CN104437589A - Silver/graphene oxide/carbon nitride composite photocatalytic material and preparation method thereof - Google Patents
Silver/graphene oxide/carbon nitride composite photocatalytic material and preparation method thereof Download PDFInfo
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- CN104437589A CN104437589A CN201410621933.2A CN201410621933A CN104437589A CN 104437589 A CN104437589 A CN 104437589A CN 201410621933 A CN201410621933 A CN 201410621933A CN 104437589 A CN104437589 A CN 104437589A
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Abstract
The invention relates to a silver/graphene oxide/carbon nitride composite photocatalytic material and a preparation method thereof. The preparation method comprises the following steps: dispersing graphene oxide into deionized water, and carrying out ultrasonic treatment to obtain graphene oxide dispersion liquid; dropwise adding a silver nitrate solution into the graphene oxide dispersion liquid under magnetic stirring so as to obtain a mixed solution A; slowly and dropwise adding dicyanodiamine dispersion liquid into a mixed pecursor solution A under the magnetic stirring, then continuing to stir the obtained mixed solution, standing for one night, carrying out suction filtration on an obtained product, repeatedly washing the product by virtue of absolute ethanol and deionized water, and carrying out vacuum drying; putting the obtained product into a proper crucible, covering the crucible, putting the crucible into a high temperature atmosphere oven, and sintering in the presence of nitrogen protection so as to obtain a powdery sample. The silver/graphene oxide/carbon nitride composite photocatalytic material presents a relatively high activity to an organic dye, namely Rhodamin B under visible light excitation and has wide practical value and application prospect in the fields of preparation techniques of heterojunction photocatalytic materials as well as sewage treatment.
Description
Technical field
the present invention relates to a kind of silver/graphene oxide/carbonitride composite photocatalyst material and preparation method thereof, refer to that a kind of aqueous solution ion exchange methods prepares the method for silver/graphene oxide/carbonitride composite photocatalyst material especially, belong to composite, photocatalysis technology and field for the treatment of of water pollution.
Background technology
Graphite phase carbon nitride g-C in recent years
3n
4due to the chemical stability of its excellence, special electronic band structure, non-metallic components, the feature such as visible light-responded is caused to the great interest of researcher; But due to the intrinsic property of polymer, as catalysis material, carbonitride exists that specific area is little, the combination that produces photo-generated carrier can high, the deficiency such as photo-generate electron-hole compound is serious, quantum efficiency is low, energy gap is larger, its large-scale promotion application at the energy and environmental area of serious restriction.
Graphene is a kind of new material of the individual layer laminated structure be made up of carbon atom, and monolayer carbon original thickness not only makes it not only be applicable to the growth of function nano material, and has good electronic conductivity, has been acknowledged as the ideal carrier material of catalyst; Experiment, using graphene oxide as precursor material, controls silver orthophosphate coring and increment in the process of reaction, makes the final zinc oxide/silver orthophosphate/Graphene composite photocatalyst material generated have homogeneous pattern and less size; The high transmission rate of Graphene, high specific area make obtained composite photocatalyst material have well dispersed and adsorptivity in the solution; Its high electrical conductance accelerates the separation of Pair production further, extends the life-span of active component, enhances the catalytic activity of composite photocatalyst material; At present, with dicyanodiamine or melamine, graphene oxide, silver nitrate for raw material, the synthesis of aqueous solution ion exchange methods is used to have the silver/graphene oxide/carbonitride composite photocatalyst material of heterojunction structure and have no report for photocatalysis degradation organic contaminant and resource of purifying waste water.
Summary of the invention
The object of the present invention is to provide that a kind of flow process is simple, environmental friendliness, the method for silver/graphene oxide/carbonitride composite photocatalyst material of heterojunction structure preparing controllable appearance, homogeneous distribution with low cost, the composite photocatalyst material of preparation has visible light-responded characteristic and remarkable photocatalytic pollutant degradation performance widely.
Realizing the technical solution adopted in the present invention is: take graphene oxide as precursor material, prepares silver oxide/graphene oxide/carbonitride composite photocatalyst material by ion-exchange, and its concrete preparation method's step is as follows:
(1) graphene oxide is dissolved in deionized water for ultrasonic dispersion, obtains graphene oxide dispersion.
(2) silver nitrate is dissolved in deionized water for stirring, obtains liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic agitation condition, dropwises rear solution and at room temperature continue to stir, obtain mixing precursor solution A.
(3) dicyanodiamine or melamine are dissolved in deionized water for ultrasonic dispersion, obtain dicyanodiamine or melamine dispersion liquid.
(4) dicyanodiamine step (3) prepared under the condition of magnetic agitation or melamine dispersion liquid dropwise slowly add in mixing precursor solution A prepared by step (2), the mixed solution obtained after dropwising continues to stir rear hold over night, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration.
(5) product obtained is loaded after suitable crucible is built and be put in high-temperature atmosphere furnace, under the condition of nitrogen protection, sinter a period of time, obtain powdered samples.
In step (1), the time of ultrasonic disperse is 5h, adds 0.1-4g graphene oxide in every premium on currency.
The time of stirring in step (2) is 10min, and the concentration of silver nitrate is 0.3 mol/L, and the time of continuing to stir is 6h; The mass ratio of silver nitrate and graphene oxide is 254:1-40.
In step (3), the time of ultrasonic disperse is 30 min; The mol ratio of described dicyanodiamine or melamine and silver nitrate is 1:1.
The time that mixed solution in step (4) continues to stir is 6h.
In step (5), product at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, naturally cooled to room temperature.
The present invention has the following advantages compared with prior art:
A (), by the cooperative effect between silver and carbonitride and graphene oxide three, obtained composite photocatalyst material has enhancing and has visible light-responded scope and utilization ratio.
B (), using graphene oxide as presoma, the active attachment point of surface of graphene oxide effectively can regulate and control size and the pattern of silver nano-grain and carbonitride, strengthen the Interface composites effect of this part of three.
C specific area that () graphene oxide is larger is conducive to the absorption to pollutant, and between photocatalytic process person three kinds of materials, photo-generate electron-hole separating effect and electron transfer capabilities make composite photocatalyst material have efficient photocatalytic activity fast.
D technique prepared by () is simple, with low cost, energy-conserving and environment-protective and the superior performance of material.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of silver/graphene oxide/carbonitride composite photocatalyst material.
Fig. 2 is the X-ray diffractogram of silver/graphene oxide/carbonitride composite photocatalyst material.
Fig. 3 is the UV-vis DRS spectrogram of silver/graphene oxide/carbonitride composite photocatalyst material.
Fig. 4 is silver/graphene oxide/carbonitride composite photocatalyst material photocatalytic degradation curve map to rhodamine B under visible light conditions.
Fig. 5 is the semiconductor energy gap structure chart of carbonitride.
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 1
10 mg graphene oxides are scattered in 100 ml deionized water for ultrasonic and within 5 hours, obtain graphene oxide dispersion; Take 15mmol(2.54 g) after silver nitrate is dissolved in 50 ml deionized water for stirring 10 min, obtain liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic stirring, dropwises rear solution and at room temperature continue to stir 6h, obtain mixing precursor solution A; Take 15 mmol (1.26 g) dicyanodiamine be dissolved in 50 ml deionized waters, obtain dicyanodiamine dispersion liquid; Under the condition of magnetic agitation, dicyanodiamine dispersion liquid is dropwise slowly added in mixing precursor solution A, hold over night after mixed solution continuation stirring 6 h obtained after dropwising, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration; Being loaded by the product obtained after suitable crucible is built is put in high-temperature atmosphere furnace, under the condition of nitrogen protection, at the uniform velocity rises to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cools to room temperature, obtain powdered samples.
Embodiment 2
20 mg graphene oxides are scattered in 100 ml deionized water for ultrasonic and within 5 hours, obtain graphene oxide dispersion; Take 15mmol(2.54 g) after silver nitrate is dissolved in 50 ml deionized water for stirring 10 min, obtain liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic stirring, dropwises rear solution and at room temperature continue to stir 6h, obtain mixing precursor solution A; Take 15 mmol (1.26 g) dicyanodiamine be dissolved in 50 ml deionized waters, obtain dicyanodiamine dispersion liquid; Dicyanodiamine dispersion liquid is dropwise slowly added in mixing precursor solution A under the condition of magnetic agitation, hold over night after the mixed solution continuation stirring 6h obtained after dropwising, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration; Being loaded by the product obtained after suitable crucible is built is put in high-temperature atmosphere furnace, under the condition of nitrogen protection, at the uniform velocity rises to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cools to room temperature, obtain powdered samples.
Embodiment 3
50 mg graphene oxides are scattered in 100 ml deionized water for ultrasonic and within 5 hours, obtain graphene oxide dispersion; Take 15mmol(2.54 g) after silver nitrate is dissolved in 50 ml deionized water for stirring 10 min, obtain liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic stirring, dropwises rear solution and at room temperature continue to stir 6h, obtain mixing precursor solution A; Take 15 mmol (1.26 g) dicyanodiamine be dissolved in 50 ml deionized waters, obtain dicyanodiamine dispersion liquid; Dicyanodiamine dispersion liquid is dropwise slowly added in mixing precursor solution A under the condition of magnetic agitation, hold over night after the mixed solution continuation stirring 6h obtained after dropwising, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration; Being loaded by the product obtained after suitable crucible is built is put in high-temperature atmosphere furnace, under the condition of nitrogen protection, at the uniform velocity rises to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cools to room temperature, obtain powdered samples.
Embodiment 4
100 mg graphene oxides are scattered in 100 ml deionized water for ultrasonic and within 5 hours, obtain graphene oxide dispersion; Take 15mmol(2.54 g) after silver nitrate is dissolved in 50 ml deionized water for stirring 10 min, obtain liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic stirring, dropwises rear solution and at room temperature continue to stir 6h, obtain mixing precursor solution A; Take 15 mmol (1.26 g) dicyanodiamine be dissolved in 50 ml deionized waters, obtain dicyanodiamine dispersion liquid; Dicyanodiamine dispersion liquid is dropwise slowly added in mixing precursor solution A under the condition of magnetic agitation, hold over night after the mixed solution continuation stirring 6h obtained after dropwising, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration; Being loaded by the product obtained after suitable crucible is built is put in high-temperature atmosphere furnace, under the condition of nitrogen protection, at the uniform velocity rises to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cools to room temperature, obtain powdered samples.
Embodiment 5
200 mg graphene oxides are scattered in 100 ml deionized water for ultrasonic and within 5 hours, obtain graphene oxide dispersion; Take 15mmol(2.54 g) after silver nitrate is dissolved in 50 ml deionized water for stirring 10 min, obtain liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic stirring, dropwises rear solution and at room temperature continue to stir 6h, obtain mixing precursor solution A; Take 15 mmol (1.26 g) dicyanodiamine be dissolved in 50 ml deionized waters, obtain dicyanodiamine dispersion liquid; Dicyanodiamine dispersion liquid is dropwise slowly added in mixing precursor solution A under the condition of magnetic agitation, hold over night after the mixed solution continuation stirring 6h obtained after dropwising, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration; Being loaded by the product obtained after suitable crucible is built is put in high-temperature atmosphere furnace, under the condition of nitrogen protection, at the uniform velocity rises to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cools to room temperature, obtain powdered samples.
Embodiment 6
400 mg graphene oxides are scattered in 100 ml deionized water for ultrasonic and within 5 hours, obtain graphene oxide dispersion; Take 15mmol(2.54 g) after silver nitrate is dissolved in 50 ml deionized water for stirring 10 min, obtain liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic stirring, dropwises rear solution and at room temperature continue to stir 6h, obtain mixing precursor solution A; Take 15 mmol (1.26 g) dicyanodiamine be dissolved in 50 ml deionized waters, obtain dicyanodiamine dispersion liquid; Dicyanodiamine dispersion liquid is dropwise slowly added in mixing precursor solution A under the condition of magnetic agitation, hold over night after the mixed solution continuation stirring 6h obtained after dropwising, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration; Being loaded by the product obtained after suitable crucible is built is put in high-temperature atmosphere furnace, under the condition of nitrogen protection, at the uniform velocity rises to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cools to room temperature, obtain powdered samples.
In addition, the silver/graphene oxide/carbonitride composite photocatalyst material prepared by the present invention be used to simultaneously organic dyestuff rhodamine B photocatalytic degradation experiment, detailed process and step as follows:
The last the silver/graphene oxide/carbonitride composite photocatalyst material of 100 mg being scattered in the rhodamine B solution of 100 milliliter of 100 ppm ultrasonic 10 minutes, the dispersion liquid mixed is transferred in the quartzy bottle in xenon lamp catalytic reactor, stir under dark condition after within 30 minutes, making it reach adsorption equilibrium and open xenon source, extracting the postradiation mixed dispersion liquid of 4 mL every 10 minutes with syringe transfers in the centrifuge tube of mark, xenon source is closed after radiation of visible light certain hour, by the sample centrifugation in all centrifuge tubes, centrifugal rear obtained supernatant liquor transfers in quartz colorimetric utensil the absorbance measured on ultraviolet-visible spectrophotometer under the different photocatalysis time further, thus under obtaining each time period silver/graphene oxide/carbonitride composite photocatalyst material under visible light illumination to the photocatalytic degradation curve map of rhodamine B.
Fig. 1 is prepared silver/graphene oxide/carbonitride composite scintigram, clearly can find out the C of composite sheet from Fig. 1
3n
4with sheet graphene oxide; In the composite adopting dicyanodiamine presoma to obtain, the particle of silver is relatively little, is wrapped in the C of stratiform
3n
4with in sheet graphene oxide.
Fig. 2 is the XRD figure of prepared silver/graphene oxide/carbon nitride material, and through contrasting can confirm with JCPDS standard card, 4 the strong diffraction maximums occurred in composite can well be pointed out as crystal face corresponding to Ag, due to C in composite sample
3n
4lower and relative to the diffraction maximum of strong silver with the ratio of GO, obvious C cannot be observed in XRD collection of illustrative plates
3n
4with GO diffraction maximum; And, not there is the diffraction maximum of other stronger phases or element in collection of illustrative plates, illustrate that the introducing of silver does not change the crystal structure of composite.
Fig. 3 is the UV-vis DRS spectrogram of prepared silver/graphene oxide/carbonitride composite, as can be seen from figure we, this composite all has good absorption at whole ultraviolet-visible district (200-800 nm), and absorbance is more than 0.3.
Fig. 4 be prepared silver/graphene oxide/carbonitride composite photocatalyst material under visible light conditions to the photocatalytic degradation curve map of rhodamine B, as can be seen from Figure 4, this composite radiation of visible light after 40 minutes to the degradation rate of rhodamine B more than 60%, reach 80% to the degradation rate of rhodamine B after 60 minutes, photocatalytic degradation curve map shows that silver/graphene oxide/carbonitride composite photocatalyst material has good photocatalytic degradation effect to organic dyestuff rhodamine B under visible light illumination.
Fig. 5 is the semiconductor energy gap structure chart of carbonitride; As seen from the figure, the C in its structure, atom N are with sp
2the pi-conjugated system of hydridization height of formation delocalization; Wherein, Np
ztrack composition g-C
3n
4highest occupied molecular orbital (HOMO), Cp
ztrack composition lowest unoccupied molecular orbital (LUMO), energy gap ~ 2.7 eV between them, can absorb the royal purple light that solar spectrum medium wavelength is less than 475 nm.Theory calculate and experimental study show, g-C
3n
4also have most suitable semiconductor band edge position, itself HOMO and LUMO lays respectively at+1.4 V and-1.3 V (vs NHE, PH=7), meets photodissociation aquatic products hydrogen, produces the thermodynamic requirement of oxygen; In addition graphene oxide has excellent electronic conduction ability and lower fermi level, effectively can catch light induced electron, suppresses the serious compound of photo-generated carrier; The composite of three-system, is injected into the conduction band of wide bandgap semiconductor, is spatially separated with hole by light induced electron by the light induced electron of generation, fast activating molecular oxygen produces superoxide radical (O
2 -) and photohole, realize the photocatalytic degradation of organic pollution in aqueous phase.
Claims (7)
1. silver/graphene oxide/carbonitride composite photocatalyst material, it is characterized in that: described composite photocatalyst material is formed by carbonitride, silver and graphene oxide three kinds of Material claddings, wherein Argent grain is embedded in carbonitride layer structure or is deposited on graphene oxide lamella surface; Described composite photocatalyst material has efficient photocatalytic degradation effect to organic dyestuff rhodamine B under excited by visible light: reach 80 % to rhodamine B solution 60 minutes degradation rates of 100 ppm.
2. the preparation method of a kind of silver/graphene oxide/carbonitride composite photocatalyst material as claimed in claim 1, is characterized in that preparation process is as follows:
(1) graphene oxide is dissolved in deionized water for ultrasonic dispersion, obtains graphene oxide dispersion;
(2) silver nitrate is dissolved in deionized water for stirring, obtains liquor argenti nitratis ophthalmicus; Liquor argenti nitratis ophthalmicus is added drop-wise in above-mentioned graphene oxide dispersion under magnetic agitation condition, dropwises rear solution and at room temperature continue to stir, obtain mixing precursor solution A;
(3) dicyanodiamine or melamine are dissolved in deionized water for ultrasonic dispersion, obtain dicyanodiamine or melamine dispersion liquid;
(4) dicyanodiamine step (3) prepared under the condition of magnetic agitation or melamine dispersion liquid dropwise slowly add in mixing precursor solution A prepared by step (2), the mixed solution obtained after dropwising continues to stir rear hold over night, with absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing after products therefrom suction filtration;
(5) product obtained is loaded after suitable crucible is built and be put in high-temperature atmosphere furnace, under the condition of nitrogen protection, sinter a period of time, obtain powdered samples.
3. the preparation method of a kind of silver/graphene oxide/carbonitride composite photocatalyst material as claimed in claim 2, is characterized in that: in step (1), the time of ultrasonic disperse is 5h, adds 0.1-4g graphene oxide in every premium on currency.
4. the preparation method of a kind of silver/graphene oxide/carbonitride composite photocatalyst material as claimed in claim 2, is characterized in that: the time of stirring in step (2) is 10min, and the concentration of silver nitrate is 0.3 mol/L, and the time of continuing to stir is 6h; The mass ratio of silver nitrate and graphene oxide is 254:1-40.
5. the preparation method of a kind of silver/graphene oxide/carbonitride composite photocatalyst material as claimed in claim 2, is characterized in that: in step (3), the time of ultrasonic disperse is 30 min; The mol ratio of described dicyanodiamine or melamine and silver nitrate is 1:1.
6. the preparation method of a kind of silver/graphene oxide/carbonitride composite photocatalyst material as claimed in claim 2, is characterized in that: the time that the mixed solution in step (4) continues to stir is 6h.
7. the preparation method of a kind of silver/graphene oxide/carbonitride composite photocatalyst material as claimed in claim 2, it is characterized in that: in step (5), product at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, naturally cool to room temperature.
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