CN104084228A - Oxygen-doped carbon nitride/zinc oxide photo-catalyst as well as preparation method and application thereof - Google Patents
Oxygen-doped carbon nitride/zinc oxide photo-catalyst as well as preparation method and application thereof Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses an oxygen-doped carbon nitride/zinc oxide photo-catalyst as well as a preparation method and application of the oxygen-doped carbon nitride/zinc oxide photo-catalyst. The preparation method comprises the following steps: taking dicyandiamide or melamine as a precursor, calcining to prepare a carbon nitride nanosheet; adding a zinc oxide precursor into absolute ethyl alcohol, then adding dethylenetriamine, carrying out ultrasonic dispersion and subsequently enabling dispersion liquid to be subjected to hydrothermal reaction, so as to obtain zinc oxide nano material; enabling the zinc oxide nano material and the carbon nitride nanosheet to be subjected to ultrasonic dispersion in deionized water, subsequently adding hydrogen peroxide, then carrying out hydrothermal reaction again, and thus obtaining the oxygen-doped carbon nitride/zinc oxide photo-catalyst after the reaction is ended. The oxygen-doped carbon nitride/zinc oxide photo-catalyst adopts low-cost and easily available raw materials; the preparation condition can be easily achieved; the raw materials do not need to be calcined under the condition of high temperature, so that the cost for preparing the oxygen-doped carbon nitride/zinc oxide photo-catalyst is reduced, and the popularization and application of the preparation method are facilitated; meanwhile, the photo-catalyst is low in photo-production electron-cavity compounding efficiency and high in photo-catalytic activity.
Description
Technical field
The invention belongs to technical field of function materials, be specifically related to a kind of oxygen doping carbonitride/photocatalyst of zinc oxide and preparation method thereof and application.
Background technology
In recent years, because energy crisis and problem of environmental pollution become increasingly conspicuous, utilize pollutant in photocatalyst for degrading environment as a kind of environmental friendliness and technology cheaply, and obtain extensive concern.Conventional photochemical catalyst is titanium dioxide at present.Although it is nontoxic, efficient and cheap that titanium dioxide has advantages of,, its wider energy gap causes it can only absorb in sunshine about 4% ultraviolet light, and this has limited its application greatly.Therefore, develop a kind of can be at visible light catalytic, cheap, the photochemical catalyst of stable performance or its composite are most important.
The carbonitride of graphite-like, because it has visible light catalysis activity, is studied widely, yet graphitic carbon nitride materials, due to defects such as the recombination rate in light induced electron and hole are higher, and specific area is large, and quantum conversion is low, is unfavorable for its extensive use.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is to provide a kind of preparation method of oxygen doping carbonitride/photocatalyst of zinc oxide.
The oxygen doping carbonitride/photocatalyst of zinc oxide that provides above-mentioned preparation method to make is provided.
A further object of the present invention is to provide the application of oxygen doping carbonitride/photocatalyst of zinc oxide that above-mentioned preparation method makes.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for oxygen doping carbonitride/photocatalyst of zinc oxide, comprises the following steps:
(1) take dicyandiamide or melamine as presoma, through calcining, make azotized carbon nano sheet;
(2) zinc oxide precursor is joined to absolute ethyl alcohol good, then add diethylenetriamines, after ultrasonic dispersion, dispersion liquid is carried out to hydro-thermal reaction, after reaction, obtain nano zinc oxide material;
(3) ultrasonic being scattered in deionized water of azotized carbon nano sheet that nano zinc oxide material step (2) being made and step (1) make, then add hydrogen peroxide, carry out again hydro-thermal reaction, after reaction, obtain described oxygen doping carbonitride/photocatalyst of zinc oxide.
Preferably, the described calcining concrete operations of step (1) are: presoma is warmed up to 400～600 ℃ of calcining 2～8h with 0.1～5 ℃/min, the solid abrasive obtaining is become to fine powder, then fine powder is warmed up to 400～600 ℃ of calcining 2～6h with 1～10 ℃/min.
Preferably, in step (2), the ratio of zinc oxide precursor, absolute ethyl alcohol and diethylenetriamines is (1～8) g:(10～80) mL:(0.01～4.00) mL; Hydrothermal temperature is 110～180 ℃, and the reaction time is 6～20 hours.
Preferably, in step (2), obtain nano zinc oxide material successively through absolute ethyl alcohol and deionized water washing, after filtration and dry processing, carry out again next step operation.
Preferably, the described zinc oxide precursor of step (2) is at least one in zinc acetate, zinc nitrate and zinc chloride.
Preferably, described in step (3), hydrogen peroxide volume fraction is 30%; The ratio of the hydrogen peroxide of the gross mass of nano zinc oxide material and azotized carbon nano sheet, deionized water and 30% volume fraction is (0.05～4.50) g:(10～80) mL:(1～60) mL, wherein the mass ratio of nano zinc oxide material and azotized carbon nano sheet is (0.1:9.9)～(9.9:0.1); Hydrothermal temperature is 90～170 ℃, and the reaction time is 1～10 hour.
Preferably, oxygen doping carbonitride/photocatalyst of zinc oxide that step (3) obtains, through absolute ethyl alcohol and deionized water washing successively, filters and dry processing.
Oxygen doping carbonitride/photocatalyst of zinc oxide that above-mentioned preparation method obtains.
Oxygen doping carbonitride/photocatalyst of zinc oxide of the present invention can be applicable to the organic polluting water of degrading, and prepares electrode of solar battery and water photodissociation hydrogen etc.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention adopts raw material preparation cheap and easy to get, and preparation condition is easily realized, and has reduced the cost of preparing oxygen doping carbonitride/photocatalyst of zinc oxide, is conducive to applying of this technology.
(2) oxygen doping carbonitride/photocatalyst of zinc oxide of the present invention, graphitic carbon nitride and zinc oxide carry out compound, can improve the separated of electronics and hole, and by suitable doping and compound, can reduce widely the recombination rate in electronics and hole, thereby improve its photocatalytic activity; By add hydrogen peroxide in reaction, obtain oxygen doping carbonitride/photocatalyst of zinc oxide, the combined efficiency in its light induced electron-hole is low simultaneously, and photocatalytic activity is high.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take melamine as presoma, first presoma is placed in to calcination environment, with the programming rate of 5 ℃/min, be warmed up to 600 ℃ and keep temperature calcining 2h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 10 ℃/min, be warmed up to 500 ℃ and keep temperature calcining 2h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 10 volume units, add the zinc oxide precursor (zinc acetate) of 1 mass unit, the diethylenetriamines that adds again 0.01 volume unit, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 110 ℃ of conditions, reacted 20 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 10 unit volumes of the azotized carbon nano sheet (the two mass ratio is 0.1:9.9) that makes of the nano zinc oxide material that makes of the step (2) of 0.05 mass unit and step (1), the hydrogen peroxide that adds again 30% volume fraction of 1 unit volume, transfer to again in hydrothermal reaction kettle, under 90 ℃ of conditions, react 10 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
Measure as follows the photocatalytic activity of oxygen doping carbonitride/photocatalyst of zinc oxide that the present embodiment obtains: the catalyst of getting 50 milligrams joins 50 milliliters of 15mgmL
-1methyl orange solution in, under dark condition, place 30 minutes, with ultraviolet specrophotometer, survey its light absorption value, and be converted into concentration C according to methyl orange calibration curve
0, then, under the xenon lamp with 420nm optical filter, irradiate 60 minutes, survey its light absorption value, and be converted into concentration C, according to formula, calculate degradation rate: degradation rate=(C
0-C)/C
0* 100%.
The prepared oxygen doping of the present embodiment carbonitride/photocatalyst of zinc oxide is tested, and the degradation rate of methyl orange reaches 54%.
Embodiment 2
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take dicyandiamide as presoma, first presoma is placed in to calcination environment, with the programming rate of 0.1 ℃/min, be warmed up to 400 ℃ and keep temperature calcining 8h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 1 ℃/min, be warmed up to 400 ℃ and keep temperature calcining 6h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 80 volume units, add the zinc oxide precursor (zinc nitrate) of 8 mass units, the diethylenetriamines that adds again 4 volume units, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 180 ℃ of conditions, reacted 6 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 80 unit volumes of the azotized carbon nano sheet (the two mass ratio is 9.9:0.1) that makes of the nano zinc oxide material that makes of the step (2) of 4.50 mass units and step (1), the hydrogen peroxide that adds again 30% volume fraction of 60 unit volumes, transfer to again in hydrothermal reaction kettle, under 170 ℃ of conditions, react 1 hour, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
The photocatalytic activity of the oxygen doping carbonitride/photocatalyst of zinc oxide obtaining by method mensuration the present embodiment of embodiment 1, finally records its degradation rate to methyl orange and reaches 15%.
Embodiment 3
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take dicyandiamide as presoma, first presoma is placed in to calcination environment, with the programming rate of 0.5 ℃/min, be warmed up to 500 ℃ and keep temperature calcining 3h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 5 ℃/min, be warmed up to 450 ℃ and keep temperature calcining 4h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 45 volume units, add the zinc oxide precursor (zinc chloride) of 3 mass units, the diethylenetriamines that adds again 1.0 volume units, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 130 ℃ of conditions, reacted 10 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 20 unit volumes of the azotized carbon nano sheet (the two mass ratio is 5.0:5.0) that makes of the nano zinc oxide material that makes of the step (2) of 0.30 mass unit and step (1), the hydrogen peroxide that adds again 30% volume fraction of 10 unit volumes, transfer to again in hydrothermal reaction kettle, under 110 ℃ of conditions, react 3 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
The photocatalytic activity of the oxygen doping carbonitride/photocatalyst of zinc oxide obtaining by method mensuration the present embodiment of embodiment 1, finally records its degradation rate to methyl orange and reaches 86%.
Embodiment 4
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take melamine as presoma, first presoma is placed in to calcination environment, with the programming rate of 2 ℃/min, be warmed up to 400 ℃ and keep temperature calcining 3h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 2 ℃/min, be warmed up to 500 ℃ and keep temperature calcining 2h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 40 volume units, add the zinc oxide precursor (zinc acetate) of 5 mass units, the diethylenetriamines that adds again 0.4 volume unit, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 150 ℃ of conditions, reacted 8 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 55 unit volumes of the azotized carbon nano sheet (the two mass ratio is 1.0:9.0) that makes of the nano zinc oxide material that makes of the step (2) of 0.60 mass unit and step (1), the hydrogen peroxide that adds again 30% volume fraction of 15 unit volumes, transfer to again in hydrothermal reaction kettle, under 130 ℃ of conditions, react 5 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
The photocatalytic activity of the oxygen doping carbonitride/photocatalyst of zinc oxide obtaining by method mensuration the present embodiment of embodiment 1, finally records its degradation rate to methyl orange and reaches 35%.
Embodiment 5
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take dicyandiamide as presoma, first presoma is placed in to calcination environment, with the programming rate of 4 ℃/min, be warmed up to 450 ℃ and keep temperature calcining 3h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 3 ℃/min, be warmed up to 420 ℃ and keep temperature calcining 4h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 40 volume units, add the zinc oxide precursor (zinc nitrate) of 1 mass unit, the diethylenetriamines that adds again 0.8 volume unit, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 120 ℃ of conditions, reacted 12 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 45 unit volumes of the azotized carbon nano sheet (the two mass ratio is 3.0:7.0) that makes of the nano zinc oxide material that makes of the step (2) of 1.20 mass units and step (1), the hydrogen peroxide that adds again 30% volume fraction of 20 unit volumes, transfer to again in hydrothermal reaction kettle, under 130 ℃ of conditions, react 7 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
The photocatalytic activity of the oxygen doping carbonitride/photocatalyst of zinc oxide obtaining by method mensuration the present embodiment of embodiment 1, finally records its degradation rate to methyl orange and reaches 89%.
Embodiment 6
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take dicyandiamide as presoma, first presoma is placed in to calcination environment, with the programming rate of 2.5 ℃/min, be warmed up to 480 ℃ and keep temperature calcining 6h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 8 ℃/min, be warmed up to 450 ℃ and keep temperature calcining 2h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 40 volume units, add the zinc oxide precursor (zinc chloride) of 5 mass units, the diethylenetriamines that adds again 4 volume units, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 110 ℃ of conditions, reacted 16 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 65 unit volumes of the azotized carbon nano sheet (the two mass ratio is 4.0:6.0) that makes of the nano zinc oxide material that makes of the step (2) of 2.40 mass units and step (1), the hydrogen peroxide that adds again 30% volume fraction of 60 unit volumes, transfer to again in hydrothermal reaction kettle, under 150 ℃ of conditions, react 6 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
The photocatalytic activity of the oxygen doping carbonitride/photocatalyst of zinc oxide obtaining by method mensuration the present embodiment of embodiment 1, finally records its degradation rate to methyl orange and reaches 95%.
Embodiment 7
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take melamine as presoma, first presoma is placed in to calcination environment, with the programming rate of 6 ℃/min, be warmed up to 400 ℃ and keep temperature calcining 5h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 6 ℃/min, be warmed up to 500 ℃ and keep temperature calcining 2h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 70 volume units, add the zinc oxide precursor (zinc acetate) of 1 mass unit, the diethylenetriamines that adds again 3 volume units, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 140 ℃ of conditions, reacted 14 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 50 unit volumes of the azotized carbon nano sheet (the two mass ratio is 6.0:4.0) that makes of the nano zinc oxide material that makes of the step (2) of 3.60 mass units and step (1), the hydrogen peroxide that adds again 30% volume fraction of 30 unit volumes, transfer to again in hydrothermal reaction kettle, under 120 ℃ of conditions, react 6 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
The photocatalytic activity of the oxygen doping carbonitride/photocatalyst of zinc oxide obtaining by method mensuration the present embodiment of embodiment 1, finally records its degradation rate to methyl orange and reaches 76%.
Embodiment 8
Prepare according to the following steps oxygen doping carbonitride/photocatalyst of zinc oxide:
(1) take melamine as presoma, first presoma is placed in to calcination environment, with the programming rate of 0.1 ℃/min, be warmed up to 400 ℃ and keep temperature calcining 8h, then the yellow solid obtaining is ground to form to fine powder, again fine powder is placed in to calcination environment, with the programming rate of 1 ℃/min, be warmed up to 400 ℃ and keep temperature calcining 6h, make azotized carbon nano sheet;
(2) in the absolute ethyl alcohol of 40 volume units, add the zinc oxide precursor (zinc nitrate) of 7 mass units, the diethylenetriamines that adds again 3.5 volume units, ultrasonic dispersion, then, the solution obtaining is transferred in hydrothermal reaction kettle, under 160 ℃ of conditions, reacted 8 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain nano zinc oxide material;
(3) by gross mass, be in the ultrasonic deionized water that is distributed to 50 unit volumes of the azotized carbon nano sheet (the two mass ratio is 7.0:3.0) that makes of the nano zinc oxide material that makes of the step (2) of 4.00 mass units and step (1), the hydrogen peroxide that adds again 30% volume fraction of 25 unit volumes, transfer to again in hydrothermal reaction kettle, under 110 ℃ of conditions, react 13 hours, through absolute ethyl alcohol, deionized water washing, filter and dry processing, obtain oxygen doping carbonitride/photocatalyst of zinc oxide.
The photocatalytic activity of the oxygen doping carbonitride/photocatalyst of zinc oxide obtaining by method mensuration the present embodiment of embodiment 1, finally records its degradation rate to methyl orange and reaches 68%.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under Spirit Essence of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (9)
1. a preparation method for oxygen doping carbonitride/photocatalyst of zinc oxide, is characterized in that, comprises the following steps:
(1) take dicyandiamide or melamine as presoma, through calcining, make azotized carbon nano sheet;
(2) zinc oxide precursor is joined to absolute ethyl alcohol good, then add diethylenetriamines, after ultrasonic dispersion, dispersion liquid is carried out to hydro-thermal reaction, after reaction, obtain nano zinc oxide material;
(3) ultrasonic being scattered in deionized water of azotized carbon nano sheet that nano zinc oxide material step (2) being made and step (1) make, then add hydrogen peroxide, carry out again hydro-thermal reaction, after reaction, obtain described oxygen doping carbonitride/photocatalyst of zinc oxide.
2. preparation method according to claim 1, it is characterized in that, the described calcining concrete operations of step (1) are: presoma is warmed up to 400～600 ℃ of calcining 2～8h with 0.1～5 ℃/min, the solid abrasive obtaining is become to fine powder, then fine powder is warmed up to 400～500 ℃ of calcining 2～6h with 1～10 ℃/min.
3. preparation method according to claim 1, is characterized in that, in step (2), the ratio of zinc oxide precursor, absolute ethyl alcohol and diethylenetriamines is (1～8) g:(10～80) mL:(0.01～4.00) mL; Hydrothermal temperature is 110～180 ℃, and the reaction time is 6～20 hours.
4. preparation method according to claim 1, is characterized in that, obtains nano zinc oxide material through absolute ethyl alcohol and deionized water washing in step (2), after filtration and dry processing, carries out next step operation again.
5. preparation method according to claim 1, is characterized in that, the described zinc oxide precursor of step (2) is at least one in zinc acetate, zinc nitrate and zinc chloride.
6. preparation method according to claim 1, is characterized in that, described in step (3), hydrogen peroxide volume fraction is 30%; The ratio of the hydrogen peroxide of the gross mass of nano zinc oxide material and azotized carbon nano sheet, deionized water and 30% volume fraction is (0.05～4.50) g:(10～80) mL:(1～60) mL, wherein the mass ratio of nano zinc oxide material and azotized carbon nano sheet is (0.1:9.9)～(9.9:0.1); Hydrothermal temperature is 90～170 ℃, and the reaction time is 1～10 hour.
7. preparation method according to claim 1, is characterized in that, oxygen doping carbonitride/photocatalyst of zinc oxide that step (3) obtains, through absolute ethyl alcohol and deionized water washing, filters and dry processing.
8. oxygen doping carbonitride/photocatalyst of zinc oxide, is prepared by preparation method described in claim 1～7 any one.
Oxygen claimed in claim 8 doping carbonitride/photocatalyst of zinc oxide at degraded organic polluting water, prepare the application in electrode of solar battery or water photodissociation hydrogen.
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