CN113828334A - Ce-doped BiOBr nano photocatalyst and preparation method and application thereof - Google Patents
Ce-doped BiOBr nano photocatalyst and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 7
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 38
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- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 abstract 1
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 abstract 1
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 2
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- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
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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
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a high-efficiency nano visible light photocatalyst prepared by doping Ce element into BiOBr, a preparation method and application thereof, wherein bismuth nitrate pentahydrate (Bi (NO)3)3·5H2O), sodium bromide (NaBr), cerium nitrate hexahydrate (Ce (NO)3)3·6H2O) is used as a raw material and is prepared by adopting a one-step hydrothermal method. The method comprises the following steps: (1) adding Bi (NO)3)3·5H2O and Ce (NO)3)3·6H2Dissolving O in ethylene glycol, and performing ultrasonic treatment until the O is dissolved; (2) dissolving NaBr in ultrapure waterStirring until the mixture is dissolved; (3) the solutions in steps (1) and (2) were mixed and then stirred for 5 min without light. And after stirring, moving the mixture into a 50mL hydrothermal kettle, and reacting for 12 h in an oven at constant temperature of 160 ℃ to obtain the Ce-doped BiOBr (Ce-BiOBr) photocatalyst. The photocatalyst obtained by the invention has higher photocatalytic degradation performance on bisphenol A and antibiotic (tetracycline hydrochloride) under the irradiation of visible light (more than or equal to 420 nm), the degradation rate on bisphenol A under the irradiation of visible light for 180min is about 90%, and the degradation rate on antibiotic (tetracycline hydrochloride) within 60 min is more than 90%.
Description
Technical Field
The invention relates to a Ce-doped BiOBr nano visible light driven photocatalyst as well as preparation and application thereof, belonging to the technical field of nano materials. The catalytic target substances are bisphenol A and tetracycline hydrochloride, belong to nondegradable pollutants, and have no dye sensitization under visible light.
Background
Bismuth oxyhalides (BiOX) are a class of semiconductor materials with special layer structures, [ Bi ]2O2]2+Layer and [ X ]2]2-The layers are arranged alternately. Wherein, [ X ]2]2-The layers are bonded by van der waals forces, and the crystal structure can be adjusted to a certain extent, thereby realizing various modifications and alterations. More importantly, [ Bi ] due to the difference in electronegativity between different atoms2O2]2+Layer and [ X ]2]2-A strong electrostatic field vertical to each atomic layer is generated between the layers, and photo-generated electrons and holes can be effectively separated under the induction of the electric field, so that the BiOX has the advantage of being unique in the aspect of carrier separation and is an ideal photocatalytic material. In BiOX, the band gap width of BiOCl is 3.2-3.4 eV, and the BiOCl can only absorb ultraviolet light; the band gap width of the BiOI is narrow (about 1.7 eV), but the photogenerated holes have poor oxidizing capability; and the BiOBr has moderate band gap width (about 2.8 eV), relatively high visible light catalytic activity and stability, and is suitable for degrading organic pollutants by visible light catalysis, but the visible light utilization rate of the BiOBr in degrading organic pollutants by photocatalysis is low.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the Ce-BiOBr nano photocatalyst, the preparation method thereof and the application of the Ce-BiOBr nano photocatalyst to the degradation of emerging pollutants are provided, the band structure of BiOBr is adjusted by doping Ce element, the wavelength range of absorbable light is enlarged, the utilization rate of visible light is improved, the impedance of materials is reduced, the transport efficiency of carriers is improved, and the problem of low visible light utilization rate of the BiOBr in the photocatalytic degradation of organic pollutants is solved.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the Ce-doped BiOBr photocatalyst is composed of flaky BiOBr and Ce ions, and is a nano flaky material with the Ce ions uniformly dispersed in a BiOBr unit cell.
Preferably, the mass fraction of Ce in the Ce-doped BiOBr photocatalyst is 0.17-0.5%.
Preferably, the catalyst is a two-dimensional nano flaky photocatalyst, the size of the catalyst is D =200 nm, and the thickness of the catalyst is 30-40 nm.
The preparation method of the Ce-doped BiOBr photocatalyst comprises the following steps:
1) quantitative determination of Bi (NO)3)3·5H2O and Ce (NO)3)3·6H2Dissolving O in ethylene glycol, and performing ultrasonic treatment until the O is completely dissolved to obtain a solution I;
2) dissolving NaBr in ultrapure water, and stirring until the NaBr is dissolved to obtain a solution II;
3) mixing the solution I and the solution II, and then stirring uniformly under the condition of no light;
4) after stirring, pouring the mixture into a hydrothermal reaction kettle, then placing the reaction kettle in an oven, and fully reacting at high temperature;
5) and centrifuging, washing and drying the white precipitate to obtain white powder, namely the Ce-BiOBr high-efficiency photocatalyst.
Wherein, Bi (NO) described in step 1)3)3·5H2The molar volume ratio of O to ethylene glycol is 2 mmol: 5 mL-2 mmol: 15 mL, and the ultrasonic time in the step 1) is 5-10 min.
Said Bi (NO)3)3·5H2O, NaBr in a mass ratio of 1: 1, Ce (NO)3)3·6H2The amount of O substance is 0.1～1 mmol。
And 3) mixing the solution I and the solution II, wherein the mixing process is to stir for 5 min at a stirring speed of 300-400 rpm, and the step 4) is to perform a constant-temperature reaction for 10-12 h at a constant temperature of 150-180 ℃.
And 5) centrifuging, washing and drying the white precipitate, namely centrifuging for 3-5 min at the rotating speed of 6000-8000 rpm, respectively cleaning for 3-5 times by using ultrapure water and absolute ethyl alcohol, and finally drying for 6-8 h at 80-100 ℃ to obtain white powder.
The invention also provides an application of the Ce-doped BiOBr nano photocatalyst, and the catalyst is applied to photodegradation of pollutants bisphenol A and antibiotics (tetracycline hydrochloride) in water. The pollutants bisphenol A and the antibiotics (tetracycline hydrochloride) in the photodegradation water are degraded by using a xenon lamp and a visible light wavelength filter as a light source, and the concentration of the bisphenol A and the tetracycline is 5-10 mg/L.
Has the advantages that: compared with the prior art, the invention has the following advantages: the doping of Ce successfully introduces a doping energy level above the conduction band position of the BiOBr, Ce is used as a multi-electron atom, and after the Bi atom is replaced, redundant electrons can be transferred onto the BiOBr conduction band with lower energy, so that the number of electrons on the conduction band is increased, and more electrons participate in the generation reaction of free radicals (as shown in fig. 7 a); in addition, the existing doped modified BiOBr catalyst catalytic degradation target is colored dye, the target degradation product of the invention is bisphenol A and antibiotic, the degradation field of the photocatalyst is expanded, the dye sensitization effect (shown in figure 7 b) is avoided, dye molecules are changed into an unstable excited state after absorbing light energy, electrons on an LOMO track can jump to a conduction band of the photocatalyst, and the degradation of the dye is carried out under the action of a series of oxygen free radicals generated by the reaction of the electrons and dissolved oxygen and the like.
On the other hand, compared with the original micron-sized Ce-doped BiOBr nano photocatalyst, the Ce-doped BiOBr nano photocatalyst (Ce-BiOBr) prepared by a simple and mild hydrothermal method is reduced to the nano level; the doped metal elements are dispersed in the BiOBr unit cell, the forbidden bandwidth of the BiOBr is reduced to 2.56 eV, the corresponding absorption edge is red-shifted, and the utilization rate of visible light is increased; under the irradiation of visible light, the degradation rate of Ce-BiOBr to bisphenol A is close to 90% within 180min, and the degradation rate to tetracycline is over 90% within 60 min.
Drawings
FIG. 1 is an XRD pattern of Ce-BiOBr;
FIG. 2 (a, b) is an SEM photograph of Ce-BiOBr; (c, d) is an SEM photograph of BiOBr;
FIG. 3 is a TEM detection mapping chart of Ce-BiOBr;
FIG. 4 (a) is a diffuse reflectance graph of BiOBr and Ce-BiOBr, and FIG. 4 (b) is a Tauc curve of BiOBr and Ce-BiOBr;
FIG. 5 is a graph of the degradation profile of BiOBr and Ce-BiOBr photocatalysts for bisphenol A;
FIG. 6 is a graph of the degradation profile of BiOBr and Ce-BiOBr photocatalysts for tetracycline;
FIG. 7 is a graph comparing (a) the degradation mechanism of Ce-BiOBr to degrade non-dye contaminants and (b) photosensitization of the dye.
Detailed Description
Example 1:
the preparation method of the Ce-doped BiOBr photocatalyst comprises the following steps:
weighing 2 mmol (0.97 g) of Bi (NO)3)3·5H2O and 0.1 mmol (0.0434 g) of Ce (NO)3)3·6H2And (3) putting the O into a beaker, measuring 15 mL of glycol as a cosolvent by using a liquid transfer gun, adding the glycol into the beaker, and putting the beaker into an ultrasonic machine for ultrasonic treatment until the glycol is completely dissolved.
② weighing 2 mmol (0.206 g) NaBr, then weighing 20 mL deionized water by using a liquid transfer gun, and adding the deionized water into a beaker of NaBr for dissolution.
③ the two solutions were mixed into a beaker and then stirred for 5 min in the absence of light at a stirring speed of 400 rpm.
And fourthly, after the stirring is finished, pouring the mixture into a 50mL hydrothermal reaction kettle, and then placing the reaction kettle in an oven to react for 12 hours at 160 ℃.
Fifthly, after the reaction is finished, naturally cooling to room temperature, taking out the material, separating out the powder product by using a centrifugal machine, then washing the powder product three times by using deionized water and ethanol respectively, washing off impurities on the surface of the material, after the washing is finished, putting the material into an oven at 80 ℃ for drying for 10 hours, and cooling to obtain the Ce-BiOBr photocatalytic material.
The Ce-doped BiOBr nanosheet photocatalyst prepared by the method has the size diameter of about 100-200 nm and the thickness of about 30-40 nm. The method is applied to degradation of organic pollutants bisphenol A and tetracycline hydrochloride in water, a 500W xenon lamp is adopted as a light source, a 420 nm filter is arranged, and the concentration of bisphenol A and tetracycline is 10 mg/L.
Example 2:
the Ce doped BiOBr nanosheet photocatalyst prepared above was phase characterized using a japan science Smartlab (3) (Cu target) instrument. The results are shown in figure 1, which shows that the XRD patterns of the BiOBr material before and after doping do not change the basic morphology of the BiOBr, and the results are consistent with the basic card of the BiOBr (JCPDS No. 09-0393), which indicates that Ce is highly dispersed in the BiOBr and does not change the phase of the product.
Example 3:
and (3) identifying the surface morphology of the prepared Ce-doped BiOBr nanosheet photocatalyst by adopting a ZEISSGemini 300 instrument. Results are shown in the SEM pictures of the BiOBr and Ce-BiOBr materials shown in FIG. 2, and the mapping pictures of Ce-BiOBr, and from FIGS. 2 (a, b) and 2 (c, d), it can be seen that both Ce-BiOBr and BiOBr are nanosheet materials with uniform thickness.
Example 4:
elemental composition analysis of the Ce-doped BiOBr nanosheet photocatalyst prepared above was performed using a FEI Talos F200s instrument, and the results are shown in fig. 3 mapping, which shows that Ce was successfully doped into BiOBr and was uniformly dispersed in BiOBr.
Example 5:
the energy band structure and the absorption edge of the prepared Ce-doped BiOBr nanosheet photocatalyst are tested by a PELambda 950 instrument. Figure 4 shows that Ce doping results in a red-shift of the bibbr absorption edge, from 435 to 451 nm; and the band gap width is reduced from 2.67 eV to 2.56 eV, and the BiOBr energy band structure is successfully changed.
Example 6:
FIG. 5 shows the degradation curves of BiOBr and Ce-BiOBr nano-photocatalyst photocatalytic degradation of bisphenol A, in order to compare the difference of the BiOBr and Ce-BiOBr samples in the degradation effect of bisphenol A, 10 mg of BiOBr and Ce-BiOBr are respectively weighed and added into 40mL of 10 mg/L bisphenol A solution, and the result shows that the degradation rate of bisphenol A after 3 h of BiOBr illumination is about 30%, and the degradation rate of bisphenol A after 3 h of Ce-BiOBr illumination is close to 90%, compared with the significant improvement of the degradation rate of bisphenol A by BiOBr. The method for detecting bisphenol A is high performance liquid chromatography, the instrument is Japanese Hitachi Primaide 1430 type, the chromatographic column adopts C18 column, and the column temperature is 30 ℃.
Example 7:
figure 7 presents a graph comparing the degradation mechanism of Ce-BiOBr to non-dye contaminants versus photosensitization of the dye. The introduction of Ce doping energy level increases electrons on a BiOBr conduction band, so that the process of generating a series of oxygen radicals through the reaction of the electrons and oxygen adsorbed on the surface of the material is enhanced, the degradation efficiency of a sample on pollutants is enhanced, and the sensitization effect of the dye is avoided. As for dye molecules, the dye molecules can be changed into an unstable excited state after absorbing light energy, electrons on an LOMO orbit can jump to a conduction band of a photocatalyst, and degradation of the dye is performed under the action of a series of oxygen radicals generated by the reaction of the electrons and dissolved oxygen and the like, so that degradation performed by using the dye as a target pollutant cannot accurately evaluate the degradation performance of the photocatalyst.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The Ce-doped BiOBr photocatalyst is characterized by consisting of flaky BiOBr and Ce ions, and is a nano flaky material with the Ce ions uniformly dispersed in a BiOBr unit cell.
2. The Ce-doped BiOBr photocatalyst according to claim 1, wherein the mass fraction of Ce in the Ce-doped BiOBr photocatalyst is 0.17-0.5%.
3. The Ce-doped BiOBr photocatalyst as claimed in claim 1, wherein: the catalyst is a two-dimensional nano flaky photocatalyst, the size of the catalyst is D =200 nm, and the thickness of the catalyst is 30-40 nm.
4. The method for preparing the Ce-doped BiOBr photocatalyst according to claim 1, comprising the following steps of:
1) quantitative determination of Bi (NO)3)3·5H2O and Ce (NO)3)3·6H2Dissolving O in ethylene glycol, and performing ultrasonic treatment until the O is completely dissolved to obtain a solution I;
2) dissolving NaBr in ultrapure water, and stirring until the NaBr is dissolved to obtain a solution II;
3) mixing the solution I and the solution II, and then stirring uniformly under the condition of no light;
4) after stirring, pouring the mixture into a hydrothermal reaction kettle, then placing the reaction kettle in an oven, and fully reacting at high temperature;
5) and centrifuging, washing and drying the white precipitate to obtain white powder, namely the Ce-BiOBr high-efficiency photocatalyst.
5. The method of claim 4 for preparing a Ce-doped BiOBr photocatalyst, wherein the method comprises the following steps: bi (NO) described in step 1)3)3·5H2The molar volume ratio of O to ethylene glycol is 2 mmol: 5 mL-2 mmol: 15 mL, and the ultrasonic time in the step 1) is 5-10 min.
6. The method of claim 4 for preparing a Ce-doped BiOBr photocatalyst, wherein the method comprises the following steps: said Bi (NO)3)3·5H2O, NaBr in a mass ratio of 1: 1, Ce (NO)3)3·6H2The amount of O is 0.1 to 1 mmol.
7. The method of claim 4 for preparing a Ce-doped BiOBr photocatalyst, wherein the method comprises the following steps: and 3) mixing the solution I and the solution II, wherein the mixing process is to stir for 5 min at a stirring speed of 300-400 rpm, and the step 4) is to perform a constant-temperature reaction for 10-12 h at a constant temperature of 150-180 ℃.
8. The method of claim 4 for preparing a Ce-doped BiOBr photocatalyst, wherein the method comprises the following steps: and 5) centrifuging, washing and drying the white precipitate, namely centrifuging for 3-5 min at the rotating speed of 6000-8000 rpm, respectively cleaning for 3-5 times by using ultrapure water and absolute ethyl alcohol, and finally drying for 6-8 h at 80-100 ℃ to obtain white powder.
9. Use of a Ce-doped BiOBr photocatalyst as claimed in claim 1 in the field of nano-photocatalysts, characterized in that: the catalyst is applied to visible light degradation of pollutants bisphenol A and antibiotics (tetracycline hydrochloride) in water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114602516A (en) * | 2022-04-13 | 2022-06-10 | 华北理工大学 | Fe-doped BiOBr photo-Fenton catalytic material rich in oxygen vacancies and preparation method thereof |
| CN116371397A (en) * | 2023-01-05 | 2023-07-04 | 华南理工大学 | Ce doped Bi 0 /Bi 2 O 3 /Bi 2 O 2.75 Nanosheet photocatalyst and preparation and application thereof |
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| CN110773204A (en) * | 2019-10-29 | 2020-02-11 | 东南大学 | S-doped BiOBr nano photocatalyst and preparation and application thereof |
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| CN110773204A (en) * | 2019-10-29 | 2020-02-11 | 东南大学 | S-doped BiOBr nano photocatalyst and preparation and application thereof |
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| M. HU, ET AL.: ""Hydrothermal method to prepare Ce-doped BiOBr nanoplates with enhanced carrier transfer and photocatalytic activity"", 《MATERIALS RESEARCH BULLETIN》 * |
| 贺全宝等: ""BiOX( X = Cl，Br，I) 复合光催化材料降解水体中抗生素研究进展"", 《应用化学》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114602516A (en) * | 2022-04-13 | 2022-06-10 | 华北理工大学 | Fe-doped BiOBr photo-Fenton catalytic material rich in oxygen vacancies and preparation method thereof |
| CN116371397A (en) * | 2023-01-05 | 2023-07-04 | 华南理工大学 | Ce doped Bi 0 /Bi 2 O 3 /Bi 2 O 2.75 Nanosheet photocatalyst and preparation and application thereof |
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