentioned reaction product of washed with de-ionized water, namely obtains the Fe that the CdS quantum dot is modified
3O
4/ SiO
2/ TiO
2Magnetic nano-particle;
In the supersaturation sodium sulfite solution that 90 ℃ are dissolved in 0.4 g selenium powder 100 ml, make sodium thiosulfate solution, getting 0.23 g caddy is dissolved in the 100 ml deionized waters, drip 0.5 ml TGA, add gradually again 1.0 M sodium hydroxide solutions, the pH value of solution is reached about 9.0, at this moment solution becomes water white TGA cadmium solution, measure 10 ml TGA cadmiums, add 40 ml deionized waters, add again sodium thiosulfate solution, ultrasonic dispersion 30 min, it is mixed, then solution is transferred in the there-necked flask, add 0.6 g Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle and 0.5ml mercaptopropionic acid, 60 ℃ of uniform stirring 30 min, centrifugal recovery with alcohol and the above-mentioned reaction product of washed with de-ionized water, namely obtains the Fe that the CdSe quantum dot is modified
3O
4/ SiO
2/ TiO
2Magnetic nano-particle.
The present invention utilizes Fe
3O
4The superparamagnetism of nano particle is elected it as magnetic nuclear, examines surperficial coated Si O at magnetic
2Protective layer, again composite Ti O
2Catalysis material is modified with CdS, CdSe quantum dot at last, obtains Fe
3O
4/ SiO
2/ TiO
2/ CdS and Fe
3O
4/ SiO
2/ TiO
2/ CdSe composite Nano photochemical catalyst.
Wherein, Fe
3O
4Both had higher saturation magnetization, be convenient to magnetic recovery; Good paramagnetism is arranged again, be convenient to the dispersion of magnetic loading catalysis material.Simultaneously, for the preparation of Fe
3O
4Raw material cheap and easy to get, be conducive to reduce cost.Thereby, Fe
3O
4It is one of photocatalysis magnetic loading material that has most application prospect.Catalysis material is loaded on Fe
3O
4On, utilize external magnetic field that catalyst is separated effectively fast and reclaim, can improve its cyclic utilization rate.
At catalysis material and Fe
3O
4Between introduce the inertia intermediate layer, such as SiO
2Protective layer can stop photo-generated carrier to the migration of magnetic nuclear, improves photocatalysis efficiency.SiO
2Protective layer can also stop particle to be reunited, and effectively reduces the dipolar interaction between the magnetic nano-particle; And make compound system have good biological hydrophily, compatibility and extraordinary colloidal stability and chemical stability.
TiO
2Be excellent semiconductor light-catalyst, be widely used in photocatalysis degradation organic contaminant and the light decomposition water obtains hydrogen energy source.Yet TiO
2Energy gap be 3.2 eV, corresponding absorbing wavelength is at 365 nm, only ultraviolet light is had strong assimilation effect.And ultraviolet light only accounts for 5% of sunshine, in order to make TiO
2Can efficiently utilize sunshine, widen photochemical catalyst to the response range of solar spectrum, improve catalytic efficiency, introduce semiconductor-quantum-point.Be compounded with many advantages with semiconductor-quantum-point: (1) can regulate level structure by the size of control quantum dot, makes its absorption spectrum can mate sunshine spectrum, realizes wide spectral response; (2) natural dipole moment of semiconductor-quantum-point can make electric charge separate fast, is beneficial to the electric charge transmission; (3) photon of quantum dot absorption can produce a plurality of light induced electrons, is expected to significantly improve photoelectric transformation efficiency.CdS and CdSe are important II-VI compounds of group, and their energy gap is respectively 2.25 eV and 1.7 eV.The introducing of quantum dot has improved photocatalysis efficiency and its utilization rate to sunshine.Result of study shows, the Fe that does not have quantum dot to modify
3O
4/ SiO
2/ TiO
2Photochemical catalyst does not have visible light-responded ability, and the Fe that semiconductor-quantum-point is modified
3O
4/ SiO
2/ TiO
2/ CdS and Fe
3O
4/ SiO
2/ TiO
2/ CdSe composite Nano photochemical catalyst has very high catalytic effect, as shown in Figure 2.
In sum, Fe
3O
4/ SiO
2/ TiO
2/ quantum dot composite Nano photochemical catalyst has good visible light catalytic ability, and this catalyst has good degradation effect to azo dyes such as rose-red, methylene blue, methyl oranges, and can utilize the quick recycling use of permanent magnet, greatly reduces production costs.
Description of drawings
Fig. 1 is magnetic Fe of the present invention
3O
4/ SiO
2/ TiO
2The structural representation of/quantum dot composite Nano photochemical catalyst.
Fig. 2 is common Fe
3O
4/ SiO
2/ TiO
2Photochemical catalyst and the Fe that modifies with CdS, CdSe quantum dot
3O
4/ SiO
2/ TiO
2The experimental curve diagram of nano particle photocatalyst degradation of methylene blue under visible light.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
As shown in Figure 1, present embodiment provides a kind of magnetic Fe
3O
4/ SiO
2/ TiO
2/ quantum dot composite Nano photochemical catalyst, this photochemical catalyst adopts Fe
3O
4Nano particle is magnetic nuclear, examines surperficial coated Si O at magnetic
2Protective layer, again composite Ti O
2Catalysis material is modified with CdS, CdSe quantum dot at last.
Present embodiment also provides a kind of above-mentioned magnetic Fe
3O
4/ SiO
2/ TiO
2The preparation method of/quantum dot composite Nano photochemical catalyst, this photochemical catalyst adopts the synthetic Fe of coprecipitation
3O
4Magnetic nuclear utilizes hydrolysis and the polycondensation reaction of tetraethyl orthosilicate (TEOS) to prepare SiO
2Protective layer is used sol-gel process composite Ti O again
2Layer namely gets Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle is modified Fe with CdS, CdSe quantum dot at last
3O
4/ SiO
2/ TiO
2Nano particle, it specifically may further comprise the steps:
(1) coprecipitation prepares magnetic nuclear Fe
3O
4Nano particle
Take by weighing 5.44 g FeCl
3With 3 g FeCl
2Be dissolved into respectively in the 50 ml deionized waters, more respectively toward FeCl
3And FeCl
2The aqueous solution in add the Macrogol 2000 of 2 g, stir with glass bar they fully dissolved; The FeCl of dissolve complete
3And FeCl
2The aqueous solution transfer in the there-necked flask, nitrogen protection, 60 ℃ of stirring in water bath add 50 ml ammoniacal liquor again in the there-necked flask, stop after stirring 1.5 h, leave standstill 0.5 h; Clean respectively above-mentioned reaction product 3 times with alcohol and deionized water after reaction is finished, the dilval magnet stronger with magnetic reclaims flushing to above-mentioned reaction product, namely gets Fe
3O
4Nano particle;
(2) hydrolysis and the polycondensation reaction of tetraethyl orthosilicate (TEOS) prepare SiO
2Protective layer
The Fe of preparation in (1)
3O
4Nano particle is dispersed in the mixed solution of ethanol and deionized water, mixed proportion 4:1,120 ml alcohol; 30 ml water; nitrogen protection is heated to 60 ℃, and 30 min stir; successively 4 ml ethyl orthosilicates (TEOS) and 4 ml ammoniacal liquor are added in the above-mentioned mixed liquor; after continue stirring 12 h, above-mentioned reaction product is shifted out, put into vacuum drying chamber after cleaning successively 3 times with alcohol and deionized water; at 60 ℃ of lower dry 24 h, namely get Fe
3O
4/ SiO
2Compound particle;
(3) sol-gel process composite Ti O
2Layer
Take by weighing the Fe of preparation in (2)
3O
4/ SiO
2Compound particle 0.65 g adds 0.5 ml isopropyl titanate in the 60 ml absolute ethyl alcohols, and the hydrochloric acid with 0.1 ml concentration 33% joins in the 40 ml absolute ethyl alcohols again, above-mentioned three is mixed the there-necked flask of transferring to 250 ml, nitrogen protection is heated to 60 ℃, stirs 30 min it is mixed; Deionized water with 9 ml joins in the there-necked flask at last, continue to stir 12 h, be put into 60 ℃ of dryings in the vacuum drying chamber after the above-mentioned reaction product that obtains cleaned 3 times successively with alcohol and deionized water, put into again 550 ℃ of annealing of annealing furnace, 1 h, namely get Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle;
(4) CdS, CdSe quantum dot are modified the Fe3O4/SiO2/TiO2 magnetic nano-particle
Take by weighing the Fe of preparation in (3)
3O
4/ SiO
2/ TiO
2Magnetic nano-particle 0.6 g is dispersed in the 300 ml deionized waters, to the CdCl that wherein adds 15 ml, 0.1 M
2The thiourea solution of the sodium citrate solution of solution, 20 ml, 0.1 M and 30 ml, 0.1 M mixes, and with ammoniacal liquor pH is transferred to about 10.5,65 ℃ of uniform stirring 2 h, centrifugal recovery with alcohol and the above-mentioned reaction product of washed with de-ionized water, namely obtains the Fe that the CdS quantum dot is modified
3O
4/ SiO
2/ TiO
2Magnetic nano-particle;
In the supersaturation sodium sulfite solution that 90 ℃ are dissolved in 0.4 g selenium powder 100 ml, make sodium thiosulfate solution, getting 0.23 g caddy is dissolved in the 100 ml deionized waters, drip 0.5 ml TGA, add gradually again 1.0 M sodium hydroxide solutions, the pH value of solution is reached about 9.0, at this moment solution becomes water white TGA cadmium solution, measure 10 ml TGA cadmiums, add 40 ml deionized waters, add again sodium thiosulfate solution, ultrasonic dispersion 30 min, it is mixed, then solution is transferred in the there-necked flask, add 0.6 g Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle and 0.5 ml mercaptopropionic acid, 60 ℃ of uniform stirring 30 min, centrifugal recovery with alcohol and the above-mentioned reaction product of washed with de-ionized water, namely obtains the Fe that the CdSe quantum dot is modified
3O
4/ SiO
2/ TiO
2Magnetic nano-particle.
As shown in Figure 2, be common Fe
3O
4/ SiO
2/ TiO
2Photochemical catalyst and the Fe that modifies with CdS, CdSe quantum dot
3O
4/ SiO
2/ TiO
2The experimental curve diagram of nano particle photocatalyst degradation of methylene blue under visible light.With methyl orange solution simulative organic wastewater solution, the Fe that checking is modified with CdS, CdSe quantum dot
3O
4/ SiO
2/ TiO
2The photocatalysis characteristic of nano particle.Get the TiO that 0.5 g modifies with CdS, CdSe quantum dot
2/ SiO
2/ Fe
3O
4Nano particle is put into the methyl orange solution of 10 mg/L of 50 ml, stirs, and puts into the ultraviolet lamp box of 25 W, carries out the photocatalysis experiment.
The Fe that CdS, CdSe quantum dot are modified
3O
4/ SiO
2/ TiO
2Nano particle has excellent visible light photocatalysis performance, effectively degrade azo dyestuff methylene blue.As can be seen from Figure 2, through the visible light illumination of 60 min, the Fe that CdS, CdSe quantum dot are modified
3O
4/ SiO
2/ TiO
2Nano particle can be degraded methylene blue solution more than 85%.After degraded was finished, catalyst can reclaim with magnet.After washing, can reuse.
Claims (4)
1. magnetic Fe
3O
4/ SiO
2/ TiO
2/ quantum dot composite Nano photochemical catalyst is characterized in that: this photochemical catalyst adopts Fe
3O
4Nano particle is magnetic nuclear, examines surperficial coated Si O at magnetic
2Protective layer, again composite Ti O
2Catalysis material is modified with CdS, CdSe quantum dot at last.
2. magnetic Fe as claimed in claim 1
3O
4/ SiO
2/ TiO
2The preparation method of/quantum dot composite Nano photochemical catalyst is characterized in that: this photochemical catalyst adopts the synthetic Fe of coprecipitation
3O
4Magnetic nuclear utilizes hydrolysis and the polycondensation reaction of tetraethyl orthosilicate (TEOS) to prepare SiO
2Protective layer is used sol-gel process composite Ti O again
2Layer namely gets Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle is modified Fe with CdS, CdSe quantum dot at last
3O
4/ SiO
2/ TiO
2Nano particle.
3. magnetic Fe according to claim 2
3O
4/ SiO
2/ TiO
2The preparation method of/quantum dot composite Nano photochemical catalyst is characterized in that the method may further comprise the steps:
(1) coprecipitation prepares magnetic nuclear Fe
3O
4Nano particle
Take by weighing 5.44 g FeCl
3With 3 g FeCl
2Be dissolved into respectively in the 50 ml deionized waters, more respectively toward FeCl
3And FeCl
2The aqueous solution in add the Macrogol 2000 of 2 g, stir with glass bar they fully dissolved; The FeCl of dissolve complete
3And FeCl
2The aqueous solution transfer in the there-necked flask, nitrogen protection, 60 ℃ of stirring in water bath add 50 ml ammoniacal liquor again in the there-necked flask, stop after stirring 1.5 h, leave standstill 0.5 h; Clean respectively above-mentioned reaction product 3 times with alcohol and deionized water after reaction is finished, the dilval magnet stronger with magnetic reclaims flushing to above-mentioned reaction product, namely gets Fe
3O
4Nano particle;
(2) hydrolysis and the polycondensation reaction of tetraethyl orthosilicate (TEOS) prepare SiO
2Protective layer
The Fe of preparation in (1)
3O
4Nano particle is dispersed in the mixed solution of ethanol and deionized water, mixed proportion 4:1,120 ml alcohol; 30 ml water; nitrogen protection is heated to 60 ℃, and 30 min stir; successively 4 ml ethyl orthosilicates (TEOS) and 4 ml ammoniacal liquor are added in the above-mentioned mixed liquor; after continue stirring 12 h, above-mentioned reaction product is shifted out, put into vacuum drying chamber after cleaning successively 3 times with alcohol and deionized water; at 60 ℃ of lower dry 24 h, namely get Fe
3O
4/ SiO
2Compound particle;
(3) sol-gel process composite Ti O
2Layer
Take by weighing the Fe of preparation in (2)
3O
4/ SiO
2Compound particle 0.65 g adds 0.5 ml isopropyl titanate in the 60 ml absolute ethyl alcohols, and the hydrochloric acid with 0.1 ml concentration 33% joins in the 40 ml absolute ethyl alcohols again, above-mentioned three is mixed the there-necked flask of transferring to 250 ml, nitrogen protection is heated to 60 ℃, stirs 30 min it is mixed; Deionized water with 9 ml joins in the there-necked flask at last, continue to stir 12 h, is put into 60 ℃ of dryings in the vacuum drying chamber after above-mentioned reaction product is cleaned 3 times successively with alcohol and deionized water, puts into 550 ℃ of annealing furnaces, 1 h that anneals again, and namely gets Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle;
(4) CdS, CdSe quantum dot are modified Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle
Take by weighing the Fe of preparation in (3)
3O
4/ SiO
2/ TiO
2Magnetic nano-particle 0.6 g is dispersed in the 300 ml deionized waters, to the CdCl that wherein adds 15 ml, 0.1 mol/L
2The thiourea solution of the sodium citrate solution of solution, 20 ml, 0.1 mol/L and 30 ml, 0.1 mol/L, mix, with ammoniacal liquor pH is transferred to about 10.5,65 ℃ of uniform stirring 2 h, centrifugal recovery, with alcohol and the above-mentioned reaction product of washed with de-ionized water, namely obtain the Fe that the CdS quantum dot is modified
3O
4/ SiO
2/ TiO
2Magnetic nano-particle; In the supersaturation sodium sulfite solution that 90 ℃ are dissolved in 0.4 g selenium powder 100 ml, make sodium thiosulfate solution, getting 0.23 g caddy is dissolved in the 100 ml deionized waters, drip the 0.5ml TGA, add gradually again 1.0 M sodium hydroxide solutions, the pH value of solution is reached about 9.0, at this moment solution becomes water white TGA cadmium solution, measure 10 ml TGA cadmiums, add 40 ml deionized waters, add again sodium thiosulfate solution, ultrasonic dispersion 30 min, it is mixed, then solution is transferred in the there-necked flask, add 0.6 g Fe
3O
4/ SiO
2/ TiO
2Magnetic nano-particle and 0.5ml mercaptopropionic acid, 60 ℃ of uniform stirring 30 min, centrifugal recovery with alcohol and the above-mentioned reaction product of washed with de-ionized water, namely obtains the Fe that the CdSe quantum dot is modified
3O
4/ SiO
2/ TiO
2Magnetic nano-particle.
4. magnetic Fe claimed in claim 1
3O
4/ SiO
2/ TiO
2/ quantum dot composite Nano photochemical catalyst under the irradiation of visible light, the organic macromolecule pollutant in the industrial and agricultural wastewater that can be used for degrading.
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