CN107552082A - A kind of quaternary multifunction magnetic nano composite material and preparation method thereof - Google Patents
A kind of quaternary multifunction magnetic nano composite material and preparation method thereof Download PDFInfo
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- CN107552082A CN107552082A CN201710904838.7A CN201710904838A CN107552082A CN 107552082 A CN107552082 A CN 107552082A CN 201710904838 A CN201710904838 A CN 201710904838A CN 107552082 A CN107552082 A CN 107552082A
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Abstract
The invention discloses a kind of quaternary multifunction magnetic nano composite material and preparation method thereof, including the nano titanium oxide of certain mass component, urea, graphene and ferroso-ferric oxide.The photochemical catalyst that adding ferroso-ferric oxide makes to disperse in solution can be reclaimed under externally-applied magnetic field, realized efficiently separating for photochemical catalyst and water, be easy to recycling for photochemical catalyst, avoid the loss of nano particle；The doping of nitrogen may replace TiO2Lacking oxygen in lattice, Ti N keys or Ti O N keys are formed, significantly increases its responsiveness and photocatalysis effect under visible light；Ferroso-ferric oxide reduces intergranular reunion to a certain extent with titanium dioxide and the compound of graphene, add the spatial joint clearance of composite, be advantageous to the transmission of electroactive component, increase the contact surface of composite and electrolyte component, improve the ability of storage electric charge.The removal effect of organic pollutant degradation is significantly increased at normal temperatures, there is very strong economic value.
Description
Technical field
The present invention relates to a kind of nano composite material, and in particular to a kind of quaternary multifunction magnetic nano composite material and its
Preparation method.
Background technology
Photocatalytic oxidation compared to conventional oxidation method, with it is nontoxic, pollution-free, cost is low, efficiency high, does not produce secondary dirt
The features such as dye, receives significant attention, and titanium dioxide optical catalyst is always the focus of research in recent years.
Under illumination of the energy not less than band-gap energy (anatase 3.2ev), titanium dioxide, which is excited, produces light induced electron,
Electronics is transferred to conduction band from valence band, while respective hole is produced in valence band.The water and oxygen in light induced electron and hole and surface etc.
, can be by most of organic matter permineralization into CO with reference to hydroxyl radical free radical and superoxide radical etc. of generation strong oxidizing property2, H2O and
Inorganic constituents, efficiency high, do not produce secondary pollution.
Although titanium dioxide has many advantages as photochemical catalyst, there is also some shortcomings.On the one hand wider band
Gap can make it to be not more than 365nm ultraviolet excitation, and this is equivalent to only 3%-5% solar energy by effective profit
With；On the other hand, relatively low quantum efficiency makes electron-hole pair easily compound, and research shows about 90% electron-hole pair
Reconfigured after releasing with faster speed, which greatly limits the large-scale application of titanium dioxide.
At present, there has been largely on titania modified report for problem above, wherein nitrogen and graphene is mixed
Miscellaneous is a kind of effective reduction energy gap, the method for improving quantum efficiency, but most of N/TiO at present2/ GO photochemical catalysts are
Powdered, suspended dispersed, is not easily recycled in the solution, is easily lost in.Although there are many support materials partly to solve
Problem is stated, but most of support materials have harmful effect to the photocatalysis performance of photochemical catalyst.
The content of the invention
To solve the deficiencies in the prior art, it is an object of the invention to provide one kind to have strong absorption property, high catalytic property
Energy, high recyclability and quaternary multifunction magnetic nano composite material with visible light catalysis activity and preparation method thereof.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of quaternary multifunction magnetic nano composite material, including the nano titanium oxide of certain mass component, urea, stone
Black alkene and ferroso-ferric oxide.
Above-mentioned nano titanium oxide be powdered, urea be graininess, graphene be individual layer sheet, ferroso-ferric oxide is powder
Last shape.
The mass ratio of above-mentioned graphene and titanium dioxide is 1：18-20.
A kind of preparation method of above-mentioned quaternary multifunction magnetic nano composite material, comprises the following steps：
S1, take a certain amount of graphene to be dissolved in deionized water, ultrasonic disperse, dispersion liquid is made；
S2, a certain amount of nano titanium oxide and urea, ferroso-ferric oxide are taken in mass ratio, while add above-mentioned dispersion liquid
In, ultrasonic mixing is uniform, and mixed liquor is made；
S3, above-mentioned mixed liquor are transferred in autoclave, and a period of time is reacted under vacuum, dry environment；
S4, the above-mentioned reacted mixed liquor of centrifugation, washing precipitate；After repeated centrifugation, washing several times, unreacted is removed
Material, mainly unnecessary urea；
S5, export centrifuge obtained sediment for the last time, after freeze-day with constant temperature, grind into powder, and obtained dark gray powder
Shape N-TiO2-GO/Fe3O4Composite photocatalyst material.
Graphene in above-mentioned steps S1 is 0.05g, and deionized water 100-150ml, the ultrasonic disperse time is 30min.
Titanium dioxide in above-mentioned steps 2 is 0.95g, urea 6-8g, ferroso-ferric oxide 0.2-1.0g；Ultrasonic time
For 1.5-2.5h.
Autoclave in above-mentioned steps S3 has polytetrafluoroethyllining lining, volume 150ml；Reaction temperature be 180 DEG C-
200 DEG C, reaction time 8-12h.
Centrifugal rotational speed is 2000r/s, centrifugation time 4min in above-mentioned steps S4；Number of repetition is 3-5 times.
Titanium dioxide in above-mentioned steps S1 is P25.
The present invention is advantageous in that：
Compared with existing other technologies, magnetic photocatalyst prepared by the present invention is synthesized using one step hydro thermal method, and raw material is easy
, preparation method is simply easily achieved；The photochemical catalyst that the addition of ferroso-ferric oxide makes to disperse in solution can be under externally-applied magnetic field
Reclaimed, realize efficiently separating for photochemical catalyst and water, be easy to recycling for photochemical catalyst, avoid the stream of nano particle
Lose；The doping of nitrogen may replace TiO2Lacking oxygen in lattice, Ti-N keys or Ti-O-N keys are formed, reduce forbidden energy gap energy, swashed
Hair wavelength is extended to visible region by ultraviolet region, significantly increases its responsiveness and photocatalysis effect under visible light
Fruit；Nitrogen-atoms is introduced into graphene, thus it is possible to vary graphene electronic structure, and the band gap of graphene is opened, so as to make it have
Wider application value；Graphene can make excitation wavelength red shift, and its good electronic transmission performance reduces light induced electron-sky
Compound, and its 2600m in cave2/ g specific surface area substantially increases adsorption capacity of the photochemical catalyst to organic matter, after being beneficial to
Continuous light-catalyzed reaction；Ferroso-ferric oxide reduces intergranular group to a certain extent with titanium dioxide and the compound of graphene
It is poly-, the spatial joint clearance of composite is added, these interporal lacunas can provide good electron propagation ducts, be advantageous to electroactive group
The transmission divided, increase the contact surface of composite and electrolyte component, improve the ability of storage electric charge.
It is demonstrated experimentally that photochemical catalyst prepared by the present invention, which has, is better than P25 and N-TiO2- GO absorption property and photocatalysis
Performance, and there is visible light activity, especially the removal effect of organic pollutant degradation is significantly increased at normal temperatures, had very strong
Economic value, there is very strong practicality and wide applicability.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of catalysis material prepared by embodiments of the invention 2；
Fig. 2 is the energy spectrum analysis figure (EDS) of catalysis material prepared by embodiments of the invention 2；
The catalysis material and P25, TIO2/N/GO that Fig. 3 is prepared for embodiments of the invention 2 are under same light source to humic
The removal effect comparison diagram of acid.
Embodiment
Make specific introduce to the present invention below in conjunction with the drawings and specific embodiments.
A kind of quaternary multifunction magnetic nano composite material, mainly by titanium dioxide (P25), urea, graphene and four oxygen
Change three-iron composition；Titanium dioxide (P25) is nanometer powder shape, urea is graininess, graphene is individual layer sheet, ferroso-ferric oxide
To be powdered.
According to the following steps, the quaternary multifunction magnetic nano composite material of the present invention is prepared：
S1, take a certain amount of graphene to be dissolved in deionized water, ultrasonic disperse, dispersion liquid is made；
S2, a certain amount of nano titanium oxide and urea, ferroso-ferric oxide are taken in mass ratio, while add above-mentioned dispersion liquid
In, ultrasonic mixing is uniform, and mixed liquor is made；
S3, above-mentioned mixed liquor are transferred in the autoclave of 150ml polytetrafluoroethyllining linings, in vacuum, dry ring
A period of time is reacted under border；
S4, the above-mentioned reacted mixed liquor of centrifugation, washing precipitate；After repeated centrifugation, washing several times, unreacted is removed
Material；
S5, export centrifuge obtained sediment for the last time, after freeze-day with constant temperature, grind into powder, and obtained dark gray powder
Shape N-TiO2-GO/Fe3O4Composite photocatalyst material.
Accompanying drawing 1 is the scanning electron microscope (SEM) photograph (SEM) of catalysis material prepared by embodiments of the invention 2, as seen from the figure, this hair
Uniformly, there is not the agglomeration of bulky grain, for photocatalysis effect in catalysis material dispersiveness prepared by bright embodiment 2
Performance have positive role.
SEM equipment is Tescan MIRA3.
Fig. 2 is the energy spectrum analysis figure (EDS) of catalysis material prepared by embodiments of the invention 2, as seen from the figure, is gone out in figure
The characteristic peak of existing C, N, O, Ti, Fe element, illustrates that nitrogen, ferroso-ferric oxide, graphene and titanium dioxide successfully adulterate, material system
Standby success.
EDS equipment is oxford X-MAX.
The catalysis material and P25, TIO2/N/GO that Fig. 3 is prepared for embodiments of the invention 2 are under same light source to humic
The removal effect comparison diagram of acid.
FTNG-0.6 is the catalysis material prepared according to embodiment 2.
TNG is to be not added with Fe according to embodiment 23O4Under the conditions of the TiO2/N/GO for preparing.
Humic acid, it is the representative of natural organic matter in water, water environment has negative effect, is the main right of drinking water treatment
As.Bought from Shanghai biochemical technology Co., Ltd of Aladdin company.
Light source is the 365nm ultraviolet light of solidification.
Operating procedure is：
Ultrasound is adsorbed in the dark state, and adsorption reaction continues 30 minutes, and light-catalyzed reaction is shone in 365nm uviol lamps
Penetrate lower stirring to carry out, detected per sub-sampling 4-5ml, sample interval is 10-30 minutes.
Detecting instrument uses UV254 detection method, surveys ultraviolet absorptivity of the solution at 254nm
The use of instrument is ultraviolet-uisible spectrophotometer, model UV-1000, Beijing Pu Xi general finites company.
From accompanying drawing 3, at normal temperatures, FTNG-0.6 catalysis materials prepared by embodiments of the invention 2 are to humic acid
Clearance reached more than 80%.
The clearance of humic acid is significantly increased at normal temperatures compared to P25 and TNG.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, the invention is not limited in any way for above-described embodiment, all to be obtained by the way of equivalent substitution or equivalent transformation
Technical scheme, all fall within protection scope of the present invention.
Claims (9)
1. a kind of quaternary multifunction magnetic nano composite material, it is characterised in that include the nanometer titanium dioxide of certain mass component
Titanium, urea, graphene and ferroso-ferric oxide.
A kind of 2. quaternary multifunction magnetic nano composite material according to claim 1, it is characterised in that the nanometer two
Titanium oxide be powdered, urea be graininess, graphene be individual layer sheet, ferroso-ferric oxide is powdered.
A kind of 3. quaternary multifunction magnetic nano composite material according to claim 1, it is characterised in that the graphene
Mass ratio with titanium dioxide is 1：18-20.
A kind of 4. preparation method of quaternary multifunction magnetic nano composite material according to claim 1, it is characterised in that
Comprise the following steps：
S1, take a certain amount of graphene to be dissolved in deionized water, ultrasonic disperse, dispersion liquid is made；
S2, a certain amount of nano titanium oxide and urea, ferroso-ferric oxide are taken in mass ratio, while add in above-mentioned dispersion liquid,
Ultrasonic mixing is uniform, and mixed liquor is made；
S3, above-mentioned mixed liquor are transferred in autoclave, and a period of time is reacted under vacuum, dry environment；
S4, the above-mentioned reacted mixed liquor of centrifugation, washing precipitate；After repeated centrifugation, washing several times, unreacted reactant is removed
Matter；
S5, export centrifuge obtained sediment for the last time, after freeze-day with constant temperature, grind into powder, and obtained quaternary multifunction magnetic
Nano composite material.
A kind of 5. preparation method of quaternary multifunction magnetic nano composite material according to claim 4, it is characterised in that
Graphene in the step S1 is 0.05g, and deionized water 100-150ml, the ultrasonic disperse time is 30min.
A kind of 6. preparation method of quaternary multifunction magnetic nano composite material according to claim 4, it is characterised in that
Titanium dioxide in the step 2 is 0.95g, urea 6-8g, ferroso-ferric oxide 0.2-1.0g；Ultrasonic time is 1.5-
2.5h。
A kind of 7. preparation method of quaternary multifunction magnetic nano composite material according to claim 4, it is characterised in that
Autoclave in the step S3 has polytetrafluoroethyllining lining, volume 150ml；Reaction temperature is 180 DEG C -200 DEG C, instead
It is 8-12h between seasonable.
A kind of 8. preparation method of quaternary multifunction magnetic nano composite material according to claim 4, it is characterised in that
Centrifugal rotational speed is 2000r/s, centrifugation time 4min in the step S4；Number of repetition is 3-5 times.
A kind of 9. preparation method of quaternary multifunction magnetic nano composite material according to claim 4, it is characterised in that
Titanium dioxide in the step S1 is P25.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588946A (en) * | 2022-01-13 | 2022-06-07 | 河海大学 | Preparation method and application of ferrous iron-doped Fe-MOF-based composite material |
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| CN101773841A (en) * | 2010-01-29 | 2010-07-14 | 苏州科技学院 | Photocatalyst for water treatment |
| CN103816869A (en) * | 2014-03-11 | 2014-05-28 | 济南大学 | Preparation method for magnetic mesoporous titanium dioxide / graphene oxide adsorbing material |
| CN105749915A (en) * | 2015-11-12 | 2016-07-13 | 天津工业大学 | Method for preparing magnetic graphene-based titanium dioxide composite |
| CN106621833A (en) * | 2016-12-19 | 2017-05-10 | 河海大学 | Preparation method of ultrafiltration membrane with anti-fouling performance enhanced by nitrogen-doped graphene oxide/TiO2 composite particles |
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| CN114588946A (en) * | 2022-01-13 | 2022-06-07 | 河海大学 | Preparation method and application of ferrous iron-doped Fe-MOF-based composite material |
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Application publication date: 20180109 |