CN102950016B - Preparation method of ZnO/g-C3N4 composite photocatalyst - Google Patents
Preparation method of ZnO/g-C3N4 composite photocatalyst Download PDFInfo
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- CN102950016B CN102950016B CN201210421522.XA CN201210421522A CN102950016B CN 102950016 B CN102950016 B CN 102950016B CN 201210421522 A CN201210421522 A CN 201210421522A CN 102950016 B CN102950016 B CN 102950016B
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Abstract
The invention relates to a preparation method of a ZnO / g-C3N4 composite photocatalyst. A two-stage solvent thermal / ultrasonic dispersing method is employed to prepare the ZnO / g-C3N4 composite photocatalyst. After the two-stage solvent thermal treatment, porous ZnO nano crystalline with high dispersion grown on the g-C3N4 can be obtained, and the ZnO nanocrystalline and the g-C3N4 can form a good composite structure; the ultrasonic treatment reduces agglomeration among the ZnO / g-C3N4 composite particles, and improves dispersion of the composite catalyst; and the nano composite particles with high dispersion strengthen effective utilization of sun light by the catalyst, and improve activity of the catalyst. The preparation method provided by the invention has the advantages of cheap raw materials and simple process; and the prepared composite photocatalyst has a broad application prospects in the fields of wastewater treatment and gas purification.
Description
[technical field]
The present invention relates to catalyst technical field, specifically, is a kind of ZnO/g-C
3n
4the preparation method of composite photo-catalyst.
[background technology]
Due to the high speed development of economic society and increasing rapidly of population, environmental pollution and energy crisis become the severe challenge that current social development faces, and the energy of development and utilization clean and effective becomes the task of top priority of various countries.For this reason, how to utilize better solar energy to become the research emphasis of various countries.
Photochemical catalyst is because of its room temperature deep reaction and can directly or indirectly utilize solar energy to drive the advantages such as reaction, becomes a kind of desirable environmental pollution improvement and clean energy resource utilization and production technology.
Because its spectrochemical property is stable, nontoxic, with low cost etc., advantage becomes one of photochemical catalyst the most with potential applications in numerous semiconductor light-catalysts to ZnO.But the spectral response of ZnO is at ultraviolet region, and because photo-generated carrier is very easily compound, cause quantum efficiency lower, restricted its performance to the utilization of solar energy and photocatalysis efficiency.
G-C
3n
4be graphite-phase C
3n
4a kind of novel photochemical catalyst, owing to thering is good chemical stability, narrower energy gap (E
g=2.7eV) etc. advantage causes people's concern.By with g-C
3n
4compound, can improve the separation of charge effect of ZnO photochemical catalyst, expand its light abstraction width.G-C
3n
4reasonable (the g-C of relative position of energy band coupling with ZnO
3n
4conduction band current potential more negative than the conduction band of ZnO, and the valence band current potential of ZnO compares g-C
3n
4valence band corrigendum), can effectively realize the right separation in light induced electron hole producing on two kinds of semiconductors, thereby improve significantly ZnO/g-C
3n
4the photocatalysis performance of compound.
Existing making ZnO/g-C
3n
4the method of composite photo-catalyst mainly contains ball-milling method.Ball-milling method is generally distinguished making ZnO and g-C in advance
3n
4pressed powder, is then transferred to ball milling in ball mill them and mixes the regular hour, finally obtains the ZnO/g-C of micro-(receiving) meter level
3n
4.Although preparation technology is easier for this method, the ZnO/g-C of preparation
3n
4in particle, ZnO and g-C
3n
4between the composite construction that mutually combines a little less than, can not give full play to two kinds of energy level matching effects between semiconductor, and easily form aggregate structure between particle, seriously reduced catalyst activity.
[summary of the invention]
The object of the invention is to overcome the deficiencies in the prior art, a kind of ZnO/g-C is provided
3n
4the preparation method of composite photo-catalyst.The inventive method has that raw material is easy to get, the feature of simple process, the ZnO/g-C of preparation
3n
4photochemical catalyst has good dispersiveness and larger specific area, not only can absorb efficiently sunshine, and can be by ZnO and g-C
3n
4between stronger compound action, effectively realize the separation of electron hole, improve significantly the photocatalysis efficiency of composite photo-catalyst.
The object of the invention is to be achieved through the following technical solutions:
A kind of ZnO/g-C
3n
4the preparation method of composite photo-catalyst, its concrete steps are:
By raw material, be zinc acetate, ethanol, diethanol amine, protonated g-C
3n
4, strong agitation is mixed 1～10h, and being preferably is 3～7h; Then mixed system is transferred in polytetrafluoroethyllining lining autoclave to 110～160 ℃ of solvent thermal reaction 10～50h, 160～200 ℃ of solvent thermal reaction 10～50h; Cooled and filtered, filter cake disperses in deionized water for ultrasonic, washing, filter, repeatedly, until filtrate pH is 6.8～7.2, filter cake is dried in supersound washing, and in air atmosphere 450～600 ℃ of roasting 1～10h, roasting time is preferably 3～7h; Obtain ZnO/g-C
3n
4composite photo-catalyst powder.
Described material quality is than being zinc acetate: ethanol: diethanol amine: protonated g-C
3n
4=1: (5.0～50.0): (10.0～50.0): (0.1～10.0).
ZnO/g-C of the present invention
3n
4photochemical catalyst has following characteristics: by low-temperature solvent heat treatment, form and have high specific surface area, high dispersive, porous ZnO nanocrystal, granular size is about 20-150nm, and high dispersive is at g-C
3n
4the nanocrystalline adsorb organic compound effectively of lip-deep porous ZnO; By high temperature section solvent heat treatment, make ZnO nano crystalline substance and g-C
3n
4form suitable composite construction, be conducive to electronics from g-C
3n
4to ZnO, effectively move, strengthened the separating effect of electron hole, and increased the degree of crystallinity of ZnO, further improved the activity of composite photo-catalyst.
Compared with prior art, good effect of the present invention is:
Adopt two-part solvent thermal reaction condition, low-temperature zone is conducive to the quick nucleation of ZnO, at g-C
3n
4it is nanocrystalline that upper growth in situ goes out the porous ZnO of polymolecularity, suppressed the reunion of nano particle, improves the specific area of ZnO.ZnO surface band negative electrical charge, the solvent heat treatment under hot conditions, is conducive to ZnO and positively charged protonated g-C
3n
4there is useful effect, impel ZnO to be attached to g-C
3n
4surface, forms good composite construction by high temperature section solvent heat treatment, and high-temperature solvent heat treatment has improved the degree of crystallinity of ZnO.
At ZnO/g-C
3n
4the preparatory phase of photochemical catalyst, adopts ultra-sonic dispersion method, can more effectively disperse ZnO/g-C
3n
4aggregate between composite nanometer particle, has increased the dispersiveness of composite particles.The Nano composite granules of polymolecularity has improved the utilization rate to sunshine, has strengthened ZnO/g-C
3n
4photocatalysis efficiency.
The ZnO/g-C obtaining by preparation method of the present invention
3n
4composite photo-catalyst, can ultraviolet light, visible ray and sunshine be light source, is applicable to photocatalysis degradation organic contaminant, photocatalytic hydrogen production by water decomposition.
[specific embodiment]
The present invention is below provided a kind of ZnO/g-C
3n
4the preparation method's of composite photo-catalyst the specific embodiment.
Embodiment 1
ZnO/g-C
3n
4preparation adopt two-part solvent heat-ultrasonic method.According to zinc acetate, ethanol, diethanol amine, g-C
3n
4mass ratio=1: the ratio of 10: 20: 1.5 is mixed, strong agitation 6h; Then mixed system is transferred in polytetrafluoroethyllining lining autoclave to 150 ℃ of reaction 24h, 190 ℃ of reaction 24h; (frequency is 40KH in ultrasonic dispersion afterwards after filtration,
z, power is 300W), washing, repeat after four times, filtration cakes torrefaction, and in air atmosphere 500 ℃ of roasting 2h; Cooling rear grind into powder.
Embodiment 2
ZnO/g-C
3n
4preparation adopt two-part solvent heat-ultrasonic method.ZnO/g-C
3n
4preparation according to zinc acetate, ethanol, diethanol amine, g-C
3n
4mass ratio=1: the ratio of 15: 20: 2.0 is mixed, strong agitation 8h; Then mixed system is transferred in polytetrafluoroethyllining lining autoclave to 130 ℃ of reaction 30h, 180 ℃ of reaction 18h; (frequency is 40KH in ultrasonic dispersion afterwards after filtration,
z, power is 600W), washing, repeat after four times, filtration cakes torrefaction, and in air atmosphere 500 ℃ of roasting 1h; Cooling rear grind into powder.
Reference examples 1
In order to carry out Contrast on effect with embodiment, choose reference examples 1.Reference examples 1 adopts one-part form solvent heat-ultrasonic method.ZnO/g-C
3n
4preparation according to zinc acetate, ethanol, diethanol amine, g-C
3n
4mass ratio=1: 15:20: 2.0 ratio is mixed, strong agitation 6h; Then mixed system is transferred in polytetrafluoroethyllining lining autoclave, 180 ℃ of reaction 48h, afterwards after filtration, (frequency is 40KH in ultrasonic dispersion
z, power is 600W), washing, repeat after four times, filtration cakes torrefaction, and in air atmosphere 500 ℃ of roasting 1h; Cooling rear grind into powder.
Reference examples 2
In order to carry out Contrast on effect with embodiment, choose reference examples 2.Reference examples 2 adopts two-part solvent-thermal method, but does not adopt ultrasonic dispersion technology.ZnO/g-C
3n
4preparation according to zinc acetate, ethanol, diethanol amine, g-C
3n
4mass ratio=1: the ratio of 15: 20: 2.0 is mixed, strong agitation 6h; Then mixed system is transferred in polytetrafluoroethyllining lining autoclave to 150 ℃ of reaction 20h, 190 ℃ of reaction 36h; Afterwards after filtration, agitator treating, repeat after four times, filtration cakes torrefaction, opens 500 ℃ of roasting 1h in air atmosphere; Cooling rear grind into powder.
Subordinate list embodiment, reference examples specific area and MO degradation rate table
Methyl orange in table (MO) degradation experiment condition is: catalytic amount is 1g/L, and methyl orange (MO) concentration is 20ml/L, radiation of visible light 3h.
From the result of subordinate list, the composite photo-catalyst of preparing according to two-part solvent heat-ultra-sonic dispersion method of the present invention has good photocatalytic activity.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (7)
1. a ZnO/g-C
3n
4the preparation method of composite photo-catalyst, is characterized in that, concrete steps are:
By raw material, be zinc acetate, ethanol, diethanol amine, protonated g-C
3n
4, be uniformly mixed 1～10h; Then mixed system is transferred in polytetrafluoroethyllining lining autoclave to 110～160 ℃ of solvent thermal reaction 10～50h, 160～200 ℃ of solvent thermal reaction 10～50h; Cooled and filtered, filter cake disperses in deionized water for ultrasonic, washing, filter, repeatedly, until filtrate pH is 6.8～7.2, filter cake is dried in supersound washing, and in air atmosphere 450～600 ℃ of roasting 1～10h; Obtain ZnO/g-C
3n
4composite photo-catalyst powder.
2. a kind of ZnO/g-C as claimed in claim 1
3n
4the preparation method of composite photo-catalyst, is characterized in that, at ZnO/g-C
3n
4the preparatory phase of photochemical catalyst, adopts two-part solvent heat treatment method, 110～160 ℃ of processing 10～50h of low-temperature zone, 160～200 ℃ of processing 10～50h of high temperature section.
3. a kind of ZnO/g-C as claimed in claim 1
3n
4the preparation method of composite photo-catalyst, is characterized in that, at ZnO/g-C
3n
4the preparatory phase of photochemical catalyst, adopts ultrasonic dispersion washing methods, by filter cake ultrasonic cleaning filtrate pH, is 6.8～7.2.
4. a kind of ZnO/g-C as claimed in claim 1
3n
4the preparation method of composite photo-catalyst, is characterized in that, described material quality is than being zinc acetate: ethanol: diethanol amine: protonated g-C
3n
4=1:(5.0～50.0): (10.0～50.0): (0.1～10.0).
5. a kind of ZnO/g-C as claimed in claim 1
3n
4znO/g-C prepared by the preparation method of composite photo-catalyst
3n
4composite photo-catalyst, is characterized in that, described ZnO/g-C
3n
4photochemical catalyst has porous ZnO nanocrystal, and granular size is 20～150nm.
6. a kind of ZnO/g-C as claimed in claim 1
3n
4the preparation method of composite photo-catalyst, is characterized in that, the time of being uniformly mixed is 3～7h.
7. a kind of ZnO/g-C as claimed in claim 1
3n
4the preparation method of composite photo-catalyst, is characterized in that, roasting time is 3～7h.
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