CN104588065A - Rare-earth composite g-C3N4 graphene photocatalyst and preparation method thereof - Google Patents
Rare-earth composite g-C3N4 graphene photocatalyst and preparation method thereof Download PDFInfo
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- CN104588065A CN104588065A CN201510063091.8A CN201510063091A CN104588065A CN 104588065 A CN104588065 A CN 104588065A CN 201510063091 A CN201510063091 A CN 201510063091A CN 104588065 A CN104588065 A CN 104588065A
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Abstract
The invention relates to a photocatalytic material for treating organic pollutants in water and a preparation method thereof. The photocatalytic material is formed by compounding layered semiconductor g-C3N4 graphene material with visible-light response and beta-NaYF4: Yb<3+>, Tm<3+> rare-earth nanoparticles with upconversion performance, wherein the beta-NaYF4: Yb<3+>, Tm<3+> rare-earth nanoparticles are uniformly distributed on the surface of the g-C3N4 graphene material, and a composite photocatalytic material with heterostructure and near-infrared light response is formed. According to successful compounding of the rare-earth nanoparticles, the g-C3N4 graphene can absorb visible light emitted by the rare earth through upconversion, so that the infrared light response is realized. The catalyst has excellent catalytic activity under near-infrared light, the concentration of the organic pollutants in the water can be rapidly reduced in a short time, and finally the pollutants can be almost completely degraded. The preparation method is simple and feasible, and the catalyst can be conveniently recycled and has wide application prospects.
Description
Technical field
The invention belongs to a kind of catalysis material and preparation method thereof, specifically a kind of rare earth compound g-C
3n
4class graphene photo-catalyst and preparation method thereof, this catalyst can be activated by near infrared light, the organic pollution in catalytic degradation water.
Background technology
Since Fujishima in 1972 has found that titanium dioxide can since decomposition water under action of ultraviolet light, Photocatalitic Technique of Semiconductor is progressively emerging to grow up.Semiconductor light-catalyst is as the environmentally friendly catalysis new technology of one, can not only oxidative degradation organic pollution, make the material permineralization of a lot of bio-refractory, and itself is nontoxic, stable performance, do not produce that secondary pollution, cost are low, less energy consumption, reaction condition gentle, operate simple and easy, the recyclable advantage such as to recycle, become the focus of countries in the world scholar's research.
Most of semiconductor light-catalyst can only respond ultraviolet light or visible ray, and the titanium dioxide as being widely used in photocatalysis field at present can only respond ultraviolet light, metal-free g-C
3n
4class graphene semiconductor also can only responding to visible light.Although Chinese scholars has carried out a large amount of study on the modification to semiconductor light-catalyst, example photoresponse being extended to infrared light region is very limited, and its utilization ratio has much room for improvement.Near infrared light about 44% in solar energy, this part infrared light is not utilized effectively, and greatly reduces the utilization rate of photochemical catalyst to solar energy, thus affects its photocatalysis efficiency.
Rare earth up-conversion luminescent material is as a kind of material that lower energy photon can be converted to high-energy photon, and we are by itself and g-C
3n
4class Graphene, by certain combination compound, utilizes the characteristic of up-conversion luminescent material, absorbs near infrared light, is sent the visible ray of short wavelength by up conversion, makes semiconductor indirect utilization near infrared light, improves the comprehensive utilization ratio to solar energy.
Summary of the invention
The object of the present invention is to provide a kind of rare earth compound g-C
3n
4class Graphene catalysis material and preparation method thereof, obtained composite photo-catalyst can respond near infrared light, improve the utilization ratio near infrared light region in Photocatalitic Technique of Semiconductor field, thus improve it to solar energy utilization rate, and be applied to field of environmental improvement.
The technical scheme that the present invention takes is:
A kind of rare earth compound g-C
3n
4class graphene photo-catalyst, is characterized in that this photochemical catalyst is β-NaYF
4: Yb
3+, Tm
3+nano particle and g-C
3n
4class grapheme material compound forms, β-NaYF
4: Yb
3+, Tm
3+nano particle is evenly distributed in the heterojunction structure that stratiform class graphene nanometer sheet is formed, and preparation method's step is:
(1) 0.1 g Y is taken
2o
3in three-necked bottle, toward wherein adding 10 ml trifluoroacetic acids and 10 ml deionized waters, again three-necked bottle is placed in the oil bath pan of 75 DEG C, add hot reflux 6 h under magnetic stirring, until the white solution bleach clarification of muddiness, finally taking-up is put into 80 DEG C of oven for drying and just can be obtained (CF a whole night
3cOO)
3y powdered product.In addition, (CF has been prepared in the same way
3cOO)
3yb and (CF
3cOO)
3tm powder;
(2) trifluoroacetate (Y that 1 mmol step (1) prepares is taken
3+: Yb
3+: Tm
3+mol ratio be 0.78:0.2:0.02) in 100 ml three-necked bottles, then add 2 mmol sodium trifluoroacetates in wherein, then add oleic acid, 1-octadecylene and oleyl amine that mol ratio is 8:10:5 successively.Under nitrogen protection atmosphere, the above-mentioned three-necked bottle magnetic agitation in the oil bath pan of 110 DEG C having added various reaction reagent is heated 30 min, until mixed solution becomes clarification, obtain solution A;
(3) under nitrogen protection atmosphere, by solution A continuous heating 1 h at 330 DEG C, after question response terminates, be cooled to room temperature, with deionized water and time rear drying of absolute ethyl alcohol centrifuge washing number, just can obtain up-conversion luminescence nano particle β-NaYF
4: Yb
3+, Tm
3+.
(4) take melamine powder to add and have in the semi-enclosed porcelain crucible of lid, be then the heating rate to 500 DEG C of 10 DEG C/min with firing rate and continue 2 h.Then carry out further deammoniation process again, be namely heated to 520 DEG C, and continue 2 h.Finally cool room temperature, grind calcined after material just can obtain yellow g-C
3n
4powder.
(5) g-C that step (4) has prepared is taken
3n
4semiconductor powder adds in the beaker of the methanol solution be equipped with, and after then beaker being put into the ultrasonic 30min of ultrasonic device, then adds the β NaYF that step (3) prepared inside
4: Yb
3+, Tm
3+, then beaker is placed magnetic agitation 24h in ventilating kitchen, until the methanol solution in beaker all evaporates dry, finally obtained product is calcined at 250 DEG C 1h and just obtain near-infrared composite photo-catalyst.Up-conversion luminescence nano particle β-NaYF
4: Yb
3+, Tm
3+mass ratio near infrared light composite photo-catalyst is 5% ~ 50% adjustable.
The photoresponse scope of semiconductor light-catalyst can be extended near infrared light by the present invention indirectly, up-conversion luminescence nano particle β NaYF
4: Yb
3+, Tm
3+can the near infrared light of absorption be converted to visible ray, and then vitalizing semiconductor g-C
3n
4and there is photocatalysis.This is used for semiconductor light-catalyst field near infrared light provides a kind of new Technology Ways, and for solving, day by day serious problem of environmental pollution is significant.
Accompanying drawing explanation
Fig. 1 is the rare-earth beta-NaYF obtained by embodiment 1
4: Yb
3+, Tm
3+nano particle figure (transmission electron microscope photo);
Fig. 2 is the near-infrared composite photo-catalyst β-NaYF obtained by embodiment 3
4: Yb
3+, Tm
3+/ g-C
3n
4(transmission electron microscope photo);
Fig. 3 is by the β-NaYF prepared by embodiment 3
4: Yb
3+, Tm
3+quality is the photocatalytic degradation curve map of near-infrared composite photo-catalyst to organic dyestuff methylene blue under 980nm near-infrared laser irradiates of 15%.
Detailed description of the invention
Illustrate content of the present invention further below in conjunction with specific embodiment, but these embodiments do not limit the scope of the invention.
Embodiment (one)
Up-conversion luminescence nano particle β-NaYF
4: Yb
3+, Tm
3+preparation process as follows:
(1) 0.1 g Y is taken
2o
3in three-necked bottle, toward wherein adding 10 ml deionized waters and 10 ml CF
3cOOH solution, then oil bath pan three-necked bottle being placed in 75 DEG C, add hot reflux 6 h under magnetic stirring, until the white solution bleach clarification of muddiness, finally taking-up is put into 80 DEG C of oven for drying and just can be obtained (CF a whole night
3cOO)
3y powdered product.In addition, (CF has been prepared in the same way
3cOO)
3yb and (CF
3cOO)
3tm powder.
(2) the trifluoroacetate 0.78 mmol (CF that step (1) prepares is taken
3cOO)
3y, 0.2 mmol (CF
3cOO)
3yb and 0.02 mmol (CF
3cOO)
3tm in 100 ml three-necked bottles, then adds 2 mmol sodium trifluoroacetates in wherein, then adds 10 mmol 1-octadecylenes, 8 mmol oleic acid and 5 mmol oleyl amines successively.
Under nitrogen protection atmosphere, the above-mentioned three-necked bottle magnetic agitation in the oil bath pan of 110 DEG C having added various reaction reagent is heated 30 min, until mixed solution becomes clarification, obtain solution A.Object is exactly be the water in removing solution and oxygen, for follow-up reaction is laid the groundwork.
(3) again solution A is heated to 330 DEG C, equally continuous heating 1 h under nitrogen protection atmosphere, until reaction terminates, is cooled to room temperature.Finally use ultra-pure water and absolute ethyl alcohol 1:1 mixed solution through desk centrifuge 104 rpm/10 min centrifuge washing 3 ~ 5 times.After thing to be precipitated is cleaned, put into vacuum drying chamber 80 DEG C of dryings one and become the β-NaYF that can obtain having up-conversion luminescence property night
4: Yb
3+, Tm
3+nano particle (Fig. 1).
Embodiment (two)
Semi-conducting material g-C
3n
4preparation process as follows:
Take 5g melamine powder to add and have in the semi-enclosed porcelain crucible of lid, be then the heating rate to 500 DEG C of 10 DEG C/min with firing rate and continue 2h.Then carry out further deammoniation process again, be namely heated to 520 DEG C, and continue 2h.Finally cool room temperature, grind calcined after material just can obtain yellow g-C
3n
4powder.
Embodiment (three)
β-NaYF
4: Yb
3+, Tm
3+quality is the near-infrared composite photo-catalyst β-NaYF of 15%
4: Yb
3+, Tm
3+/ g-C
3n
4preparation process as follows:
Take the g-C that 0.283 g embodiment two has prepared
3n
4semiconductor powder adds in the beaker of the methanol solution that 150 mL are housed, and after then beaker being put into ultrasonic 30 min of ultrasonic device, then adds the β-NaYF that 0.05 g embodiment one prepared inside
4: Yb
3+, Tm
3+, then beaker is placed magnetic agitation 24h in ventilating kitchen, until the methanol solution in beaker all evaporates dry, then moves in Muffle furnace and calcine 1h at 250 DEG C, just can obtain the near-infrared composite photo-catalyst β-NaYF with heterojunction structure
4: Yb
3+, Tm
3+/ g-C
3n
4(Fig. 2).
Embodiment (four)
β-NaYF
4: Yb
3+, Tm
3+quality is the near-infrared composite photo-catalyst β-NaYF of 15%
4: Yb
3+, Tm
3+/ g-C
3n
4under 980nm near-infrared laser irradiates, the specific experiment step of degradating organic dye methylene blue is as follows:
Be scattered in by near-infrared composite photo-catalyst prepared by 1 mg embodiment three in the quartzy centrifuge tube of the methylene blue solution (concentration is 15ppm) that 0.5 ml is housed, camera bellows 2 h that the dispersion liquid mixed is placed in lucifuge makes it reach adsorption equilibrium, then the near infrared light semiconductor diode laser being 980 nm with emission wavelength in camera bellows irradiates reaction system for light source (power output is for 1W), according to the time interval of 2h, from quartzy centrifuge tube, 0.3mL reactant liquor is got in 2mL centrifuge tube with 1mL syringe, with 12000 rpm rotating speed high speed centrifugation 10 min, get supernatant 0.25mL in micro-quartz colorimetric utensil, its absorbance (refunded after having surveyed again and continue illumination to quartzy centrifuge tube) is surveyed in spectrophotometer, thus under obtaining each time period near-infrared composite photo-catalyst to the photocatalytic degradation effect figure of methylene blue.
Fig. 3 is prepared β-NaYF
4: Yb
3+, Tm
3+quality is the photocatalytic degradation curve map of near-infrared composite photo-catalyst to organic dyestuff methylene blue under 980nm near-infrared laser irradiates of 15%.As can be seen from the figure, at 980nm near-infrared laser according to after 6h, β-NaYF
4: Yb
3+, Tm
3+quality be 15% near-infrared composite photo-catalyst can reach 82.7% to the clearance of organic dyestuff methylene blue, and as the β-NaYF prepared by the embodiment one of reference under similarity condition
4: Yb
3+, Tm
3+with the g-C prepared by embodiment two
3n
4the removal of organic dyestuff methylene blue is not almost affected.
Claims (6)
1. a rare earth compound g-C
3n
4class graphene photo-catalyst, is characterized in that: this photochemical catalyst is β-NaYF
4: Yb
3+, Tm
3+nano particle and g-C
3n
4class grapheme material compound forms, β-NaYF
4: Yb
3+, Tm
3+nano particle is evenly distributed in g-C
3n
4the heterojunction structure that stratiform class graphene nanometer sheet is formed.
2. a kind of rare earth compound g-C as claimed in claim 1
3n
4class graphene photo-catalyst, is further characterized in that: β-NaYF
4: Yb
3+, Tm
3+nano particle has six side's phase structures; Diameter is spherical 10-100 nm's; g-C
3n
4class Graphene is the composite that laminar nano sheet is formed.
3. a kind of rare earth compound g-C as claimed in claim 1
3n
4class graphene photo-catalyst, its preparation method is divided into three steps:
(1) three kinds of group of the lanthanides trifluoroacetates and sodium trifluoroacetate are added in three-necked bottle; add a certain proportion of oleic acid, 1-octadecylene and oleyl amine again; 330 DEG C of pyroreaction 1h under nitrogen protection atmosphere; with absolute ethyl alcohol and deionized water centrifuge washing number time after room temperature to be cooled, put into 80 DEG C of oven for drying and just can obtain up-conversion luminescence nano particle β-NaYF
4: Yb
3+, Tm
3+.
4.(2) take a certain amount of melamine to be placed with in the dry pot of lid, more dry pot is put into Muffle furnace high-temperature calcination, control heating rate and heat time, just can obtain flaxen semi-conducting material g-C
3n
4.
5.(3) by g-C prepared in step (2)
3n
4in methyl alcohol, ultrasonic 30min, obtains g-C
3n
4dispersion liquid; Take β-NaYF prepared in step (1) again
4: Yb
3+, Tm
3+add wherein, Keep agitation 24h is until methanol solution all evaporates under magnetic stirring, finally obtained product is calcined 1h at 250 DEG C, just can obtain rare earth compound g-C
3n
4class graphene photo-catalyst.
6. a kind of rare earth compound g-C as claimed in claim 1
3n
4class graphene photo-catalyst, the feature of its preparation method is also: the quality of rare earth nanometer particle on class graphene nanometer sheet regulates in 5% ~ 50% scope; Its specific area is at 10-32.2 m
2between/g.
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