CN115814837A - Hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]Photocatalyst and process for producing the same - Google Patents
Hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]Photocatalyst and process for producing the same Download PDFInfo
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- 238000000034 method Methods 0.000 title abstract description 8
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- 239000000203 mixture Substances 0.000 claims abstract description 14
- 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 claims abstract description 11
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- YISOXLVRWFDIKD-UHFFFAOYSA-N bismuth;borate Chemical compound [Bi+3].[O-]B([O-])[O-] YISOXLVRWFDIKD-UHFFFAOYSA-N 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 7
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- 239000002135 nanosheet Substances 0.000 description 7
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- 229960000907 methylthioninium chloride Drugs 0.000 description 5
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- 235000019364 tetracycline Nutrition 0.000 description 5
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 3
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 3
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- OFVLGDICTFRJMM-WESIUVDSSA-N tetracycline Chemical compound C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O OFVLGDICTFRJMM-WESIUVDSSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
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- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003522 tetracyclines Chemical class 0.000 description 2
- WUUHFRRPHJEEKV-UHFFFAOYSA-N tripotassium borate Chemical compound [K+].[K+].[K+].[O-]B([O-])[O-] WUUHFRRPHJEEKV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
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- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
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- 238000011065 in-situ storage Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
Hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]A photocatalyst, belongs to the technical field of photocatalysts and can solve the problem of the existing Bi 2 O 2 [BO 2 (OH)]The invention overcomes the defects that the photo-generated electron recombination rate of the photocatalytic material is high and the light absorption range is only in the ultraviolet light section, and the invention uses Bi (NO) 3 ) 3 ·5H 2 Ultrasonic mixing of O and ethanol to obtain bismuth borate solutionLiquid, BCN and K 2 B 4 O 7 ·4H 2 Adding O into ethanol, ultrasonically mixing, then dripping bismuth nitrate solution into the ethanol, fully stirring the mixture, transferring the mixture into a reaction kettle, and reacting the mixture in a constant-temperature oven at the temperature of between 120 and 200 ℃ for 12 to 36 hours. Naturally cooling to room temperature, and carrying out suction filtration, washing and drying on the obtained product to obtain the hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]A photocatalyst. The method is simple and low in cost.
Description
Technical Field
The invention belongs to the technical field of photocatalysts, and particularly relates to a hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]A photocatalyst.
Background
Due to the large amount of pollutants such as dyes, antibiotics, phenols, pesticides, etc., many efforts have been made to treat water, such as reverse osmosis, filtration, adsorption, precipitation, chemical and biological treatment, etc. However, these methods cannot completely decompose organic matters in wastewater. In recent years, photocatalysis has been favored as a green technology that oxidizes organic pollutants to CO 2 、H 2 O or small molecules, and does not cause secondary pollution. Most of the existing reported photocatalysts have the defects of low efficiency, high cost, high toxicity and the like. Among various photocatalysts, bismuth-based photocatalysts have received much attention because of their low toxicity, good stability, special electronic structure and abundant reserves. In addition, bi 2 O 2 [BO 2 (OH)]Most photocatalysts have a structure similar to Bi 2 O 2 CO 3 The layered crystal structure, the medium band gap and the strong oxidation capability of the composite material are beneficial to improving the photocatalytic performance, and the composite material is very promisingNovel macroscopic polarized photocatalyst.
Preparation of layered photocatalyst Bi by Rui Zhang et al (CrystEngComm, 16 (2014) 4931) 2 O 2 [BO 2 (OH)]The nanosheet has internal polarity field enhanced photocatalysis, but the single photocatalyst has high photo-generated electron recombination rate and high catalytic activity reduction speed; shuuguan Li et al (Applied Surface Science,582 (2022) 152407) halogenation treatment using a halogen ion solution soaking method, I - Grafted Bi 2 O 2 [BO 2 (OH)]The nano-sheet expands the light absorption range and remarkably improves the degradation performance on BPA, but the nano-sheet only reacts to ultraviolet rays and cannot fully utilize solar energy, and Bi/OVs co-modified Bi is prepared by Xi Zhou et al (Journal of Hazardous Materials,436 (2022) 129271) by a hydrothermal method and a chemical deposition method 2 O 2 [BO 2 (OH)]The covalent ring formed by charge alternation and oxygen vacancy (surface cation → plasma metal → anion) can significantly improve the charge separation efficiency and the yield of active oxygen, but the catalyst has a single appearance and an insufficient reactive surface.
Disclosure of Invention
The invention aims at the existing Bi 2 O 2 [BO 2 (OH)]The photocatalytic material has the defects of high photon-generated electron recombination rate and light absorption range only in an ultraviolet section, and provides the Z-type heterojunction BCN/Bi which is simple to operate, controllable in morphology, capable of accelerating the carrier separation of light-excited charges, inhibiting the carrier recombination and widening the light absorption range 2 O 2 [BO 2 (OH)]A preparation method of the photocatalyst.
The invention adopts the following technical scheme:
hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]The preparation method of the photocatalyst comprises the following steps:
in the first step, bi (NO) is added 3 ) 3 ·5H 2 Ultrasonically mixing O and ethanol to obtain a bismuth borate solution;
second, BCN and K are mixed 2 B 4 O 7 ·4H 2 Adding O into ethanol, ultrasonically mixing, and dripping bismuth nitrate solutionAdding the mixture into a reaction kettle, fully stirring the mixture, transferring the mixture into the reaction kettle, and reacting the mixture in a constant-temperature oven at the temperature of between 120 and 200 ℃ for 12 to 36 hours;
thirdly, after the reaction is finished, naturally cooling to room temperature, carrying out suction filtration, washing and drying on the obtained product to obtain the hollow flower-shaped spherical Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]A photocatalyst.
Further, said Bi (NO) in the first step 3 ) 3 ·5H 2 The mass ratio of O to ethanol is 1 to 16 to 1.
Further, said Bi (NO) 3 ) 3 ·5H 2 The mass ratio of O to ethanol is 1.
Further, the BCN and K in the second step 2 B 4 O 7 ·4H 2 The mass ratio of O to ethanol is 0.01.
Further, the BCN and K 2 B 4 O 7 ·4H 2 The mass ratio of O to ethanol is 0.025.
Further, the reaction temperature in the second step is 160 ℃, and the reaction time is 24 hours.
Further, in the third step, the drying temperature is 60 ℃ and the drying time is 24 hours.
The invention has the following beneficial effects:
the method is simple and low in cost, and the hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi is prepared through in-situ hydrothermal reaction 2 O 2 [BO 2 (OH)]The photocatalyst and the prepared material have uniform appearance, stable structure and large specific surface area, and the special Z-shaped heterojunction structure can rapidly carry out photocatalytic degradation on Methylene Blue (MB) and Tetracycline (TC) under the irradiation of visible light.
Drawings
FIG. 1 is an X-ray powder diffraction spectrum of a sample prepared in example 1.
Fig. 2 is an SEM image of the sample prepared in example 1.
Fig. 3 is a TEM image of the sample prepared in example 1.
FIG. 4 is an HR-TEM image of the sample prepared in example 1.
Fig. 5 is an SEM image of the sample prepared in comparative example 1.
Fig. 6 is an SEM image of BCN.
Fig. 7 is an SEM image of the sample prepared in example 2.
Fig. 8 is an SEM image of the sample prepared in example 3.
FIG. 9 shows BCN nanosheets and Bi 2 O 2 [BO 2 (OH)]Hollow ball of flowers, BCN/Bi prepared in example 1 2 O 2 [BO 2 (OH)]BCN/Bi prepared in example 2 2 O 2 [BO 2 (OH)]And BCN/Bi prepared in example 3 2 O 2 [BO 2 (OH)]MB is degraded photocatalytically under the irradiation of visible light.
FIG. 10 shows BCN nanosheets, bi 2 O 2 [BO 2 (OH)]Hollow ball of flowers, BCN/Bi prepared in example 1 2 O 2 [BO 2 (OH)]BCN/Bi prepared in example 2 2 O 2 [BO 2 (OH)]And BCN/Bi prepared in example 3 2 O 2 [BO 2 (OH)]And (3) degrading TC in a photocatalytic manner under the irradiation of visible light.
Detailed Description
The present invention will be further described with reference to specific examples.
The BCN nanoplates used in the following examples were prepared according to the following method: 1.24 g of H 3 BO 3 Mixed with 10 g of urea, ground to a fine powder in an agate mortar and transferred to a covered corundum crucible. Subsequently, the crucible is placed in a tube furnace with the reagents, in N 2 Heating to 550 deg.C at 2.5 deg.C/min under atmosphere, maintaining for 3 hr, and naturally cooling to obtain product B doped with g-C 3 N 4 （BCN）。
Example 1
0.73g Bi(NO 3 ) 3 ·5H 2 And O is added into 10 mL of ethanol, and the mixture is subjected to ultrasonic treatment for 30 min to obtain a bismuth nitrate solution. 50 Adding mg BCN into 30 mL ethanol, performing ultrasonic treatment for 30 min, and adding 2 g K 2 B 4 O 7 ·4H 2 O stirring for 30 min. Finally, the bismuth nitrate solution is dripped into the solution and is continuously stirred for 30 min. Mixing the componentsThe resultant solution is put into a reaction kettle to react for 24 hours at 160 ℃. After the reaction is finished, naturally cooling, filtering, washing, and drying in a constant-temperature drying oven at 60 ℃ for 24 hours to obtain the hollow flower-shaped spherical Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]。
The inventors characterized the beige powder obtained in example 1 using an X-ray diffractometer, a cold field emission scanning electron microscope, and a field emission transmission electron microscope, and the results are shown in fig. 1 to 4. From the XRD results in FIG. 1, the sample was BCN/Bi 2 O 2 [BO 2 (OH)]. As can be seen from FIGS. 2 and 3, the morphology of the composite material is characterized by a nano-sheet assembled hollow open flower-like structure with a diameter of about 2 μm. Bi can be detected in high resolution TEM of FIG. 4 2 O 2 [BO 2 (OH)]The characteristic crystal lattice stripes of the (130) crystal face and the (002) crystal face of the BCN exist, and a clear crystal face interface region exists between the two phases, which indicates that the compound BCN/Bi 2 O 2 [BO 2 (OH)]The heterojunction is successfully formed in the medium.
Comparative example 1
0.73g Bi(NO 3 ) 3 ·5H 2 And O is added into 10 mL of ethanol, and the mixture is subjected to ultrasonic treatment for 30 min to obtain a bismuth nitrate solution. 2 g K 2 B 4 O 7 ·4H 2 And adding O into 30 mL of ethanol, stirring for 30 min to obtain a potassium borate solution, dripping the bismuth nitrate solution into the potassium borate solution, and continuing stirring for 30 min. And finally, putting the mixed solution into a reaction kettle to react for 24 hours at 160 ℃. After the reaction is finished, naturally cooling, carrying out suction filtration and washing, and drying in a constant-temperature drying oven at 60 ℃ for 24 hours to obtain a sample Bi 2 O 2 [BO 2 (OH)]Hollow ball flower.
Example 2
0.73g Bi(NO 3 ) 3 ·5H 2 And O is added into 10 mL of ethanol, and the mixture is subjected to ultrasonic treatment for 30 min to obtain a bismuth nitrate solution. 20 Adding mg BCN into 30 mL ethanol, performing ultrasonic treatment for 30 min, and adding 2 g K 2 B 4 O 7 ·4H 2 O stirring for 30 min. Finally, the bismuth nitrate solution is dripped into the solution and is continuously stirred for 30 min. The mixed solution is put into a reaction kettle to react for 24 hours at 160 ℃. After the reaction is finished, naturally cooling, filtering, washing, and drying in a constant-temperature drying oven at 60 DEG CDrying for 24h to obtain the hollow flower-shaped spherical Z-shaped heterojunction 20 BCN/Bi 2 O 2 [BO 2 (OH)]。
Example 3
0.73g Bi(NO 3 ) 3 ·5H 2 And O is added into 10 mL of ethanol, and the mixture is subjected to ultrasonic treatment for 30 min to obtain a bismuth nitrate solution. 100 Adding mg BCN into 30 mL ethanol, performing ultrasonic treatment for 30 min, and adding 2 g K 2 B 4 O 7 ·4H 2 O stirring for 30 min. Finally, the bismuth nitrate solution is dripped into the solution and is continuously stirred for 30 min. The mixed solution is put into a reaction kettle to react for 24 hours at 160 ℃. After the reaction is finished, naturally cooling, filtering, washing, and drying in a constant-temperature drying oven at 60 ℃ for 24 hours to obtain the hollow flower-shaped spherical Z-shaped heterojunction 100 BCN/Bi 2 O 2 [BO 2 (OH)]。
In order to prove the beneficial effects of the invention, the inventor takes MB and TC as research objects, and respectively adds BCN nano-sheet and Bi 2 O 2 [BO 2 (OH)]Hollow ball of flowers, BCN/Bi prepared in example 1 2 O 2 [BO 2 (OH)]BCN/Bi prepared in example 2 2 O 2 [BO 2 (OH)]And BCN/Bi prepared in example 3 2 O 2 [BO 2 (OH)]Degradation experiments were performed under visible light irradiation, and the results are shown in fig. 9 and 10. The results show that: BCN/Bi prepared in inventive example 1 2 O 2 [BO 2 (OH)]The photocatalytic degradation performance of the heterojunction catalyst is more excellent than that of a composite heterojunction material prepared by a single sample and other proportions. Due to the Z-type heterojunction BCN/Bi formed under the optimal proportion 2 O 2 [BO 2 (OH)]The method has the advantages of wider light absorption range, improved light utilization rate, stronger redox capability, effective promotion of charge separation and transfer, remarkable enhancement of the photocatalytic activity of BCN/BOBH in the embodiment 1, and effective photocatalytic degradation of methylene blue and tetracycline.
Claims (7)
1. Hollow flower-ball-shaped Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]A photocatalyst, characterized in that: the photocatalyst is prepared by the following methodThe following:
in the first step, bi (NO) is added 3 ) 3 ·5H 2 Ultrasonically mixing the O and the ethanol to obtain a bismuth borate solution;
second, BCN and K are added 2 B 4 O 7 ·4H 2 Adding O into ethanol, ultrasonically mixing, then dripping bismuth nitrate solution into the ethanol, fully stirring the mixture, transferring the mixture into a reaction kettle, and reacting the mixture in a constant-temperature oven at the temperature of between 120 and 200 ℃ for 12 to 36 hours;
thirdly, after the reaction is finished, naturally cooling to room temperature, carrying out suction filtration, washing and drying on the obtained product to obtain the hollow flower-shaped spherical Z-shaped heterojunction BCN/Bi 2 O 2 [BO 2 (OH)]A photocatalyst.
2. The hollow spheriform Z-type heterojunction BCN/Bi of claim 1 2 O 2 [BO 2 (OH)]A photocatalyst, characterized in that: in the first step of said Bi (NO) 3 ) 3 ·5H 2 The mass ratio of O to ethanol is 1 to 16 to 1.
3. The hollow spheriform Z-type heterojunction BCN/Bi of claim 2 2 O 2 [BO 2 (OH)]A photocatalyst, characterized in that: the Bi (NO) 3 ) 3 ·5H 2 The mass ratio of O to ethanol is 1.
4. The hollow spheriform Z-type heterojunction BCN/Bi of claim 1 2 O 2 [BO 2 (OH)]A photocatalyst, characterized in that: in the second step, said BCN, K 2 B 4 O 7 ·4H 2 The mass ratio of O to ethanol is 0.01.
5. The hollow spheriform Z-type heterojunction BCN/Bi of claim 4 2 O 2 [BO 2 (OH)]A photocatalyst, characterized in that: the BCN and K 2 B 4 O 7 ·4H 2 The mass ratio of O to ethanol is 0.025.
6. The hollow spheriform Z-type heterojunction BCN/Bi of claim 1 2 O 2 [BO 2 (OH)]A photocatalyst, characterized in that: in the second step, the reaction temperature is 160 ℃, and the reaction time is 24 hours.
7. The hollow spheriform Z-type heterojunction BCN/Bi of claim 1 2 O 2 [BO 2 (OH)]A photocatalyst, characterized in that: in the third step, the drying temperature is 60 ℃, and the drying time is 24 hours.
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