CN109985657A - BiVO4/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst - Google Patents
BiVO4/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 50
- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 63
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000002604 ultrasonography Methods 0.000 claims abstract description 18
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000012719 thermal polymerization Methods 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 1
- 229920000877 Melamine resin Polymers 0.000 abstract description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 abstract description 7
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 238000006731 degradation reaction Methods 0.000 abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 238000005215 recombination Methods 0.000 abstract description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 4
- 229940043267 rhodamine b Drugs 0.000 abstract description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 11
- 238000003756 stirring Methods 0.000 description 11
- 239000010410 layer Substances 0.000 description 8
- 229910002651 NO3 Inorganic materials 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 5
- 229910000474 mercury oxide Inorganic materials 0.000 description 5
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000004435 EPR spectroscopy Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 125000004193 piperazinyl group Chemical group 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention discloses a kind of BiVO4/2D g‑C3N4The preparation method of Z-type heterojunction photocatalyst, method particularly includes: first pass through hydro-thermal reaction method preparation BiVO4, thermal polymerization melamine preparation graphite phase carbon nitride (g-C3N4), it removes to obtain 2D g-C by thermal oxide3N4, then using methanol as solvent, BiVO is prepared by ultrasound assisted chemical absorption method4/2D g‑C3N4Z-type heterojunction photocatalyst.BiVO prepared by the present invention4/2D g‑C3N4In Z-type heterojunction photocatalyst, 2D g-C3N4It is distributed in BiVO4Surface formed Z-type heterojunction structure, can quick separating light induced electron and hole, improve the photoelectronic service life, reduce photo-generate electron-hole recombination rate, there is good response to visible light, after 40min is reacted in catalysis, the degradation rate of rhodamine B solution can reach 93.0%.The material can be used for light degradation organic pollutant, have great importance to environmental improvement.
Description
Technical field
The invention belongs to photocatalyst technology fields, are related to a kind of BiVO4/2D g-C3N4Z-type heterojunction photocatalyst
Preparation method.
Background technique
Photocatalysis technology based on conductor oxidate, does not pollute by its own, completes simple process, can
As reaction light source and the good characteristics such as clean energy resource directly can be produced using solar energy, become object of curbing environmental pollution at present
Relatively effective technology.BiVO4As a kind of novel semiconductor material, band gap is narrow (2.40eV or so), can with outstanding
Light-exposed response, conduction band and valence band location (contrast standard hydrogen electrode) are suitable, are to have photodissociation aquatic products oxygen, reduction, degradation dirty simultaneously
Contaminate a kind of effective semiconductor light-catalyst of object ability.However, BiVO4Photochemical catalyst have charge transport ability it is poor, it is compound fastly,
The features such as adsorptivity is poor limits its photocatalytic activity.BiVO4Constructing appropriate composite photocatalyst material with other semiconductors is
Photogenerated charge separation is improved, extends photo-generate electron-hole to one of service life effective way.
g-C3N4A kind of organic polymer semiconductor, be as formed by the carbonitride thin slice stacked in multi-layers of single layer, have with
Lamellar structure as graphite dilute phase, therefore referred to as class graphite phase carbon nitride.Basic composed structure unit on its layer can be by three
Piperazine ring (C3N3) and seven piperazine ring (C6N7) constitute.In both structural units, sp occurs for C, N atom2Hydridization passes through PzTrack
Upper lone pair electrons form the big pi bond for being similar to benzene ring structure, form the conjugated system of a height delocalization.g-C3N4Lead
Band is by C atom PzTrack composition, conduction band positions are about -1.30eV；And valence band is then by the P of N atomzTrack composition, valence band
Position is about 1.40eV, g-C3N4Band gap width be 2.70eV.It is known that by BiVO4And g-C3N4Photochemical catalyst is compound
At hetero-junctions, photocatalytic activity can be promoted.
The preparation method of the prior art, there are photo-generated carriers by the body mutually big, photo-generate electron-hole to surface transmission range
Pair the high disadvantage of recombination rate, make BiVO4And g-C3N4Between synergistic effect be difficult to effectively play, limit its photocatalysis
It is active to further increase.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of BiVO4/2D g-C3N4The system of Z-type heterojunction photocatalyst
Preparation Method, the Z-type heterojunction photocatalyst of preparation can promote charge to efficiently separate, have highlight catalytic active, this is compound
2D g-C in photochemical catalyst3N4It is distributed in BiVO4Surface recombination form Z-type heterojunction structure, fully using both high oxygen
Change and reducing power, meanwhile, the g-C after thermal oxide removing3N4The conduction band edge (CB) is mobile to more negative position, so that photoproduction
Transmission range of the carrier by body mutually to surface reduces, and improves the separative efficiency in light induced electron and hole, effectively improves light
Catalytic performance.It is with a wide range of applications in fields such as environment pollution control, the energy.
The present invention is implemented as follows:
A kind of BiVO4/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, specifically includes the following steps:
S1, BiVO is prepared using hydro-thermal reaction method4:
With Bi (NO3)3·5H2O is that raw material is dissolved in the HNO that concentration is 2mol/L3Solution is sufficiently stirred to form solution A；With
NH4VO3It is dissolved in the NaOH solution that concentration is 2mol/L for raw material, is sufficiently stirred to form B solution；B solution is poured slowly into solution A
In, and be stirred continuously, yellow mixture suspension is formed, it is 7~9 that the NaOH solution for the use of concentration being 2mol/L, which adjusts pH value,
After being sufficiently stirred, the BiVO that will prepare4Precursor liquid, which pours into, carries out hydro-thermal reaction in water heating kettle, be cooled to room temperature to reaction kettle,
Sample is washed with water and ethyl alcohol respectively, drying obtains the BiVO of yellow4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
C will be housed3N3(NH2)3Crucible be put into Muffle furnace, be fired to 550 DEG C with the heating rate of 4 DEG C/min, calcining
4h is cooled to room temperature, grinding, and obtained sample is body phase g-C3N4；
S3, hot soarfing are from obtaining 2D g-C3N4:
Take body phase g-C made from step S23N4Hot soarfing is carried out in air atmosphere from existing with 4~5 DEG C/min of heating rate
2~4h is calcined at 550 DEG C, obtains 2D g-C3N4；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 2D g-C3N4It is dispersed in methanol solution, carries out ultrasonic reaction at room temperature, later, BiVO is added4, continue ultrasound
1h, and stirred for 24 hours in draught cupboard, after methanol volatilization, products therefrom and the dry 12h at 60 DEG C are collected, BiVO is obtained4/2D
g-C3N4Z-type heterojunction photocatalyst.
Preferably, the Bi (NO being added in step S13)3·5H2O and NH4VO3Molar ratio is 1:1.
Preferably, hydro-thermal reaction is that 12h is reacted at 180 DEG C in step S1, and the temperature of drying is 80 DEG C, and drying time is
6-12h。
Preferably, hot soarfing is controlled in step S3 from obtained 2D g-C3N4Quality is hot soarfing from precursor phase g-C3N4Quality
4%~6%.
Preferably, the time of ultrasonic reaction is 1~2h in step S4, and ultrasonic power is 100~150W.
Preferably, 2D g-C in step S43N4The relationship of additional amount and methanol additional amount is 10mg~90mg/100mL.
Preferably, BiVO in step S44Additional amount and 2D g-C3N4The mass ratio of additional amount is (0.1~10): 1.
Compared with prior art, the invention has the following advantages:
BiVO of the invention4/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst is simple, easily operated, cost
It is low and environmental-friendly.The Z-type heterojunction photocatalyst of preparation can promote charge to efficiently separate, have highlight catalytic active, should
2D g-C in photochemical catalyst3N4It is distributed in BiVO4Surface recombination form Z-type heterojunction structure, fully using both high oxygen
Change and reducing power, meanwhile, the g-C after thermal oxide removing3N4The conduction band edge (CB) is mobile to more negative position, so that photoproduction
Transmission range of the carrier by body mutually to surface reduces, and improves the separative efficiency in light induced electron and hole, makes it have quickly
Photo-generate electron-hole separating effect and electron transfer capabilities, improve the photoelectronic service life, make composite photo-catalyst have more
Efficient photocatalytic activity.It is with a wide range of applications in fields such as environment pollution control, the energy.
Detailed description of the invention
Fig. 1 is BiVO prepared by embodiment 14、2D g-C3N4And BiVO4/2D g-C3N4Z-type heterojunction photocatalyst
XRD spectrum；
Fig. 2 is BiVO prepared by embodiment 14/2D g-C3N4The SEM of Z-type heterojunction photocatalyst schemes；
Fig. 3 is BiVO prepared by embodiment 14/2D g-C3N4The High-Resolution Map of Z-type heterojunction photocatalyst；
Fig. 4 is BiVO prepared by embodiment 14、2D g-C3N4And BiVO4/2D g-C3N4Z-type heterojunction photocatalyst exists
The effect picture of rhodamine B degradation under radiation of visible light；
Fig. 5 a is BiVO prepared by embodiment 14、2D g-C3N4And BiVO4/2D g-C3N4Z-type heterojunction photocatalyst
Electron spin resonance figure；
Fig. 5 b is BiVO prepared by embodiment 14、2D g-C3N4And BiVO4/2D g-C3N4Z-type heterojunction photocatalyst
Electron spin resonance figure.
Specific embodiment
Below with reference to the attached drawing exemplary embodiment that the present invention will be described in detail, feature and aspect of performance.
The present invention provides a kind of BiVO4/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, it is anti-to first pass through hydro-thermal
Method is answered to prepare BiVO4, thermal polymerization melamine preparation graphite phase carbon nitride (g-C3N4), it removes to obtain 2D g- by thermal oxide
C3N4, then using methanol as solvent, BiVO is prepared by ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalysis
Agent, the specific steps are that:
S1, BiVO is prepared using hydro-thermal reaction method4:
With Bi (NO3)3·5H2O is that raw material is dissolved in the HNO that concentration is 2mol/L3Solution is sufficiently stirred to form solution A；With
NH4VO3It is dissolved in the NaOH solution that concentration is 2mol/L for raw material, is sufficiently stirred to form B solution；Bi(NO3)3·5H2O and NH4VO3
Molar ratio is 1:1；B solution is poured slowly into solution A, and is stirred continuously, yellow mixture suspension is formed, is using concentration
It is 7~9, after being sufficiently stirred that the NaOH solution of 2mol/L, which adjusts pH value, the BiVO that will be prepared4Precursor liquid pour into water heating kettle
12h is reacted at 180 DEG C and carries out hydro-thermal reaction, is cooled to room temperature to reaction kettle, is dried after washing sample with water and ethyl alcohol respectively, is dried
Dry temperature is 80 DEG C, and drying time 6-12h obtains the BiVO of yellow4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
C will be housed3N3(NH2)3Crucible be put into Muffle furnace, be fired to 550 DEG C with the heating rate of 4 DEG C/min, calcining
4h is cooled to room temperature, grinding, and obtained sample is body phase g-C3N4；
S3, hot soarfing are from obtaining 2D g-C3N4:
Take body phase g-C made from step S23N4Hot soarfing is carried out in air atmosphere from existing with 4~5 DEG C/min of heating rate
2~4h is calcined at 550 DEG C, obtains 2D g-C3N4, hot soarfing is controlled from obtained 2D g-C3N4Quality is hot soarfing from precursor phase g-
C3N4The 4%~6% of quality reaches best hot peeling effect；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 2D g-C3N4It is dispersed in the beaker containing methanol, 2D g-C3N4The relationship of additional amount and methanol additional amount is
10mg~90mg/100mL, carries out ultrasonic reaction at room temperature, and the time of ultrasonic reaction is 1~2h, and ultrasonic power is 100~
BiVO is added later in 150W4, continue ultrasound 1h, and stir for 24 hours in draught cupboard, after methanol volatilization, collect products therefrom simultaneously
Dry 12h, obtains BiVO at 60 DEG C4/2D g-C3N4Z-type heterojunction photocatalyst.
Embodiment 1
S1, BiVO is prepared using hydro-thermal reaction method4:
Weigh 0.58g bismuth nitrate (Bi (NO3)3·5H2O the concentration for) being dissolved in 10mL is the HNO of 2mol/L3In solution, sufficiently
Solution A is formed after stirring 30min.Weigh 0.14g ammonium metavanadate (NH4VO3) be dissolved in 10mL concentration be 2mol/L NaOH it is molten
Liquid forms B solution after 30min is sufficiently stirred.B solution is poured slowly into solution A, and is stirred continuously, yellow mixture is formed
Suspension, adjusting pH value using NaOH solution is 7,30min is sufficiently stirred later, the BiVO that will be prepared4Precursor liquid pours into water
In hot kettle, it is put into hydro-thermal 12h in 180 DEG C of baking ovens after water heating kettle is tightened sealing, is cooled to room temperature to reaction kettle, with water and ethyl alcohol
Sample is washed, lower layer's yellow mercury oxide is taken, 80 DEG C of drying 6h obtain yellow BiVO4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
Crucible equipped with 1g melamine is put into Muffle furnace, 550 DEG C is fired to the heating rate of 4 DEG C/min, forges
4h is burnt, room temperature is cooled to, is ground, obtained sample is body phase g-C3N4。
S3, hot soarfing are from obtaining 2D g-C3N4:
The body phase g-C that will be obtained3N4In air atmosphere, it is put into Muffle furnace, is fired to the heating rate of 4 DEG C/min
550 DEG C, 2h is calcined, 2D g-C is obtained3N4；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 50mg2D g-C3N4It is dispersed in the beaker containing 100mL methanol, places the beaker in ultrasonic bath 1h to obtain
Obtain uniform g-C3N4Dispersion.Later, 50mgBiVO is added4, continue ultrasound 1h, and stir for 24 hours in draught cupboard.Methanol is waved
After hair, products therefrom and the dry 12h at 60 DEG C are collected, BiVO is obtained4/2D g-C3N4Z-type heterojunction photocatalyst.
Fig. 1 is BiVO prepared by embodiment 14、2D g-C3N4And BiVO4/2D g-C3N4Z-type heterojunction photocatalyst
XRD spectrum, the BiVO in map4Diffraction maximum and BiVO4Monocline crystal phase (JCPDSNo.14-0688) it is corresponding, and feature is spread out
It penetrates that peak is sharp, shows that the sample of this method preparation is the good monoclinic phase BiVO of crystallinity4.2D g-C in map3N4It is located at
27.46 ° and 21.60 ° of two diffraction maximums are respectively belonging to 2D g-C3N4(JCPDSNo.87-1526) (002) and (100) is brilliant
Face, this is the regularly arranged feature in the stacked in multi-layers and triazine plane of a loop of carbonitride.For the BiVO of preparation4/2D g-C3N4Z
The XRD spectrum of type heterojunction photocatalyst contains monoclinic phase BiVO in map4With 2D g-C3N4All diffraction maximums, show
Composite material is only by BiVO4With 2D g-C3N4Two kinds of material compositions exist without other impurity.
Fig. 2 is BiVO prepared by embodiment 14/2D g-C3N4The SEM spectrum of Z-type heterojunction photocatalyst has sheet
The 2D g-C of structure3N4It is distributed in BiVO4On particle, illustrate that the two has been compounded to form Z-type heterojunction structure.
Fig. 3 is BiVO prepared by embodiment 14/2D g-C3N4The high-resolution map of Z-type heterojunction photocatalyst, map
Middle interplanar distance is about that 0.309nm corresponds to BiVO4(121) crystal face.In contrast, with BiVO4Closely coupled crystallinity
Weaker, the fuzzy region of lattice belongs to 2D g-C3N4Phase.Show BiVO4With 2D g-C3N4Form close interface.Theoretically
It says, this intimate interfacial can be used as carrier pathway, is conducive to carrier transfer, improves photocatalysis performance.
Fig. 4 is BiVO prepared by embodiment 14、2D g-C3N4And BiVO4/2D g-C3N4Z-type heterojunction photocatalyst exists
The effect picture of rhodamine B degradation under radiation of visible light.A-quadrant is dark surrounds in figure, and B area is radiation of visible light, from
Light irradiation starts timing, BiVO4/2D g-C3N4Z-type hetero-junctions is after 40min is reacted in catalysis, and the degradation rate of rhodamine B solution is
Reach 93.0%, illustrates BiVO4/2D g-C3N4Z-type hetero-junctions has excellent photocatalytic activity under visible light.Moreover, from
Comparison is it is found that BiVO in figure4/2D g-C3N4The photocatalytic activity of Z-type hetero-junctions is substantially better than BiVO4With 2D g-C3N4。
Fig. 5 a and Fig. 5 b are BiVO prepared by embodiment 14、2D g-C3N4And BiVO4/2D g-C3N4Z-type hetero-junctions light
The electron spin resonance figure of catalyst.Show O2-With the chief active species that OH is in photocatalytic process.In addition, in conjunction with
BiVO4With 2D g-C3N4Band structure, it was demonstrated that the BiVO formed4/2D g-C3N4Z-type hetero-junctions.
Embodiment 2
S1, BiVO is prepared using hydro-thermal reaction method4:
Weigh 0.58g bismuth nitrate (Bi (NO3)3·5H2O the concentration for) being dissolved in 10mL is the HNO of 2mol/L3In solution, sufficiently
Solution A is formed after stirring 30min.Weigh 0.14g ammonium metavanadate (NH4VO3) be dissolved in 10mL concentration be 2mol/L NaOH it is molten
Liquid forms B solution after 30min is sufficiently stirred.B solution is poured slowly into solution A, and is stirred continuously, yellow mixture is formed
Suspension, adjusting pH value using NaOH solution is 7,30min is sufficiently stirred later, the BiVO that will be prepared4Precursor liquid pours into water
In hot kettle, it is put into hydro-thermal 12h in 180 DEG C of baking ovens after water heating kettle is tightened sealing, is cooled to room temperature to reaction kettle, with water and ethyl alcohol
Sample is washed, lower layer's yellow mercury oxide is taken, 80 DEG C of drying 6h obtain yellow BiVO4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
Crucible equipped with 1g melamine is put into Muffle furnace, 550 DEG C is fired to the heating rate of 4 DEG C/min, forges
2h is burnt, room temperature is cooled to, is ground, obtained sample is body phase g-C3N4。
S3, hot soarfing are from obtaining 2D g-C3N4:
The body phase g-C that will be obtained3N4In air atmosphere, it is put into Muffle furnace, is fired to the heating rate of 4 DEG C/min
550 DEG C, 2h is calcined, 2D g-C is obtained3N4；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 10mg2D g-C3N4It is dispersed in the beaker containing 100mL methanol, places the beaker in ultrasonic bath 1h to obtain
Obtain uniform g-C3N4Dispersion.Later, 90mgBiVO is added4, continue ultrasound 1h, and stir for 24 hours in draught cupboard.Methanol is waved
After hair, products therefrom and the dry 12h at 60 DEG C are collected, BiVO is obtained4/2D g-C3N4Z-type heterojunction photocatalyst.
Embodiment 3
S1, BiVO is prepared using hydro-thermal reaction method4:
Weigh 0.58g bismuth nitrate (Bi (NO3)3·5H2O the concentration for) being dissolved in 10mL is the HNO of 2mol/L3In solution, sufficiently
Solution A is formed after stirring 30min.Weigh 0.14g ammonium metavanadate (NH4VO3) be dissolved in 10mL concentration be 2mol/L NaOH it is molten
Liquid forms B solution after 30min is sufficiently stirred.B solution is poured slowly into solution A, and is stirred continuously, yellow mixture is formed
Suspension, adjusting pH value using NaOH solution is 7,30min is sufficiently stirred later, the BiVO that will be prepared4Precursor liquid pours into water
In hot kettle, it is put into hydro-thermal 12h in 180 DEG C of baking ovens after water heating kettle is tightened sealing, is cooled to room temperature to reaction kettle, with water and ethyl alcohol
Sample is washed, lower layer's yellow mercury oxide is taken, 80 DEG C of drying 6h obtain yellow BiVO4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
Crucible equipped with 1g melamine is put into Muffle furnace, 550 DEG C is fired to the heating rate of 4 DEG C/min, forges
4h is burnt, room temperature is cooled to, is ground, obtained sample is body phase g-C3N4。
S3, hot soarfing are from obtaining 2D g-C3N4:
The body phase g-C that will be obtained3N4In air atmosphere, it is put into Muffle furnace, is fired to the heating rate of 4 DEG C/min
550 DEG C, 2h is calcined, 2D g-C is obtained3N4；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 30mg2D g-C3N4It is dispersed in the beaker containing 100mL methanol, places the beaker in ultrasonic bath 1h to obtain
Obtain uniform g-C3N4Dispersion.Later, 70mgBiVO is added4, continue ultrasound 1h, and stir for 24 hours in draught cupboard.Methanol is waved
After hair, products therefrom and the dry 12h at 60 DEG C are collected, BiVO is obtained4/2D g-C3N4Z-type heterojunction photocatalyst.
Embodiment 4
S1, BiVO is prepared using hydro-thermal reaction method4:
Weigh 0.58g bismuth nitrate (Bi (NO3)3·5H2O the concentration for) being dissolved in 10mL is the HNO of 2mol/L3In solution, sufficiently
Solution A is formed after stirring 30min.Weigh 0.14g ammonium metavanadate (NH4VO3) be dissolved in 10mL concentration be 2mol/L NaOH it is molten
Liquid forms B solution after 30min is sufficiently stirred.B solution is poured slowly into solution A, and is stirred continuously, yellow mixture is formed
Suspension, adjusting pH value using NaOH solution is 7,30min is sufficiently stirred later, the BiVO that will be prepared4Precursor liquid pours into water
In hot kettle, it is put into hydro-thermal 12h in 180 DEG C of baking ovens after water heating kettle is tightened sealing, is cooled to room temperature to reaction kettle, with water and ethyl alcohol
Sample is washed, lower layer's yellow mercury oxide is taken, 80 DEG C of drying 6h obtain yellow BiVO4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
Crucible equipped with 1g melamine is put into Muffle furnace, 550 DEG C is fired to the heating rate of 4 DEG C/min, forges
4h is burnt, room temperature is cooled to, is ground, obtained sample is body phase g-C3N4。
S3, hot soarfing are from obtaining 2D g-C3N4:
The body phase g-C that will be obtained3N4In air atmosphere, it is put into Muffle furnace, is fired to the heating rate of 4 DEG C/min
550 DEG C, 2h is calcined, 2D g-C is obtained3N4；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 70mg2D g-C3N4It is dispersed in the beaker containing 100mL methanol, places the beaker in ultrasonic bath 1h to obtain
Obtain uniform g-C3N4Dispersion.Later, 30mgBiVO is added4, continue ultrasound 1h, and stir for 24 hours in draught cupboard.Methanol is waved
After hair, products therefrom and the dry 12h at 60 DEG C are collected, BiVO is obtained4/2D g-C3N4Z-type heterojunction photocatalyst.
Embodiment 5
S1, BiVO is prepared using hydro-thermal reaction method4:
Weigh 0.58g bismuth nitrate (Bi (NO3)3·5H2O the concentration for) being dissolved in 10mL is the HNO of 2mol/L3In solution, sufficiently
Solution A is formed after stirring 30min.Weigh 0.14g ammonium metavanadate (NH4VO3) be dissolved in 10mL concentration be 2mol/L NaOH it is molten
Liquid forms B solution after 30min is sufficiently stirred.B solution is poured slowly into solution A, and is stirred continuously, yellow mixture is formed
Suspension, adjusting pH value using NaOH solution is 7,30min is sufficiently stirred later, the BiVO that will be prepared4Precursor liquid pours into water
In hot kettle, it is put into hydro-thermal 12h in 180 DEG C of baking ovens after water heating kettle is tightened sealing, is cooled to room temperature to reaction kettle, with water and ethyl alcohol
Sample is washed, lower layer's yellow mercury oxide is taken, 80 DEG C of drying 6h obtain yellow BiVO4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
Crucible equipped with 1g melamine is put into Muffle furnace, 550 DEG C is fired to the heating rate of 4 DEG C/min, forges
4h is burnt, room temperature is cooled to, is ground, obtained sample is body phase g-C3N4；
S3, hot soarfing are from obtaining 2D g-C3N4:
The body phase g-C that will be obtained3N4In air atmosphere, it is put into Muffle furnace, is fired to the heating rate of 4 DEG C/min
550 DEG C, 2h is calcined, 2D g-C is obtained3N4；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 90mg2D g-C3N4It is dispersed in the beaker containing 100mL methanol, places the beaker in ultrasonic bath 1h to obtain
Obtain uniform g-C3N4Dispersion.Later, 10mgBiVO is added4, continue ultrasound 1h, and stir for 24 hours in draught cupboard.Methanol is waved
After hair, products therefrom and the dry 12h at 60 DEG C are collected, BiVO is obtained4/2D g-C3N4Z-type heterojunction photocatalyst.
To sum up, BiVO prepared by the present invention4/2D g-C3N4Z-type heterojunction photocatalyst has more efficient photocatalysis
Activity.It is with a wide range of applications in fields such as environment pollution control, the energy.
Finally, it should be noted that above-described each embodiment is merely to illustrate technical solution of the present invention, rather than it is limited
System；Although the present invention is described in detail referring to the foregoing embodiments, those skilled in the art should understand that: its
It can still modify to technical solution documented by previous embodiment, or part of or all technical features are carried out
Equivalent replacement；And these modifications or substitutions, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution
Range.
Claims (7)
1. a kind of BiVO4/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, it is characterised in that: it specifically includes following
Step:
S1, BiVO is prepared using hydro-thermal reaction method4:
With Bi (NO3)3·5H2O is that raw material is dissolved in the HNO that concentration is 2mol/L3Solution is sufficiently stirred to form solution A；With NH4VO3
It is dissolved in the NaOH solution that concentration is 2mol/L for raw material, is sufficiently stirred to form B solution；B solution is poured slowly into solution A, and
It is stirred continuously, forms yellow mixture suspension, it is 7~9 that the NaOH solution for the use of concentration being 2mol/L, which adjusts pH value, is sufficiently stirred
After mixing, the BiVO that will prepare4Precursor liquid, which pours into, carries out hydro-thermal reaction in water heating kettle, be cooled to room temperature to reaction kettle, use respectively
Water and ethyl alcohol wash sample, and drying obtains the BiVO of yellow4Sample；
S2, body phase g-C is prepared using thermal polymerization3N4:
C will be housed3N3(NH2)3Crucible be put into Muffle furnace, be fired to 550 DEG C with the heating rate of 4 DEG C/min, calcine 4h, drop
It warms to room temperature, grinds, obtained sample is body phase g-C3N4；
S3, hot soarfing are from obtaining 2D g-C3N4:
Take body phase g-C made from step S23N4Hot soarfing is carried out in air atmosphere from 4~5 DEG C/min of heating rate at 550 DEG C
2~4h of lower calcining, obtains 2D g-C3N4；
S4, BiVO is prepared using ultrasound assisted chemical absorption method4/2D g-C3N4Z-type heterojunction photocatalyst:
By 2D g-C3N4It is dispersed in methanol solution, carries out ultrasonic reaction at room temperature, later, BiVO is added4, continue ultrasound 1h,
And stirred in draught cupboard for 24 hours, after methanol volatilization, products therefrom and the dry 12h at 60 DEG C are collected, BiVO is obtained4/2D g-
C3N4Z-type heterojunction photocatalyst.
2. BiVO according to claim 14/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, feature exist
In: the Bi (NO being added in step S13)3·5H2O and NH4VO3Molar ratio is 1:1.
3. BiVO according to claim 14/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, feature exist
In: hydro-thermal reaction is that 12h is reacted at 180 DEG C in step S1, and the temperature of drying is 80 DEG C, drying time 6-12h.
4. BiVO according to claim 14/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, feature exist
In: hot soarfing is controlled in step S3 from obtained 2D g-C3N4Quality is hot soarfing from precursor phase g-C3N4The 4%~6% of quality.
5. BiVO according to claim 14/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, feature exist
In: the time of ultrasonic reaction is 1~2h in step S4, and ultrasonic power is 100~150W.
6. BiVO according to claim 14/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, feature exist
In: 2D g-C in step S43N4The relationship of additional amount and methanol additional amount is 10mg~90mg/100mL.
7. BiVO according to claim 1 or 64/2D g-C3N4The preparation method of Z-type heterojunction photocatalyst, feature
It is: BiVO in step S44Additional amount and 2D g-C3N4The mass ratio of additional amount is (0.1~10): 1.
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