CN104475140A - Silver-modified carbon nitride composite photocatalytic material and preparation method thereof - Google Patents
Silver-modified carbon nitride composite photocatalytic material and preparation method thereof Download PDFInfo
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- CN104475140A CN104475140A CN201410621945.5A CN201410621945A CN104475140A CN 104475140 A CN104475140 A CN 104475140A CN 201410621945 A CN201410621945 A CN 201410621945A CN 104475140 A CN104475140 A CN 104475140A
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Abstract
The invention relates to a silver-modified carbon nitride composite photocatalytic material and a preparation method thereof. The preparation method comprises: dissolving dicyanodiamide or melamine in deionized water or dimethyl sulfoxide and performing ultrasonic dispersing, so as to obtain a dicyanodiamide or melamine dispersion liquid; dissolving silver nitrate in deionized water and stirring uniformly, so as to obtain a silver nitrate solution; slowly dropwise adding the silver nitrate solution into the above dicyanodiamide or melamine dispersion liquid under the condition of magnetic stirring, and continuing stirring the solution, so as to obtain a mixed precursor solution; using anhydrous ethanol and deionized water repeatedly wash the obtained mixed precursor solution for multiple times, and performing vacuum drying; and putting the obtained product in a proper crucible and covering, putting in a high-temperature furnace, and sintering for a period under the condition of nitrogen protection, so as to obtain a powdery sample. The advantages comprise that the raw material source is wide, the preparation technology is simple and practicable, and the cost is relatively low; and the prepared composite photocatalytic material has relatively good photocatalytic degradation effect on organic dye rhodamine B under irradiation of visible light.
Description
Technical field
the present invention relates to a kind of silver-colored modification carbonitride composite photocatalyst material and preparation method thereof, refer to that a kind of aqueous solution ion exchange methods prepares the method for silver/carbonitride composite photocatalyst material especially, belong to composite, photocatalysis technology and field for the treatment of of water pollution.
Background technology
Along with industrial expansion, the originally limited water resource of the mankind is subject to day by day serious pollution, and removing toxic and harmful substance in water body such as agricultural chemicals, organic dyestuff etc. becomes the important process of field of Environment Protection; But the processing method of water pollutions is the pollutant large for discharge capacity, concentration is higher mostly at present, purification that is low for concentration in water body, that be difficult to the priority pollutant transformed is also helpless, and the solution that the Photocatalyst that the eighties grows up is this problem provides good approach.
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.
Usually adulterate a small amount of metallic element in conductor photocatalysis material, the electronic structure of material can be changed, particularly semiconductor energy band structure, and optimize light absorpting ability to a certain extent, promote the separation that photo-generate electron-hole is right to improve its photocatalytic activity.Due to g-C
3n
4for polymeric material, there is very high exciton binding energy and comparatively low-crystallinity, be unfavorable for the right fast transferring of photo-generate electron-hole and be efficiently separated, thus cause its photocatalytic process quantum efficiency on the low side, be unfavorable for g-C
3n
4applying of photochemical catalyst; By g-C
3n
4carry out compound with other materials, form heterojunction structure, in light-catalyzed reaction process, the two simultaneously stability sunshine, produces photo-generated carrier, and under the help of built in field, light induced electron and hole are oppositely moved, and significantly suppress the compound of photo-generated carrier, improve its photocatalysis efficiency.
At present, with dicyanodiamine, silver nitrate for raw material, prepare silver/carbonitride composite photocatalyst material fast by aqueous solution ion exchange methods, and be applied to photocatalysis degradation organic contaminant and have no report.
Main photocatalysis principle is that produce electron transition, valence-band electrons is excited to conduction band when the photon irradiation being greater than composite energy gap is to photochemical catalyst, forms hole one duplet, and be adsorbed on the H on its surface
2o and O
2effect, forms active very strong free radical and superoxide ion isoreactivity oxygen; The product that they and water and oxygen react is peroxide (O
2-) and the very high hydroxy (OOH or OH) of reactivity; Because the free radical generated has very strong oxidability; wherein OH free radical has 402.8 MJ/mol reaction energy; can the keys such as organic C-C, C-H, C-N, C-O, N-H be destroyed, photochemical catalytic oxidation is played a decisive role, thus there is the ability of degradation of organic substances; The organic pollutant wastewater of degraded mainly contains dyeing waste water, agricultural chemicals waste water, oily waste water, chloro-organic waste water, waste water, pharmacy waste water etc. containing surfactant; In addition, the living radical of generation can also be degraded part inorganic hazardous pollutant, simultaneously O
2-there is very strong reproducibility, the toxic heavy metal ion in raw sewage can be gone back, generate metal simple-substance, low toxicity valence state metal ion, realize the removal of heavy metal ion.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, preparation is simple, the preparation method of the silver/carbonitride composite photocatalyst material of environmental protection and application thereof, overcome the defect that existing capability material cost is high, clean-up effect is poor, for technical foundation is established in the development of low cost, high performance surrounding purifying material and application.
Realizing the technical solution adopted in the present invention is: a kind of carbonitride/silver-colored composite photocatalyst material, and obtained by aqueous solution ion exchange methods, it is characterized in that, preparation process is as follows:
(1) dicyanodiamine or melamine are dissolved in ultrasonic disperse in deionized water or dimethyl sulfoxide (DMSO) (DMSO), obtain dicyanodiamine or melamine dispersion liquid.
(2) silver nitrate is dissolved in deionized water, stirs, obtain liquor argenti nitratis ophthalmicus; Slowly be added drop-wise under magnetic agitation condition by liquor argenti nitratis ophthalmicus in above-mentioned dicyanodiamine or melamine dispersion liquid, solution continues to stir, and obtains mixing precursor solution.
(3) by gained mixing precursor solution absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing.
(4) 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 30min.
The time of stirring in step (2) is 10min, and the time of continuing to stir is 6h.
The mol ratio of described dicyanodiamine or melamine and silver nitrate is 1:1-1:2.
Product in described step (4), in high-temperature atmosphere furnace, at the uniform velocity rose to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cooled to room temperature.
The present invention has the following advantages compared with prior art:
A) Ag nano particle is implanted g-C
3n
4interlayer and surface, g-C
3n
4layer structure is peeled off by part and is fragmentated and define compound with Ag particle, causes its interlamellar spacing constantly to become large until part is separated, and defines dispersiveness g-C relatively preferably
3n
4/ Ag composite photocatalyst.
B) can realize Ag particle and g-C without the need to applying surface activating agent in preparation process
3n
4carry out compound, form heterojunction structure, in light-catalyzed reaction process, the two simultaneously stability sunshine, produces photo-generated carrier, and under the help of built in field, light induced electron and hole are oppositely moved, and significantly suppress the compound of photo-generated carrier, improve its photocatalysis efficiency.
C) g-C
3n
4/ Ag composite photocatalyst and single g-C
3n
4compare not only extend light response range, increase specific surface and also accelerate being separated of light induced electron and hole, improve photocatalysis performance.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of carbonitride/silver-colored composite photocatalyst material.
Fig. 2 is the X-ray diffractogram of carbonitride/silver-colored composite photocatalyst material.
Fig. 3 is the UV-vis DRS spectrogram of carbonitride/silver-colored composite photocatalyst material.
Fig. 4 is carbonitride/silver-colored composite photocatalyst material photocatalytic degradation curve map to rhodamine B under UV-irradiation.
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
By 10mmol (0.84 g) dicyanodiamine be dissolved in 40 ml deionized water for ultrasonic 30 minutes, obtain dicyanodiamine dispersion liquid; Take 10mmol (1.69 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in dicyanodiamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace; under the condition of nitrogen protection; sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace; after heat preservation sintering 4h; after naturally cooling to room temperature, obtain powdered samples.
Embodiment 2
By 10mmol (0.84 g) dicyanodiamine be dissolved in 40 ml deionized water for ultrasonic 30 minutes, obtain dicyanodiamine dispersion liquid; Take 20mmol (3.38 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in dicyanodiamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; Then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace, and under the condition of nitrogen protection, sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, after naturally cooling to room temperature, obtained powdered samples.
Embodiment 3
By 10mmol (0.84 g) dicyanodiamine to be dissolved in 40 ml DMSO ultrasonic 30 minutes, obtain dicyanodiamine dispersion liquid; Take 10mmol (1.69 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in dicyanodiamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; Then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace, and under the condition of nitrogen protection, sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, after naturally cooling to room temperature, obtained powdered samples.
Embodiment 4
By 10mmol (0.84 g) dicyanodiamine to be dissolved in 40 ml DMSO ultrasonic 30 minutes, obtain dicyanodiamine dispersion liquid; Take 20mmol (3.38 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in dicyanodiamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; Then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace, and under the condition of nitrogen protection, sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, after naturally cooling to room temperature, obtained powdered samples.
Embodiment 5
By 10mmol (1.26 g) melamine be dissolved in 40 ml deionized water for ultrasonic 30 minutes, obtain melamine dispersion liquid; Take 10mmol (1.69 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in melamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; Then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace, and under the condition of nitrogen protection, sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, after naturally cooling to room temperature, obtained powdered samples.
Embodiment 6
By 10mmol (1.26 g) melamine be dissolved in 40 ml deionized water for ultrasonic 30 minutes, obtain melamine dispersion liquid; Take 20mmol (3.38 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in melamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; Then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace, and under the condition of nitrogen protection, sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, after naturally cooling to room temperature, obtained powdered samples.
Embodiment 7
By 10mmol (1.26 g) melamine to be dissolved in 40 ml DMSO ultrasonic 30 minutes, obtain melamine dispersion liquid; Take 10mmol (1.69 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in melamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; Then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace, and under the condition of nitrogen protection, sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, after naturally cooling to room temperature, obtained powdered samples.
Embodiment 8
By 10mmol (1.26 g) melamine to be dissolved in 40 ml DMSO ultrasonic 30 minutes, obtain melamine dispersion liquid; Take 20mmol (3.38 g) silver nitrate be dissolved in 40 ml deionized waters, stir 10 minutes, obtain liquor argenti nitratis ophthalmicus; Above-mentioned liquor argenti nitratis ophthalmicus is dropwise joined in melamine dispersion liquid under the condition of magnetic agitation, forms mixed liquor, after dropwising, mixed solution is slowly stirred 6 hours, obtain mixing precursor solution; 50 degree of vacuum drying after gained mixing precursor solution absolute ethyl alcohol and deionized water cyclic washing 3 times; Then being loaded by product after suitable crucible is built is put in high-temperature atmosphere furnace, and under the condition of nitrogen protection, sample at the uniform velocity rose to 550 degree by 4 hours from room temperature at high-temperature atmosphere furnace, after heat preservation sintering 4h, after naturally cooling to room temperature, obtained powdered samples.
In addition, the carbonitride prepared by the present invention/silver-colored composite photocatalyst material be used to simultaneously organic dyestuff rhodamine B photocatalytic degradation experiment, detailed process and step as follows:
The last the carbonitride of 100 mg/silver-colored composite photocatalyst material 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 visible light photo catalysis 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 carbonitride/silver-colored composite photocatalyst material under UV-irradiation to the photocatalytic degradation curve map of rhodamine B.
Fig. 1 is the scanned picture of prepared carbonitride/silver-colored composite photocatalyst material, clearly can find out the pattern of composite, C in figure
3n
4be wrapped in most Ag particle.
Fig. 2 is prepared carbonitride/silver composite material, pure C
3n
4with the XRD spectra of Ag; 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, pure g-C
3n
4(002) face of feature confirms the formation of carbonitride; Due to C in composite sample
3n
4ratio lower and relative to the diffraction maximum of strong silver, obvious g-C cannot be observed in XRD collection of illustrative plates
3n
4diffraction 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 solid-state diffuse reflection spectrum result, can find out that nano composite material has good absorption at visible ray and UV light region in figure, and it absorbs band edge approximately at 500 nm.
Fig. 4 be prepared carbonitride/silver-colored 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%, after 60 minutes, 70% is reached to the degradation rate of rhodamine B, show that carbonitride/silver-colored composite photocatalyst material has good photocatalytic degradation effect to organic dyestuff rhodamine B under visible light illumination.
Claims (6)
1. a silver-colored modification carbonitride composite photocatalyst material, is characterized in that: described composite photocatalyst material is formed by carbonitride and money kind Material cladding, and Ag nano particle implants g-C
3n
4interlayer and surface, g-C
3n
4layer structure is peeled off by part and is fragmentated and define compound with Ag particle, causes its interlamellar spacing constantly to become large until part is separated, and defines dispersiveness g-C relatively preferably
3n
4/ Ag composite photocatalyst; Described composite photocatalyst material has efficient photocatalytic degradation effect to organic dyestuff rhodamine B under excited by visible light: the rhodamine B solution to concentration being 100 ppm, the degradation efficiency of 60 minutes reaches 70 %.
2. the preparation method of a kind of silver-colored modification carbonitride composite photocatalyst material as claimed in claim 1, is characterized in that concrete steps are as follows:
(1) dicyanodiamine or melamine are dissolved in ultrasonic disperse in deionized water or dimethyl sulfoxide (DMSO) (DMSO), obtain dicyanodiamine or melamine dispersion liquid;
(2) silver nitrate is dissolved in deionized water, stirs, obtain liquor argenti nitratis ophthalmicus; Slowly be added drop-wise under magnetic agitation condition by liquor argenti nitratis ophthalmicus in above-mentioned dicyanodiamine or melamine dispersion liquid, solution continues to stir, and obtains mixing precursor solution;
(3) by gained mixing precursor solution absolute ethyl alcohol and the repeatedly final vacuum drying of deionized water cyclic washing;
(4) 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-colored modification carbonitride composite photocatalyst material as claimed in claim 2, is characterized in that: in step (1), the time of ultrasonic disperse is 30min.
4. the preparation method of a kind of silver-colored modification carbonitride composite photocatalyst material as claimed in claim 2, is characterized in that: the time of stirring in step (2) is 10min, and the time of continuing to stir is 6h.
5. the preparation method of a kind of silver-colored modification carbonitride composite photocatalyst material as claimed in claim 2, is characterized in that: the mol ratio of described dicyanodiamine or melamine and silver nitrate is 1:1-1:2.
6. the preparation method of a kind of silver-colored modification carbonitride composite photocatalyst material as claimed in claim 2, it is characterized in that: the product in described step (4) is in high-temperature atmosphere furnace, at the uniform velocity rise to 550 degree by 4 hours from room temperature, after heat preservation sintering 4h, naturally cool to room temperature.
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