CN109701584A - A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method and application - Google Patents
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method and application Download PDFInfo
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Abstract
The invention belongs to visible-light photocatalyst technical fields, are related to graphite-like carbon nitride photocatalyst more particularly to a kind of Z-type light-catalyst ZnO/Fe2O3/g‑C3N4Preparation method and.The present invention prepares pure graphite-like carbonitride with thermal polycondensation process in tube furnace first, is milled into powder after being cooled to room temperature；Graphite-like carbonitride, zinc nitrate and ferric nitrate are sufficiently mixed in deionized water；Then aqueous slkali is added, zinc ion and iron ion is made to be deposited in the surface of graphite-like carbonitride completely, realizes and is rinsed repeatedly after being separated by solid-liquid separation with deionized water and ethyl alcohol；Finally by obtained powder metallurgy calcine, after being cooled to room temperature to get.Preparation process reaction condition of the present invention is simple, by the modification to graphite-like carbonitride, reaches efficient fast degradation tetracycline.Waste water of the removal containing tetracycline is simulated by experiment, the results showed that, the rate of photocatalytic oxidation to tetracycline is 7.6 times of pure graphite-like carbonitride before modified, provides reliable theory and practice support for practical application.
Description
Technical field
The invention belongs to visible-light photocatalyst technical fields, are related to graphite-like carbon nitride photocatalyst more particularly to one
Kind Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method and application.
Background technique
In recent years, as livestock and poultry breeding industry quickly develops, while bringing economic development, the pollutant of aquaculture industry
Serious harm is also resulted in environment, pollutant includes various used in fecal pollution and treatment animal infectious disease
Antibiotic.In all antibiotic, tetracycline antibiotics are largely used due to cheap in countries in the world, and usage amount accounts for
More than half of all antibiotic, and its property is stablized, and is easy to remain in the environment, be difficult in the short time degradable.Therefore,
The method for needing a kind of efficient, the thorough innoxious removal tetracycline antibiotics of energy.
The method for being usually used in removing organic pollutants tetracycline includes bioanalysis, physical method, chemical method and photocatalysis
Method etc., be compared with other methods photocatalytic method with high catalytic efficiency, low energy consumption and stability is strong, and degrade do not generate thoroughly
The advantages that secondary pollution, has considerable application prospect.Current photochemical catalyst it is generally existing it is low to the utilization rate of visible light and
The defects such as photocatalysis efficiency is low, thus it is possible to which the research of the photochemical catalyst of tetracycline is particularly important in efficient degradation water.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is disclose a kind of ZnO/Fe2O3/g-C3N4 Z
The preparation method of type photochemical catalyst.
Technical solution:
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, thermal polycondensation process first prepares pure graphite in tube furnace
Class carbonitride is milled into powder after being cooled to room temperature；Graphite-like carbonitride, zinc nitrate and ferric nitrate is abundant in deionized water
Mixing；Then aqueous slkali is added, zinc ion and iron ion is made to be deposited in the surface of graphite-like carbonitride completely, realizes and is separated by solid-liquid separation
It is rinsed afterwards with deionized water and ethyl alcohol multiple；Finally by obtained powder metallurgy calcine, after being cooled to room temperature to get.
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, include the following steps:
A) graphite-like carbon nitride precursor is placed in Muffle furnace, 500~600 DEG C of 2~4.0h of heating under nitrogen atmosphere, preferably
550 DEG C of heating 3h, heating rate are 2.5~3.5 DEG C of min-1, nitrogen flow holding 2~5L min-1, ground after being cooled to room temperature
At powder, as graphite-like carbonitride；
B) graphite-like carbonitride, zinc nitrate and ferric nitrate are sequentially added in deionized water, be sufficiently stirred 6~12h obtain mixing it is molten
Liquid, wherein the molar ratio of zinc nitrate and ferric nitrate is 1:1~3:1, graphite-like carbonitride, zinc nitrate, ferric nitrate and deionized water
Solid-liquid mass volume ratio be 1g:0.1~0.2g:0.005~0.1g:100mL, preferably graphite-like carbonitride, zinc nitrate, nitric acid
Iron and the solid-liquid mass volume ratio of deionized water are 1g:0.1g:0.07g:100mL；
C) aqueous slkali of 0.5~2mol/L is slowly added in above-mentioned mixed solution, it is complete to precipitating that 3~6h is sufficiently stirred；
D) mixed solution is centrifugated, is rinsed repeatedly with deionized water and ethyl alcohol, 80~100 DEG C of drying are milled into powder, obtain
The graphite-like carbonitride oxide carried to zinc-iron layered bi-metal；
E) by the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal in 200~350 DEG C of 1~3h of calcining, preferably 300 DEG C
2h is calcined, powder is milled into after being cooled to room temperature, obtains Z-type light-catalyst ZnO/Fe2O3/g-C3N4。
In the more excellent disclosed example of the present invention, graphite-like carbon nitride precursor described in step a) be thiocarbamide, urea or dicyanodiamine,
It is preferred that urea.
In the more excellent disclosed example of the present invention, aqueous slkali described in step c) is potassium hydroxide, sodium hydroxide or ammonium hydroxide, preferably hydrogen-oxygen
Change potassium.
The light-catalyst ZnO of Z-type prepared by the present invention/Fe2O3/ g-C3N4For zinc-iron layered bi-metal oxide, can use
[M2+ 1-xM3+ x(OH)2]x+[(An-)x/n•mH2O] it indicates, wherein M2+Indicate Zn2+, M3+Indicate Fe3+, An−Indicate NO3 −And CO3 2−。
Another object of the present invention is to disclose obtained Z-type light-catalyst ZnO/Fe2O3/g-C3N4Using
Tetracycline is removed in waste water.
Waste water of the simulated light catalytic elimination containing tetracycline is tested, using 500W xenon lamp come simulated solar irradiation, with the filter of 420nm
Mating plate filters out ultraviolet light, and the simulated wastewater containing tetracycline that laboratory is prepared is 10mg/L, adds 25mg in 50mL solution
When prepared composite photo-catalyst, under the irradiation of simulated visible light, when 120min, is reachable to the degradation rate of tetracycline
90.28%, reliable theories integration is provided to be further widely used in industry, there is important directive significance.
The invention has the characteristics that
(1) graphite-like carbonitride is prepared using simple thermal polycondensation process, preparation process is simple, and by-product will not generate danger to environment
Evil；
(2) the Z-type photochemical catalyst synthesized, surface have many pore structures, and specific surface area is opposite to be had greatly with pure graphite-like carbonitride
Amplitude is promoted, and provides more active sites for light-catalyzed reaction；
(3) the Z-type light-catalyst ZnO/Fe synthesized2O3/g-C3N4, the absorption region to visible light can not only be significantly widened, simultaneously
It can inhibit the compound of photo-generate electron-hole pairs, photocatalysis efficiency is promoted obviously, had broad application prospects.
Beneficial effect
The present invention discloses a kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method and application, preparation process reaction condition
Simply, by the modification to graphite-like carbonitride, reach efficient fast degradation tetracycline.Contain tetracycline by experiment simulation removal
Waste water, the results showed that, the rate of photocatalytic oxidation to tetracycline is 7.6 times of pure graphite-like carbonitride before modified, is practical
It is supported using reliable theory and practice is provided.
Specific embodiment
The following describes the present invention in detail with reference to examples, so that those skilled in the art more fully understand this hair
It is bright, but the invention is not limited to following embodiments.
Unless otherwise defined, term (including scientific and technical terminology) used herein above should be construed as having as belonging to the present invention
The identical meaning that those skilled in the art are commonly understood by.It will also be understood that term used herein above should be explained
To have the meaning consistent with their meanings in the content of this specification and the relevant technologies, and should not be with idealization
Or excessive form is explained, unless expressly so limiting here.
Embodiment 1
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, include the following steps:
A) graphite-like carbon nitride precursor thiocarbamide is placed in Muffle furnace, the lower 500 DEG C of heating 2h of nitrogen atmosphere, heating rate is
2.5℃•min-1, nitrogen flow holding 2L min-1, it is cooled to room temperature, is crushed into powder, as graphite-like carbonitride；
B) it weighs the graphite-like carbonitride prepared in certain mass a) to be added in 100ml deionized water, add into mixed solution
Enter molal weight than the zinc nitrate and ferric nitrate for 1:1,6h is sufficiently stirred at room temperature, stirring rate is 600r min-1, graphite
The mass ratio of class carbonitride, zinc nitrate and ferric nitrate is 1:0.1:0.005；
C) potassium hydroxide solution of 0.5mol/L is slowly added into the mixed solution prepared in step b), until completely heavy
It forms sediment, 3h is sufficiently stirred at room temperature, stirring rate is 600r min-1；
D) it after the mixed solution for obtaining step c) realizes separation of solid and liquid, is rinsed repeatedly, at 80 DEG C with deionized water and ethyl alcohol
Drying, is milled into powder, obtains the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal；
E) material that step d) obtains is calcined into 1h at 200 DEG C, it is milled into powder after being cooled to room temperature, obtains Z-type photocatalysis
Agent ZnO/Fe2O3/g-C3N4。
Obtained photochemical catalyst passes through waste water of the experiment simulation removal containing tetracycline, the results showed that, to the light of tetracycline
Catalytic degradation rate is 7.2 times of pure graphite-like carbonitride before modified.
Embodiment 2
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, include the following steps:
A) graphite-like carbon nitride precursor urea is placed in Muffle furnace, the lower 550 DEG C of heating 3h of nitrogen atmosphere, heating rate 3
℃•min-1, nitrogen flow holding 3L min-1, it is cooled to room temperature, is crushed into powder, as graphite-like carbonitride；
B) it weighs the graphite-like carbonitride prepared in certain mass a) to be added in 100ml deionized water, add into mixed solution
Enter molal weight than the zinc nitrate and ferric nitrate for 2:1,10h is sufficiently stirred at room temperature, stirring rate is 800r min-1, stone
The mass ratio of black class carbonitride, zinc nitrate and ferric nitrate is 1:0.1:0.007；
C) potassium hydroxide solution of 1mol/L is slowly added into the mixed solution prepared in step b), until precipitating completely,
6h is sufficiently stirred at room temperature, stirring rate is 700r min-1；
D) it after the mixed solution for obtaining step c) realizes separation of solid and liquid, is rinsed repeatedly, at 90 DEG C with deionized water and ethyl alcohol
Drying, is milled into powder, obtains the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal；
E) material that step d) obtains is calcined into 2h at 300 DEG C, it is milled into powder after being cooled to room temperature, obtains Z-type photocatalysis
Agent ZnO/Fe2O3/g-C3N4。
Obtained photochemical catalyst passes through waste water of the experiment simulation removal containing tetracycline, the results showed that, to the light of tetracycline
Catalytic degradation rate is 7.6 times of pure graphite-like carbonitride before modified.
Embodiment 3
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, include the following steps:
A) graphite-like carbon nitride precursor dicyanodiamine is placed in Muffle furnace, the lower 580 DEG C of heating 4h of nitrogen atmosphere, heating rate
For 3.5 DEG C of min-1, nitrogen flow holding 4L min-1, it is cooled to room temperature, is crushed into powder, as graphite-like carbonitride；
B) it weighs the graphite-like carbonitride prepared in certain mass a) to be added in 100ml deionized water, add into mixed solution
Enter molal weight than the zinc nitrate and ferric nitrate for 3:1,12h is sufficiently stirred at room temperature, stirring rate is 700r min-1, stone
The mass ratio of black class carbonitride, zinc nitrate and ferric nitrate is 1:0.15:0.1,；
C) ammonia spirit of 1.5mol/L is slowly added into the mixed solution prepared in step b), until precipitating completely,
5h is sufficiently stirred at room temperature, stirring rate is 700r min-1；
D) it after the mixed solution for obtaining step c) realizes separation of solid and liquid, is rinsed repeatedly, at 90 DEG C with deionized water and ethyl alcohol
Drying, is milled into powder, obtains the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal；
E) material that step d) obtains is calcined at 300 DEG C 2h, is milled into powder after being cooled to room temperature, obtains Z-type photocatalysis
Agent ZnO/Fe2O3/g-C3N4。
Obtained photochemical catalyst passes through waste water of the experiment simulation removal containing tetracycline, the results showed that, to the light of tetracycline
Catalytic degradation rate is 7.5 times of pure graphite-like carbonitride before modified.
Embodiment 4
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, include the following steps:
A) graphite-like carbon nitride precursor urea is placed in Muffle furnace, the lower 600 DEG C of heating 3.5h of nitrogen atmosphere, heating rate is
3℃•min-1, nitrogen flow holding 5L min-1, it is cooled to room temperature, is crushed into powder, as graphite-like carbonitride；
B) it weighs the graphite-like carbonitride prepared in certain mass a) to be added in 100ml deionized water, add into mixed solution
Enter molal weight than the zinc nitrate and ferric nitrate for 1.5:1,8h is sufficiently stirred at room temperature, stirring rate is 700r min-1, stone
The mass ratio of black class carbonitride, zinc nitrate and ferric nitrate is 1:0.2:0.09；
C) sodium hydroxide solution of 2mol/L is slowly added into the mixed solution prepared in step b), until precipitating completely,
4h is sufficiently stirred at room temperature, stirring rate is 800r min-1；
D) it after the mixed solution for obtaining step c) realizes separation of solid and liquid, is rinsed repeatedly, at 85 DEG C with deionized water and ethyl alcohol
Drying, is milled into powder, obtains the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal；
E) material that step d) obtains is calcined at 250 DEG C 3h, is milled into powder after being cooled to room temperature, obtains Z-type photocatalysis
Agent ZnO/Fe2O3/g-C3N4。
Obtained photochemical catalyst passes through waste water of the experiment simulation removal containing tetracycline, the results showed that, to the light of tetracycline
Catalytic degradation rate is 6.9 times of pure graphite-like carbonitride before modified.
Embodiment 5
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, include the following steps:
A) graphite-like carbon nitride precursor thiocarbamide is placed in Muffle furnace, the lower 550 DEG C of heating 2.5h of nitrogen atmosphere, heating rate is
2.5℃•min-1, nitrogen flow holding 3L min-1, it is cooled to room temperature, is crushed into powder, as graphite-like carbonitride；
B) it weighs the graphite-like carbonitride prepared in certain mass a) to be added in 100ml deionized water, add into mixed solution
Enter molal weight than the zinc nitrate and ferric nitrate for 2:1,10h is sufficiently stirred at room temperature, stirring rate is 800r min-1, stone
The mass ratio of black class carbonitride, zinc nitrate and ferric nitrate is 1:0.16:0.006；
C) sodium hydroxide solution of 2mol/L is slowly added into the mixed solution prepared in step b), until precipitating completely,
6h is sufficiently stirred at room temperature, stirring rate is 600r min-1；
D) it after the mixed solution for obtaining step c) realizes separation of solid and liquid, is rinsed repeatedly, at 95 DEG C with deionized water and ethyl alcohol
Drying, is milled into powder, obtains the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal；
E) material that step d) obtains is calcined at 200 DEG C 1.5h, is milled into powder after being cooled to room temperature, obtains Z-type light and urge
Agent ZnO/Fe2O3/g-C3N4。
Obtained photochemical catalyst passes through waste water of the experiment simulation removal containing tetracycline, the results showed that, to the light of tetracycline
Catalytic degradation rate is 7.0 times of pure graphite-like carbonitride before modified.
Embodiment 6
A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, include the following steps:
A) graphite-like carbon nitride precursor dicyanodiamine is placed in Muffle furnace, the lower 500 DEG C of heating 3h of nitrogen atmosphere, heating rate
For 3.5 DEG C of min-1, nitrogen flow holding 4L min-1, it is cooled to room temperature, is crushed into powder, as graphite-like carbonitride；
B) it weighs the graphite-like carbonitride prepared in certain mass a) to be added in 100ml deionized water, add into mixed solution
Enter molal weight than the zinc nitrate and ferric nitrate for 1:1,6h is sufficiently stirred at room temperature, stirring rate is 600r min-1, graphite
The mass ratio of class carbonitride, zinc nitrate and ferric nitrate is 1:0.2:0.1；
C) ammonia spirit of 1mol/L is slowly added into the mixed solution prepared in step b), until precipitating completely, in room
5h is sufficiently stirred under temperature, stirring rate is 700r min-1；
D) it after the mixed solution for obtaining step c) realizes separation of solid and liquid, is rinsed repeatedly, at 80 DEG C with deionized water and ethyl alcohol
Drying, is milled into powder, obtains the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal；
E) material that step d) obtains is calcined at 300 DEG C 2h, is milled into powder after being cooled to room temperature, obtains Z-type photocatalysis
Agent ZnO/Fe2O3/g-C3N4。
Obtained photochemical catalyst passes through waste water of the experiment simulation removal containing tetracycline, the results showed that, to the light of tetracycline
Catalytic degradation rate is 7.2 times of pure graphite-like carbonitride before modified.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (8)
1. a kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method, which comprises the steps of:
A) graphite-like carbon nitride precursor is placed in Muffle furnace, 500~600 DEG C of 2~4.0h of heating under nitrogen atmosphere, heating speed
Rate is 2.5~3.5 DEG C of min-1, nitrogen flow holding 2~5L min-1, it is crushed into powder after being cooled to room temperature, as graphite-like nitrogen
Change carbon；
B) graphite-like carbonitride, zinc nitrate and ferric nitrate are sequentially added in deionized water, be sufficiently stirred 6~12h obtain mixing it is molten
Liquid, wherein the graphite-like carbonitride, zinc nitrate, ferric nitrate and deionized water solid-liquid mass volume ratio be 1g:0.1~
0.2g:0.005~0.1g:100mL；
C) aqueous slkali of 0.5~2mol/L is slowly added in above-mentioned mixed solution, it is complete to precipitating that 3~6h is sufficiently stirred；
D) mixed solution is centrifugated, is rinsed repeatedly with deionized water and ethyl alcohol, 80~100 DEG C of drying are milled into powder, obtain
The graphite-like carbonitride oxide carried to zinc-iron layered bi-metal；
E) the oxide carried graphite-like carbonitride of zinc-iron layered bi-metal is cooled to room in 200~350 DEG C of 1~3h of calcining
It is milled into powder after temperature, obtains Z-type light-catalyst ZnO/Fe2O3/g-C3N4。
2. Z-type light-catalyst ZnO/Fe according to claim 12O3/g-C3N4Preparation method, it is characterised in that: step a)
The graphite-like carbon nitride precursor is thiocarbamide, urea or dicyanodiamine.
3. Z-type light-catalyst ZnO/Fe according to claim 12O3/g-C3N4Preparation method, it is characterised in that: step a)
It is described that graphite-like carbon nitride precursor is placed in Muffle furnace, the lower 550 DEG C of heating 3h of nitrogen atmosphere.
4. Z-type light-catalyst ZnO/Fe according to claim 12O3/g-C3N4Preparation method, it is characterised in that: step b)
The graphite-like carbonitride, zinc nitrate, ferric nitrate and deionized water solid-liquid mass volume ratio be 1g:0.1g:0.07g:
100mL。
5. Z-type light-catalyst ZnO/Fe according to claim 12O3/g-C3N4Preparation method, it is characterised in that: step c)
The aqueous slkali is potassium hydroxide, sodium hydroxide or ammonium hydroxide.
6. Z-type light-catalyst ZnO/Fe according to claim 12O3/g-C3N4Preparation method, it is characterised in that: step e)
The graphite-like carbonitride that zinc-iron layered bi-metal is oxide carried is in 300 DEG C of calcining 2h.
7. Z-type light-catalyst ZnO/Fe made from -6 any the methods according to claim 12O3/g-C3N4。
8. a kind of light-catalyst ZnO of Z-type described in claim 7/Fe2O3/g-C3N4Using, it is characterised in that: it is applied to useless
Tetracycline is removed in water.
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Application publication date: 20190503 |