CN109806876A - A kind of magnetism ZnFe2O4/ graphene nano composite photo-catalyst and the preparation method and application thereof - Google Patents
A kind of magnetism ZnFe2O4/ graphene nano composite photo-catalyst and the preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kind of magnetism ZnFe2O4/ graphene nano composite photo-catalyst and the preparation method and application thereof.The present invention is using diethylene glycol as solvent, using polyethylene glycol as pattern controlling agent, lauryl sodium sulfate is dispersing agent, it is hydrolyzed using sodium acetate and alkaline condition is provided, so that zinc ferrite equably nucleating growth on the surface of graphene, zinc ferrite crystal can also prevent the unordered stacking between stratiform graphene from reuniting simultaneously, to improve the surface area of composite material.Compared to single ZnFe2O4Photochemical catalyst, this composite material specific surface area with higher and excellent electron conduction；Enough reaction active sites can be both provided for light-catalyzed reaction, can also promote the migration of photo-generated carrier with separate so that ZnFe2O4/ graphene nano composite photo-catalyst shows excellent visible light photocatalysis ability.
Description
Technical field
The invention belongs to nanocomposite preparation fields, and in particular to a kind of magnetism ZnFe2O4/ graphene nano is compound
Photochemical catalyst and the preparation method and application thereof.
Background technique
As population increase and industrial development, problem of environmental pollution become increasingly conspicuous.With the continuous development of textile industry, print
Dye waste water has become the problem of environmental pollution that currently can not ignore, and has been to be concerned by more and more people.
Organic dyestuff is the maximum a class of pollutant that weaving, dyeing and other industrial process are discharged into environment, to ring
Border and human health produce significant damage.Therefore, these noxious pollutants are effectively removed from water body is the task of top priority.It passes
The physics and chemical method of system are difficult to completely remove or degrade the organic pollutant in water body, however, as a kind of advanced oxygen
Change technology, homogeneous/heterogeneous photocatalysis technology due to its degradation thoroughly, material preparation method it is simple, low in cost and using too
The advantages that sunlight, has irreplaceable role in polluted water purification field.
So far, TiO2Semiconductor material is a kind of catalysis material studied the most extensively and profoundly, has height
The advantages that photoelectric conversion and stability of effect are good.But titanium dioxide semiconductor forbidden bandwidth is big (3.2eV), it can only be by ultraviolet light
Excitation, and be difficult to recycle from dispersion, cause huge waste.So researchers are dedicated to exploitation and are received using magnetism
Rice grain carries out the photocatalysis oxidation technique of environment remediation, because magnetic nanoparticle can be recycled by magnetic field, is conducive to big
The industrial application of scale.Wherein, the ferrite semiconductor soft magnetic materials of spinel structure has narrow forbidden bandwidth, in light
Electricity conversion aspect possesses huge potentiality.
ZnFe2O4Semiconductor is a kind of important soft magnetic ferrite, its forbidden bandwidth is about 1.9eV, so
ZnFe2O4Electronics in semiconductor valence band, to transit on conduction band, can generate photo-generated carrier electricity by excited by visible light
Photoelectric conversion is completed in son and hole.Due to ZnFe2O4The valence band potential of semiconductor is lower, and photo-generated carrier recombination rate is very
Height causes its quantum efficiency low, so ZnFe2O4Semiconductor is seldom directly used as a kind of photochemical catalyst.Two-dimensional Carbon nanometer
Material graphene has the characteristics that surface area is big and electron conduction is excellent, and its valence band current potential ratio ZnFe2O4Will just, so
It can be used as ZnFe2O4Nanocrystalline carrier constructs a kind of ZnFe2O4/ graphene nano heterojunction structure, to make up single
ZnFe2O4The not high disadvantage of semiconductive light active.
Recently in the case where photochemical catalyst recycles and improves visible light, catalytic activity these two aspects forefathers be there has been
Working foundation.It is not present if doing film photocatalyst and is difficult to the problem of recycling, application No. is 200810207900.8 patent reports
A kind of preparation method of load type titanium dioxide photocatalytic film in road.By load technology, catalyst granules had both been avoided certainly
The reunion of body, and facilitate recycling；For another example it by the way that photochemical catalyst to be coated to the surface of magnetic material, forms magnetic material and makees
Core, photochemical catalyst make the structure of shell, and the purpose of separation and recovery is realized by magnetic field.Such as application No. is 200910117405 patents
It reports TiO through sol-gal process2It is coated to magnetic Fe3O4Surface forms magnetic particle and makees core, TiO2Make the photocatalysis of shell
Agent can realize the recycling of photochemical catalyst by magnetic field in this way.There is visible light-responded photochemical catalyst also to have attracted very for preparation
The sight of more researchers, such as application No. is 201010203049.9 patent report one kind can magnetic separation titanium dioxide visible light
The preparation method of catalyst, which can realize separation and recovery using externally-applied magnetic field, and have certain visible light
Catalytic activity.
But all there are many defects in above-mentioned several method, such as do supported composite photocatalyst, though to a certain extent can
Separation recovery efficiencies are improved, but will lead to active reduction due to the presence of carrier, or with the object insufficient contact that is degraded；For another example
TiO2The nucleocapsid of base can the preparation process of Magneto separate photochemical catalyst unavoidably need high-temperature calcination, can increase in industrial scale applications
Add many energy consumptions, and wants high many for the cost of titanium salt and zinc salt.
At present both at home and abroad to ZnFe2O4Magnetic property, in terms of have more paper publishings, but in photocatalysis
Research in terms of degradable organic pollutant is also at the early-stage, especially with ZnFe2O4/ graphene photocatalytic degradation of dye waste water
Research be rarely reported.
Summary of the invention
For existing TiO2The visible light utilization efficiency of photochemical catalyst is low, and expendable disadvantage, the present invention provides a kind of system
Standby magnetic ZnFe at low cost, photocatalysis performance is good2O4/ graphene nano composite photo-catalyst and preparation method thereof.
Realize technical solution of the invention are as follows: a kind of magnetism ZnFe2O4/ graphene nano composite photo-catalyst, it is special
Sign is that the composite photo-catalyst is made of basis material graphene and zinc ferrous acid nanocrystalline body, wherein carrier material graphene
Mass ratio with zinc ferrite is 1: 3~9, and the crystal structure of zinc ferrite is cube normal spinel structure.
A kind of magnetism ZnFe2O4The preparation method of/graphene nano composite photo-catalyst, includes the following steps:
1): graphene oxide being stirred by ultrasonic to dispersion in diethylene glycol, obtains finely dispersed graphene oxide dispersion, oxygen
The concentration of graphite alkene is 1~3mg/L, and the ultrasonic agitation time is 20~60min；
2): polyethylene glycol is added into the graphene oxide dispersion that step 1) obtains, is sufficiently mixed to obtain mixed liquor A；
3): taking Fe (NO3)3·9H2O and Zn (NO3)2·6H2O stirring and dissolving obtains the clear solution B of yellow in diethylene glycol,
Mixing time is 20~60min；
4): the solution B that step 3) is obtained is slowly added dropwise in the mixed liquor A obtained to step 2), stirs evenly, and obtains mixing molten
Liquid C；
5): it takes sodium acetate and lauryl sodium sulfate to be dissolved in deionized water, and is added dropwise in the mixed solution C that step 4) obtains,
Last mixed solution is transferred to autoclave and carries out solvent-thermal process reaction, obtains crude product；
6): the crude product that step 5) obtains makes annealing treatment under nitrogen atmosphere, obtains after centrifugation, washing and vacuum drying
ZnFe2O4/ graphene nano composite photo-catalyst.
In the technical scheme, use diethylene glycol for solvent and reducing agent, at reaction conditions to graphene oxide into
Row reduction, using polyethylene glycol as pattern controlling agent, lauryl sodium sulfate is dispersing agent, and sodium acetate is nucleation controlling agent, in iron
While sour zinc nucleating growth, make its uniform deposition on the surface of graphene, its growth of reuniting is prevented, to obtain single dispersing particle diameter
Ferrous acid zinc nanoparticles；Low-temperature annealing is handled so that zinc ferrite crystal is more regular, also enhances ferrous acid zinc nano material
It is magnetic.
Preferably, the volume ratio of polyethylene glycol described in step 2) and diethylene glycol is 1: 60~1: 15.
Preferably, Fe (NO described in step 3)3)3·9H2O and Zn (NO3)2·6H2O molar ratio is 2: 1； Fe
(NO3)3·9H2Concentration of the O in diethylene glycol is 30~85g/L.
Preferably, in step 5), the sodium acetate and Fe (NO3)3Molar ratio be 20~50: 1.
Preferably, lauryl sodium sulfate described in step 5) and Fe (NO3)3Molar ratio be 0.3~1.25: 1.
Preferably, the mass ratio of the sodium acetate and deionized water is 0.35~0.5: 1 in step 5).
Preferably, the solvent thermal reaction temperature is 130~200 DEG C in step 5), the solvent thermal reaction time is 8
~72h.
Preferably, annealing temperature described in step 6) is 200~500 DEG C, 0.5~3h of time is made annealing treatment.
Magnetism ZnFe prepared by the present invention2O4/ graphene nano composite photo-catalyst for waste water from dyestuff, dyeing waste water and
The photocatalysis green Cress application of wastewater from chemical industry.
Compared with prior art, the present invention the present invention has the advantage that (1) present invention uses solvent-thermal process and low temperature
Annealing technology combines, and synthesis technology is easy, not high to equipment requirement, is conducive to large-scale production；(2) diethyl two is used
Alcohol is solvent and reducing agent, is restored at reaction conditions to graphene oxide (GO), using polyethylene glycol as pattern controlling agent
(PEG), lauryl sodium sulfate (SDS) is dispersing agent, and sodium acetate is nucleation controlling agent, and water can occur in aqueous solution for sodium acetate
Solution forms a kind of very weak alkali, while ferrous acid zinc precursor nucleating growth, makes its slow uniform deposition on the surface of graphene,
Its growth of reuniting is prevented, to obtain the ferrous acid zinc nanoparticles of single dispersing particle diameter；It is as follows more particularly to key reaction:
It is stirred: diethylene glycol+GO → ultra-dispersed GO- diethylene glycol dispersion liquid
Electrostatic Absorption: SDS+GO → SDS-GO (negatively charged)
Zn2++Fe3++SDS-GO→Zn2+Fe3+- SDS-GO (Electrostatic Absorption)
Sodium acetate hydrolysis: CH3COONa+H2O→CH3COOH+OH-+Na+
Ferrous acid zinc precursor is formed: Zn2+Fe3+-SDS-GO+OH-→ZnFeOH-SDS-GO
Solvent thermal reaction: ZnFeOH-SDS-GO+PEG+ diethylene glycol → ZnFe2O4/rGO
Calcined crystalline: ZnFe2O4/rGO→ZnFe2O4/ graphene nanocomposite material.
(3) low-temperature annealing is handled so that zinc ferrite crystal is more regular, also enhances the magnetism of ferrous acid zinc nano material；This
Sample has obtained ZnFe2O4/ graphene nanocomposite material not only has good magnetic responsiveness, but also there is excellent visible light light to urge
Change activity.
Detailed description of the invention
Attached drawing 1 is ZnFe of the present invention2O4/ graphene nano composite photo-catalyst preparation flow schematic diagram.
Attached drawing 2 is 1 gained ZnFe of the embodiment of the present invention2O4/ graphene nano composite photo-catalyst is sub- for Visible Light Induced Photocatalytic
The concentration curve of methyl blue (MB).
Attached drawing 3 is 1 gained ZnFe of the embodiment of the present invention2O4The TEM photo of/graphene nano composite photocatalyst.
Attached drawing 4 is 1 gained ZnFe of the embodiment of the present invention2O4The XRD spectra of/graphene nano composite photo-catalyst.
Specific embodiment
Below mainly in combination with attached drawing 1 and specific embodiment to magnetic ZnFe2O4/ graphene nano composite photo-catalyst and its
Preparation method is described in further detail with application.
Embodiment 1
(1) it weighs 60mg graphene oxide to be added in the diethylene glycol of 60mL, 30min is stirred by ultrasonic, is uniformly dispersed
Liquid；
(2) 2mL polyethylene glycol is added into graphene oxide dispersion, obtains mixed solution A；
(3) 0.808gFe (NO is weighed3)3With 0.297gZn (NO3)2It is dissolved in 20mL diethylene glycol, sufficiently dissolution obtains uniform gold
Belong to salting liquid B；
(4) metal salt solution B is slowly dropped in graphene oxide mixed solution A, 30min is sufficiently stirred, obtain mixing molten
Liquid C；
(5) it weighs 3.5g sodium acetate and 0.58g lauryl sodium sulfate is dissolved in 10mL deionized water, and be added drop-wise to above-mentioned mixing
In solution C, mixed solution is transferred to 180 DEG C of reaction 10h of autoclave；
(6) product, in the lower 200 DEG C of annealings 2h of nitrogen atmosphere, obtains magnetism after centrifugation, washing and vacuum drying
ZnFe2O4/ graphene nano composite photo-catalyst.
As shown in degradation effect comparison diagram of Fig. 2 sample to methylene blue, single ZnFe is compared2O4, magnetic ZnFe2O4/ stone
Black alkene nano composite photo-catalyst shows excellent photocatalysis performance；Shown in the TEM figure of 1 sample of Fig. 3 embodiment, nanometer in figure
ZnFe2O4It is relatively uniform to be distributed on graphene, without obvious nanometer Zn Fe2O4Reunite, forms magnetism ZnFe2O4/ graphene is received
Rice composite photo-catalyst structure, and can see ZnFe from the XRD spectrum of Fig. 42The characteristic diffraction peak of O4, it is possible to determine
ZnFe2O4/ graphene nanocomposite material is successfully prepared.
Result is tested and analyzed by the MB degradation rate of 1 sample of embodiment in Fig. 2 it is found that embodiment 1 is close to MB degradation rate
100%, illustrate that embodiment sample has preferably Photocatalytic Degradation Property.
Embodiment 2
(1) it weighs 53.5mg graphene oxide to be distributed in 40mL diethylene glycol, 20min is stirred by ultrasonic, is uniformly dispersed
Liquid；
(2) 2mL polyethylene glycol is added into graphene oxide dispersion, obtains mixed solution A；
(3) 1.616g Fe (NO is weighed3)3·9H2O and 0.594g Zn (NO3)2·6H2O is dissolved in 20mL diethylene glycol and obtains
Uniform metal salt solution B；
(4) metal salt solution is slowly dropped in the resulting graphene oxide liquid mixture A of (2) step, 60min is sufficiently stirred,
Obtain mixed solution C；
(5) it weighs 6.56g sodium acetate and 0.3456g lauryl sodium sulfate is dissolved in 15mL deionized water, and be added drop-wise to above-mentioned
In mixed solution C, mixed solution is transferred in autoclave, 200 DEG C of reaction 8h；
(6) product, with the lower 500 DEG C of annealings 0.5h of nitrogen atmosphere, obtains magnetism after centrifugation, washing and vacuum drying
ZnFe2O4/ graphene nano composite photo-catalyst.
Embodiment 3
(1) it weighs 60mg graphene oxide to be distributed in 20mL diethylene glycol, 60min is stirred by ultrasonic, obtains uniform dispersion liquid；
(2) 1.33mL polyethylene glycol is added into graphene oxide dispersion, obtains mixed solution A；
(3) 0.604gFe (NO is weighed3)3·9H2O and 0.222gZn (NO3)2·6H2O, which is dissolved in 20mL diethylene glycol, to be obtained
One metal salt solution B；
(4) metal salt solution is slowly dropped in the resulting graphene oxide liquid mixture A of (2) step, 20min is sufficiently stirred,
Obtain mixed solution C；
(5) it weighs 6.12g sodium acetate and 0.538g lauryl sodium sulfate is dissolved in 12.24mL deionized water, and be added drop-wise to
It states in mixed solution C, mixed solution is transferred in autoclave, 130 DEG C of reaction 72h；
(6) product, with the lower 250 DEG C of annealings 3h of nitrogen atmosphere, obtains magnetism after centrifugation, washing and vacuum drying
ZnFe2O4/ graphene nano composite photo-catalyst.
Claims (10)
1. a kind of magnetism ZnFe2O4/ graphene nano composite photo-catalyst, which is characterized in that the composite photo-catalyst is by carrier
Material graphene and zinc ferrous acid nanocrystalline body form, wherein graphene and ZnFe2O4Mass ratio be 1: 3~9, the crystalline substance of zinc ferrite
Body structure is cube normal spinel structure.
2. a kind of magnetism ZnFe as described in claim 12O4The preparation method of/graphene nano composite photo-catalyst, feature
It is, the preparation method includes the following steps:
1): graphene oxide being stirred by ultrasonic to dispersion in diethylene glycol, obtains finely dispersed graphene oxide dispersion, oxygen
The concentration of graphite alkene is 1~3mg/L, and the ultrasonic agitation time is 20~60min；
2): polyethylene glycol is added into the graphene oxide dispersion that step 1) obtains, is sufficiently mixed to obtain mixed liquor A；
3): taking Fe (NO3)3·9H2O and Zn (NO3)2·6H2O stirring and dissolving obtains the clear solution B of yellow in diethylene glycol,
Mixing time is 20~60min；
4): the solution B that step 3) is obtained is slowly added dropwise in the mixed liquor A obtained to step 2), stirs evenly, and obtains mixing molten
Liquid C；
5): it takes sodium acetate and lauryl sodium sulfate to be dissolved in deionized water, and is added dropwise in the mixed solution C that step 4) obtains,
Last mixed solution is transferred to autoclave and carries out solvent-thermal process reaction, obtains crude product；
6): the crude product that step 5) obtains makes annealing treatment under nitrogen atmosphere, obtains after centrifugation, washing and vacuum drying
ZnFe2O4/ graphene nano composite photo-catalyst.
3. a kind of magnetism ZnFe according to claim 22O4The preparation method of/graphene nano composite photo-catalyst, it is special
Sign is that the volume ratio of polyethylene glycol described in step 2) and diethylene glycol is 1: 60~1: 15.
4. a kind of magnetism ZnFe according to claim 22O4The preparation method of/graphene nano composite photo-catalyst, it is special
Sign is, Fe (NO described in step 3)3)3·9H2O and Zn (NO3)2·6H2O molar ratio is 2: 1；Fe(NO3)3·9H2O exists
Concentration in diethylene glycol is 30~85g/L.
5. a kind of magnetism ZnFe according to claim 22O4The preparation method of/graphene nano composite photo-catalyst, it is special
Sign is, in step 5), the sodium acetate and Fe (NO3)3Molar ratio be 20~50: 1.
6. a kind of magnetism ZnFe according to claim 22O4The preparation method of/graphene nano composite photo-catalyst, it is special
Sign is, lauryl sodium sulfate described in step 5) and Fe (NO3)3Molar ratio be 0.3~1.25: 1.
7. a kind of magnetism ZnFe according to claim 22O4The preparation method of/graphene nano composite photo-catalyst, it is special
Sign is, in step 5), the mass ratio of the sodium acetate and deionized water is 0.35~0.5: 1.
8. a kind of magnetism ZnFe according to claim 22O4The preparation method of/graphene nano composite photo-catalyst, it is special
Sign is, in step 5), the solvent thermal reaction temperature is 130~200 DEG C, and the solvent thermal reaction time is 8~72h.
9. a kind of magnetism ZnFe according to claim 22O4The preparation method of/graphene nano composite photo-catalyst, it is special
Sign is that annealing temperature described in step 6) is 200~500 DEG C, makes annealing treatment 0.5~3h of time.
10. a kind of magnetism ZnFe as described in claim 12O4/ graphene nano composite photo-catalyst is in waste water from dyestuff, printing and dyeing
The application of the photocatalysis green Cress of waste water and wastewater from chemical industry.
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